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RELATED APPLICATION
[0001] The present invention is related to a co-pending application entitled: “SQL Debugging Using XML Dataflows”, Ser. No. ______, filed concurrently, (attorney docket no. SVL920010043US1), assigned to the assignee of the present invention and fully incorporated herein by reference.
BACKGROUND OF THE INVENTION
[0002] 1. Field of the Invention
[0003] This invention relates in general to database management systems performed by computers, and in particular to an optimized remote computer system database debugging, monitoring and managing technique useable in a client-server computing environment.
[0004] 2. Description of Related Art
[0005] Databases are computerized information storage and retrieval systems. A Relational Database Management System (RDBMS) is a database management system (DBMS) which uses relational techniques for storing and retrieving data. RDBMS software using a Structured Query Language (SQL) interface is well known in the art. The SQL interface has evolved into a standard language for RDBMS software and has been adopted as such by both the American National Standards Organization (ANSI) and the International Standards Organization (ISO).
[0006] Recently, Persistent SQL Modules (PSM) language became a standard language for coding SQL-based logic, such as stored procedures, user defined functions (UDFs) and triggers. PSM is very similar to Microsoft SQL Server's TSQL and Oracle PL/SQL, which are proprietary technologies and thus not standard. PSM allows for the development of DB2 stored procedures using the SQL language.
[0007] As with any development language, there exists a need to provide an efficient mechanism for debugging routines coded in SQL language, and especially for debugging stored procedures with SQL instructions. An efficient debugger currently exists for IBM DB2's Java and C/C++ stored procedures, which are currently debugged using IBM's Visual Age distributed debugger. There is a clear need to provide a similar cross-platform debugging support for SQL stored procedures. However, an efficient debugger for SQL stored procedures does not exist yet, and it has to be designed specifically for debugging SQL instructions written in PSM, because current DB2 implementation of PSM requires pre-compilation of PSM source code into C language code.
[0008] Currently, the support for DB2's SQL language stored procedures is achieved through a three-step compilation process. Step one compiles a PSM SQL stored procedure to an embedded SQL C file (file-name.sqc) using the DB2 PSM compiler. Step two compiles the file-name.sqc file to a standard C file using the DB2 SQL precompiler. Step three compiles the C file to generate the required execution library using any of the supported C language compilers. Therefore, the current implementation of PSM by DB2 is based on precompiling the PSM source into C language code, although in the future PSM may become an interpreted SQL language.
[0009] The basic requirement of any debugger is the ability to step through the original source code, view and modify variables, manage breakpoints, and capture execution exceptions. The C/C++ debugger is not suited to handle the debugging of SQL instructions, because the original PSM source code has to undergo three compilation steps, mentioned above, where the SQL language commands are translated into C language calls, and the SQL variables are translated into C language structures. Further, each SQL statement translates into multiple C language calls across multiple lines of code. Moreover, SQL language exception handling is very different from C/C++ exception handling, for which C/C++ debuggers are designed.
[0010] Attempts have been made to utilize the IBM's Visual Age C/C++ distributed debugger to debug SQL stored procedures. This is accomplished through some complex line macro mapping to the original SQL source file. However, there are a number of problems with this implementation that makes it very unusable. For example, C/C++ debugger is not suited for SQL language debugging because each SQL statement translates into multiple C statements, which may require multiple debugger commands to step over each line of SQL code. Next, SQL variable types translate into C structures foreign to SQL programmers. Moreover, SQL variable names are mangled while they go through the three compilation steps, and thus become hard to read by a SQL programmer. Furthermore, SQL variable values cannot be formatted according to SQL type value formatting, since they are treated as plain C/C++ types. Besides, SQL exception handling differs from C/C++ exception handling, making it difficult to detect by C/C++ debuggers.
[0011] Further, C/C++ debuggers work through standard debugger process attachment. This is an unacceptable risk to be taken by database administrators, as it not only assumes control of the SQL routine being debugged, but also the entire database engine, affecting all of its users. Moreover, C/C++ debuggers are not applicable to interpreted languages.
[0012] While there have been various techniques developed for optimizing the remote systems debugging and management functions, there is still a need in the art for further optimization techniques involving remote systems debugging operations. Therefore, it would be advantageous to provide a computer method that efficiently debugs and controls the target computer site, is easy to implement and maintain, and decreases the use of communication resources between processors.
SUMMARY OF THE INVENTION
[0013] The foregoing and other objects, features, and advantages of the present invention will be apparent from the following detailed description of the preferred embodiments, which makes reference to several drawing figures.
[0014] One preferred embodiment of the present invention is a method for SQL debugging within a computer system network. The method uses stored procedures via a console for debugging of SQL instructions located in a server, wherein preferably only one database communication line exists between the server and the console. The server has a database management system for retrieving data from a database stored in an electronic storage device coupled to the server. The method uses a debugger manager at the console for commanding and monitoring debugging operations of the server-side SQL instructions performed by a debugger engine, and uses stored procedures of a debugger router as a database communication interface for receiving commands and sending status reports between the debugger manager and the debugger engine.
[0015] The debugged SQL instructions are selected from a group comprising stored procedures, user defined functions and triggers. The method may invoke a database manager Data Access Remote Interface (DARI) process for performing debugging in a fenced server address and process space. The debugging method provides call-stack tracking, line-by-line execution status reporting, line breakpoints management, variable change breakpoints management, and has variable value reporting and modification capabilities. The debugging is performed through debugger interface software instructions, inserted during compilation of the SQL instructions as debugger hooks, for tracing the execution of the SQL instructions. The debugger interface software instructions include C API calls as debugger hooks which provide for each SQL instruction a source code line number for each SQL statement, names of variables declared by each SQL DECLARE statement, including the SQL type information, names of variables modified by the SQL statement, a current SQL code and state, for each routine entry and exit information, and for each exception entry and exit information.
[0016] Another preferred embodiment of the present invention is an apparatus implementing the above-mentioned method embodiment of the present invention.
[0017] Yet another preferred embodiment of the present invention is a program storage device readable by a computer tangibly embodying a program of instructions executable by the computer to perform method steps of the above-mentioned method embodiment of the present invention.
BRIEF DESCRIPTION OF THE DRAWINGS
[0018] Referring now to the drawings in which like reference numbers represent corresponding parts throughout:
[0019] [0019]FIG. 1 illustrates a computer hardware and software environment enabling trusted stored procedure debugging operations, according to some preferred embodiments of the present invention; and
[0020] [0020]FIG. 2 illustrates a computer hardware and software environment enabling non-trusted stored procedure debugging operations, according to other preferred embodiments of the present invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0021] In the following description of the preferred embodiments reference is made to the accompanying drawings, which form the part thereof, and in which are shown by way of illustration specific embodiments in which the invention may be practiced. It is to be understood that other embodiments may be utilized and structural and functional changes may be made without departing from the scope of the present invention.
[0022] The present invention discloses a system, method and program storage device embodying a program of instructions executable by a computer to perform the method of the present invention using stored procedures for debugging, monitoring and managing execution of stored procedures, user defined functions (UDFs), triggers and other relational database remote server resources in a computer network. The method and system are preferably used in a distributed computing environment in which two or more computer systems are connected by a network, including environments in which the networked computers are of different types. At least one database manager software system is installed on and runs on the networked server computer system. A network client computer system acts as the console for debugging, monitoring and managing resources present on a server computer system in the network. Although described herein in reference to debugging of stored procedures, the present invention is also applicable to debugging of UDFs and triggers, and especially useful for debugging of SQL instructions written in Persistent SQL Modules (PSM) language. While the preferred embodiments of the present invention are preferably debuggers for PSM SQL, the present invention is not limited to PSM, but can be used for any client-server database manager debugging operation, where the debugging session is invoked from a remote location, such as for debugging PL/SQL or TSQL instructions.
[0023] [0023]FIG. 1 illustrates an exemplary computer hardware and software environment useable by some preferred embodiments of the present invention. The environment includes a client management console 100 and a database server 102 , each having one or more conventional processors (not shown) executing instructions stored in an associated computer memory (not shown). The operating memory can be loaded with instructions received through an optional storage drive or through an interface with the network. The preferred embodiments of the present invention are especially advantageous when used in a network environment, having a console terminal 104 on the console 100 site, with the console 100 site processor networked to the server 102 site processor.
[0024] The database server 102 site processor is connected to one or more electronic storage devices 106 , such as disk drives, that store one or more relational databases. Storage devices may also be used on the console 100 site. They may comprise, for example, optical disk drives, magnetic tapes and/or semiconductor memory. Each storage device permits receipt of a program storage device, such as a magnetic media diskette, magnetic tape, optical disk, semiconductor memory and other machine-readable storage device, and allows for method program steps recorded on the program storage device to be read and transferred into the computer memory. The recorded program instructions may include the code for the method embodiment of the present invention. Alternatively, the program steps can be received into the operating memory from a computer over the network.
[0025] Operators of the console terminal 104 use a standard operator terminal interface (not shown), such as IMS/DB/DC, CICS, TSO, OS/2 or other similar interface, to transmit electrical signals to and from the console 100 , that represent commands, termed queries, for performing various debugging operations, as well as search and retrieval functions, against the databases stored on the electronic storage device 106 . In the present invention, these queries preferably conform to the Structured Query Language (SQL) standard, and invoke functions performed by a DataBase Management System (DBMS) 108 located at the server 102 site, such as a Relational DataBase Management System (RDBMS) software. In the preferred embodiments of the present invention, the RDBMS software is the DB2 product, offered by IBM for the AS400, OS390 or OS/2 operating systems, the Microsoft Windows operating systems, or any of the UNIX-based operating systems supported by the DB2. Those skilled in the art will recognize, however, that the present invention has application to any RDBMS software that uses SQL statements, and may similarly be applied to non-SQL queries.
[0026] [0026]FIG. 1 further illustrates a software environment enabling preferred embodiments of the present invention to be useable for debugging of trusted stored procedures. Trusted or unfenced SQL stored procedures are stored procedures that are allowed to run in the same address and process space as the database server 102 operations, because there is no need for special protection. In the system shown in FIG. 1, the client management console 100 further includes a client application software 110 of the present invention, capable of communicating with the database server 102 via a standard database connection communication line 112 , to invoke loading and running of a trusted SQL stored procedure on the database server 102 . The client management console 100 also includes a debugger manager software 114 with a user's interface (UI) that is capable of communicating with the database server 102 via the same standard database connection communication line 112 , during debugging.
[0027] Two server 102 site database manager agents (threads/processes) are used with the preferred embodiments of the present invention for debugging of a trusted SQL stored procedure on the database server 102 . They both use the database connection communication line 112 to communicate with the console 100 . Prior to debugging, the console-based client application 110 invokes an agent- 1 122 on the server 102 , which starts a debugger engine 118 , and commands it to load and start a debugged session 120 , running the trusted SQL stored procedure on the database server 102 . Afterwards, the trusted SQL stored procedure of the debugged session 120 is executed and debugged by the debugger engine 118 software. A session is a process (thread) executing some application software, which may include SQL stored procedures. The agent- 1 122 is also connected with the DBMS 108 and has access to the database items. It returns the debugging results back to the client application 110 , using the same database connection communication line 112 .
[0028] After the loading of the trusted SQL stored procedure, the debugging is commanded and monitored from the console terminal 104 via the debugger manager 114 software, which communicates with a debugger router 116 software, running on the server 102 as agent- 2 . The debugger router 116 software uses its own SQL stored procedures to communicate with the console 100 through the database connection communication line 112 . When the debugging and managing commands are on the server 102 site received by the debugger router 116 , it then invokes an appropriate system routine, sent to the debugger engine 118 to initiate or perform the debugging of the debugged session 120 , according to the request sent from the client management console 100 , and to return the requested information to the debugger manager 114 at the console 100 site. The debugger router 116 uses a set of stored procedures that are invoked by the debugger manager 114 to initiate and terminate the debugging, as well as send and receive data from the debugger engine 118 . Therefore, the debugger router 116 acts as a data router by forwarding client data from the debugger manager 114 to the debugger engine 118 and vice versa.
[0029] In all preferred embodiments of the present invention, shown in FIGS. 1 and 2, the debugging of the debugged session is performed through a debugger interface software. When a SQL stored procedure is compiled in debug mode, before its execution is requested by the client application, a set of debugger interface calls is included in the stored procedure code. During the debugging, these debugger interface calls are executed prior to and after executing the stored procedure SQL statement, to report the status of the stored procedure being executed and debugged. The status report includes information such as the name of the stored procedure, the current line of execution, the current variable SQL types and values, the values of the special SQLCODE and SQLSTATE DBMS registers, etc. Since the current implementation of PSM by the DB2 is based on precompiling the PSM source code into C language code, in the current implementation of the preferred embodiments of the present invention the PSM debugger interface is thus a set of C API (application programming interface) calls, that are inserted into the generated C code by the PSM compiler as debugger hooks, to trace the execution of the SQL stored procedure. Thus, these C API calls act as the interface to the debugger engine 118 . An example of a list of the PSM debugger interface C APIs insertable in the compiled PSM code, useable in the present invention, is presented below.
[0030] Void pd_EnterRoutine(
[0031] Int Line,
[0032] Char* pRoutineName,
[0033] Char* pSchema,
[0034] Char* pSpecific,
[0035] Int RoutineType);
[0036] Void pd_AtLine(
[0037] Long Sq1Code,
[0038] Char* pSq1State,
[0039] Int Line,
[0040] Int Indent);
[0041] Void pd_VarRegister(
[0042] Char* pVarName,
[0043] Char* pVarScope,
[0044] Void* pVarAddr,
[0045] Int VarType,
[0046] Int VarSize,
[0047] Int VarScale);
[0048] Void pd_VarMayChanged(
[0049] Char* pVarName,
[0050] Char* pVarScope);
[0051] Void pd_EnterException(
[0052] Long Sq1Code,
[0053] Char* pSq1State,
[0054] Int Line,
[0055] Int Indent);
[0056] Void pd_ExitException( );
[0057] Void pd_ExitRoutine(
[0058] Int Line,
[0059] Int rc);
[0060] where:
[0061] pRoutineName is the name of the SQL stored procedure (SP) or UDF. trigger, etc.
[0062] pSchema is the DB2 database schema identifier for the SP/UDF
[0063] pSpecific is the specific name for the SP, UDF, etc.
[0064] RoutineType is the type of the SQL routine: SP, UDF, etc.
[0065] Line is the text line number as per the original SQL source file
[0066] Indent is the code block indentation level
[0067] pVarName is the name of the SQL variable
[0068] pVarScope is the block scope of the variable in the source code
[0069] pVarAddr is the memory address for the variable storage
[0070] VarType is the SQL type of this variable
[0071] VarSize is the size of the var (e.g. char array size)
[0072] VarScale is the scale value for a decimal variable
[0073] Sq1Code is the current database server SQL code value
[0074] pSq1State is the current database server SQL state value
[0075] rc is the return code, if any
[0076] The debugger engine 118 software is installed on and runs on the server 102 computer system in the network. The debugger engine 118 is responsible for monitoring the execution of the loaded SQL stored procedure, and for enforcing requests for execution of the next SQL stored procedure statement. Another stored procedure may be nested and its execution be requested by the previous stored procedure. The debugger engine 118 may accomplish the request enforcement by implementing a rule that the debugger interface call does not return unless the debugger engine 118 decides that the next SQL statement is to be executed. The debugger engine 118 receives client debugger manager 114 commands and sends debugger status reports back to the client console 100 . This data exchange is carried forth using the debugger router 116 . The debugger engine 118 preferably communicates with the debugger router 116 using system message queues, a standard inter-process communication mechanism.
[0077] [0077]FIG. 2 illustrates a computer hardware and software environment enabling non-trusted stored procedure debugging operations, according to other preferred embodiments of the present invention. Non-trusted (fenced) SQL stored procedures are stored procedures that are run in a separate address and process space of a server 202 , isolated from the regular database server 202 address and process space. The system shown in FIG. 2 is very similar to the system shown in FIG. 1. A client management console 200 includes a terminal 204 , a processor (not shown) and a memory (not shown). It also includes a client application 210 software and a debugger manager 214 with a user's interface (UI), that is capable of communicating with the database server 202 via a standard database connection communication line 212 , during debugging.
[0078] In the server 202 , there is a processor (not shown) and a memory (not shown). The database server 202 site processor is connected to one or more electronic storage devices 206 , and a DBMS 208 . The same two server 202 site database manager agents (threads) are used with these preferred embodiments of the present invention of FIG. 2 for debugging of non-trusted SQL stored procedures on the database server 202 . They both use the database connection communication line 212 to communicate with the console 200 . Prior to debugging, the console-based client application 210 invokes an agent- 1 222 on the server 202 , which starts a debugger engine 218 , and commands loading and running of the non-trusted SQL stored procedure on the database server 202 . The non-trusted SQL stored procedure is executed and debugged by the debugger engine 218 software in a debugged session 220 . The agent- 1 222 returns the debugging results back to the client application 210 , using the same database connection communication line 212 .
[0079] After the loading of the non-trusted SQL stored procedure, the debugging is commanded and monitored from the console via the debugger manager 214 software, which communicates with a debugger router 216 software, running on the server 202 as agent- 2 . The debugger router 216 software uses its own SQL stored procedures to communicate with the console 200 through the database connection communication line 212 . When the debugging and managing commands are on the server 202 site received by the debugger router 216 , it then invokes an appropriate system routine sent to the debugger engine 218 , to initiate or perform the debugging of the debugged session 220 , according to the request sent from the client management console 200 , and to return the requested information to the debugger manager 214 at the console 200 site.
[0080] However, in the non-trusted preferred embodiments of the present invention, there is a new component, a database manager Data Access Remote Interface (DARI) process 224 , executing in a separate address and process space. When the client application 210 invokes a server side non-trusted SQL stored procedure, the database manager agent- 1 222 creates a separate, DARI process 224 on the server 202 machine and communicates with this DARI process 224 to execute the requested SQL stored procedure. The DARI process 224 executes the stored procedure, accessing the DBMS 208 , and returns the results back to the database agent- 1 222 . The database agent- 1 222 in-turn returns the results of this execution back to the client application 210 , using the database connection communication line 212 . Since the DARI process 224 is the server 202 process that executes the stored procedure, in these preferred embodiments of the present invention the debugger session 220 and debugger engine 218 are thus loaded as parts of the DARI process 224 , as shown in FIG. 2.
[0081] As mentioned above, in the preferred embodiments of the present invention, the described methods enable client-side debugging of server-side SQL stored procedures by extending a compiler to insert debugger hooks at the source level. Therefore, the preferred methods perform step-by-step debugging, by interruption of each executed instruction of a session running the stored procedure on a database server. A remote client location debugger manager, attached to the database server via a database communication line, is used to route debugger data and commands using a set of router stored procedures. While the preferred embodiments of the present invention are preferably debuggers for SQL compilers useable for PSM stored procedures with SQL instructions, the principles of the present invention are not limited to debuggers for PSM SQL instructions but can be used for any client-server database manager debugging operations, where the debugging session is invoked from a remote location.
[0082] Although shown in regard to debugging of stored procedures, the present invention can also be used in a similar way for debugging of SQL UDFs and SQL triggers, as both of these use PSM and are compiled in the same manner. As mentioned previously, in the present invention, the PSM debugger interface uses special debug C API calls as hooks. The PSM compiler inserts one or more of these debug C API calls before or after each compiled SQL statement when debugging may be needed. When a SQL stored procedure is compiled in debug mode, these debug C API calls are compiled-in and processed. However, when debugging is not needed in release mode, these debug C API calls are defined as no-operation (no-op'd) and compiled out from the SQL stored procedures. Shown below is an example of a SQL stored procedure with the required PSM Debugger Interface C API hooks inserted in the original source code of the stored procedure. The PSM Compiler inserts the following set of C APIs in the compiled PSM code as debugger hooks to trace the execution of the SQL stored procedure.
[0083] CREATE PROCEDURE iterator( )LANGUAGE SQL
[0084] BEGIN
[0085] pd_EnterRoutine(1, “iterator”, “Abdul”, “iterator”, SP);
[0086] pd_AtLine(SQLCOCDE, SQLSTATE, 3, 1);
[0087] DECLARE SQLSTATE CHAR(5);
[0088] pd_AtLine(SQLCOCDE, SQLSTATE, 4, 1);
[0089] DECLARE at_end INT DEFAULT 0;
[0090] pd_VarRegister(“at_end”, “iterator”, &at_end, INT, 4, 0);
[0091] pd_AtLine(SQLCOCDE, SQLSTATE, 5, 1);
[0092] LOOP
[0093] pd_AtLine(pDbgHdl, 6, 2);
[0094] FETCH c1 INTO v_dept, v_deptname;
[0095] pd_VarMayChanged(“v_dept”, “iterator”);
[0096] pd_VarMayChanged(“v_deptname”, “iterator”);
[0097] pd_AtLine(SQLCOCDE, SQLSTATE, 7,2);
[0098] IF at_end=1 THEN
[0099] pd_AtLine(SQLCOCDE, SQLSTATE, 8, 3);
[0100] LEAVE ins_loop;
[0101] pd_AtLine(SQLCOCDE, SQLSTATE, 9,2);
[0102] END IF;
[0103] pd_AtLine(SQLCOCDE, SQLSTATE, 10, 1);
[0104] END LOOP
[0105] pd_AtLine(SQLCOCDE, SQLSTATE, 11, 0);
[0106] END
[0107] pd_ExitRoutine(12, rc);
[0108] The PSM debugger interface calls the debugger engine 118 , 218 , and provides the functionality required of a full-fledged SQL debugger, such as call-stack tracking, line-by-line execution status reporting, line breakpoints, variable change breakpoints management, and variable value reporting and modification capabilities. The line-by-line inserted debug C API calls provide such information as the original source line number for each SQL statement, a list having names of variables declared by each SQL DECLARE statement including the SQL type information, a list having names of variables modified by the SQL statement, and a current SQL code and state. For each routine call the inserted debug C API call includes a routine entry and exit at the start and end of a SQL stored procedure, used to supply the routine information. For each exception call the inserted debug C API call includes an exception entry and exit at the start and end of a SQL exception handler, used to supply the exception information.
[0109] In the present invention, the client application 110 , 210 requests execution of a stored procedure being debugged on the server 102 , 202 site, where the debugging is controlled by a client at the client console 100 , 200 site. In the preferred embodiments the client uses the debugger router 116 , 216 stored procedures to communicate debugger user interface commands to the debugger engine 118 , 218 located at the database server 102 , 202 site, to control and monitor the execution flow of the debugged session 120 , 220 having SQL stored procedures being debugged. Therefore, the client uses stored procedures for communication with the debugger router 116 , 216 , and the debugger router uses local inter-process communication message queues to communicate with the debugger engine 118 , 218 . The debugger router forwards messages sent back and forth between the session, at the database server site, and the client at the client 110 , 200 site.
[0110] The debugger router uses a set of stored procedures required to facilitate data exchange between the debugger engine and the debugger manager. They include at least these four stored procedures: Initialize, Command, GetStatus and Terminate. The Initialize stored procedure is used to initialize the debugger router and establishes the message queue required to communicate with the debugger engine. The Command stored procedure is used to route debugging commands and data to the debugger engine. The GetStatus stored procedure is used to retrieve the status of the data obtained during the debugging operation. The Terminate stored procedure is used to terminate the debugger router operation and the communication message queue and cleans up the server's resources. In order to insure that the various debugger router Command and GetStatus stored procedures are routed to the same database agent, no transaction commit calls can be issued between the Initialize call and the Terminate call. This has no impact on the database logs, as no real database resources are locked by these debugger router stored procedures. An example of a set of stored procedures used by the debugger router 116 of the present invention, preferably defined in the db2psmdr library, is presented below.
[0111] 1. Stored procedure used to initialize the debugger engine for a specific debug session identifier:
db2psmdr!psmd_Initialize ( IN DOUBLE SessionId, OUT INTEGER Result);
[0112] 2. Stored procedure used to terminate and cleanup server resources for a specific debug session identifier:
db2psmdr!psmd_Terminate ( IN DOUBLE SessionId, OUT INTEGER Result);
[0113] 3. Stored procedure used to route user commands to the debugger engine for a specific debug session identifier:
db2psmdr!psmd_Commands ( IN DOUBLE SessionId, IN LONG VACHAR TextStream, IN LONG VACHAR FOR BIT DATA BinaryStream, OUT INTEGER Result);
[0114] 4. Stored procedure used to receive the debugger engine status report for a specific debug session identifier:
db2psmdr!psmd_GetStatus ( IN DOUBLE SessionId, OUT LONG VARCHAR TextStream, OUT LONG VARCHAR FOR BIT DATA BinaryStream, IN INTEGER WaitTimeOut, OUT INTEGER MoreDataPending, OUT INTEGER Result);
[0115] In the present invention, since the debugger router uses stored procedures to act as message routers between the debugger engine and the debugger manager, this enables the client to perform the debugging of the server-side SQL stored procedures using the same standard DB2 communication connection line 112 , 212 between the server site and client site, and does not require use of a separate connection and communication protocol. Using the stored procedures within the debugger router greatly simplifies the communication mechanism required between the client and the server, and provides a standard, well-known database communication interface for exchanging data between the debugger manager and debugger engine. The debugger manager invokes the debugger router stored procedures to send and receive data, whilst the debugger router communicates with the debugger engine using standard inter-process communication (IPC) mechanism, such as message queues, as they reside on the same server site where the debugged SQL stored procedures are running.
[0116] The preferred embodiments of the present invention thus avoid the key disadvantage of using the IBM Visual Age distributed debugger for debugging Java and C/C++ stored procedures, which rely on using TCP/IP to communicate back and forth between the server side component of the debugger and the client side debugger manager component of the debugger. Such implementation introduces additional complexity associated with setting up the proper protocol between the client and the server, whereby the server must establish a connection to a client deamon process using the pre-set TCP/IP address and port numbers. Setting up this type of model is very complex and requires a number of manual steps. Firewalls and DHCP are another obstacle in providing this type of communication mechanism. In the present invention, the use of stored procedures in the server side debugger router eliminates all this complexity, as the debugger router of the present invention uses for the communication the same DB2 communication line and protocol that is already configured by the client in order to invoke the original stored procedures being debugged, and is used for other database operations and applications, such as for database updates, etc.
[0117] The mechanism for exchange of communication debugging commands and data between the debugger engine and the debugger manager via the debugger router of the preferred embodiments of the present invention simplifies the communication protocol and content of messages sent back and forth, and eliminates the need for complex data formats and interfaces. There are two types of data that must be exchanged between the debugger engine and the debugger manager: debugging commands sent from the debugger manager to the debugger engine to control and monitor the execution of the stored procedures being debugged, and status reports sent from the debugger engine to the debugger manager reporting the status of the stored procedures being debugged.
[0118] Debuggers, regardless of language they are used with, provide a standard set of debugging commands to control the execution of the routine being debugged. Listed bellow are some of these standard debugging commands, including some SQL specific extensions, that are supported by the debugger of the present invention. The debugger of the present invention is able to support at least the following debugging commands from the debugger manager, sent to the debugger engine managing the stored procedures being debugged via the debugger router Command stored procedure: Run, Run to Line, Step Into, Step Over, Step Out, Step Return, Pause, Add Line Breakpoints, Add Variable Breakpoints, Toggle Breakpoint (enabled/disabled), Remove Breakpoints, Get Large Variable Values, Set Large Variable Value, Set Variable Value, and Run to Completion Without Further Debugging.
[0119] Run command is used to run the instructions until breakpoint is encountered or to the end. Run to Line command is used to run to the cursor line or until breakpoint is encountered. Step Into command is used to step into the next line of code. If the statement is a call to a procedure, the next statement will be the first statement in the called stored procedure. Step Over command is used to step over the next line of code skipping over any nested block of statements. If the statement is a call to another procedure, the debugging engine steps over and executes the called procedure as a unit, and then steps to the next line of code. Step Out command is used to get out of the current block of code. Step Return command is used to get out of current nested procedure and go back to the caller procedure. Pause command is used to stop the run command on the next possible line of code. Add Line Breakpoints command is used to add breakpoints for specific lines of code. Add Variable Breakpoints command is used to add variable value-changed breakpoints for specific variables. Toggle Breakpoint command is used to enable/disable breakpoints. Remove Breakpoints command is used to remove breakpoints. Get Large Variable values is used to retrieve a range value for a large variable type. Set Large Variable value command is used to modify a range value for a large variable type. Set Variable Value command is used to modify a variable value. Run to Completion command is used to run the stored procedure to completion without breaking.
[0120] Debuggers, regardless of language, also provide a standard set of debugging status reports to show the status of the routine being debugged. Listed bellow are some of these reports that are supported by standard debuggers, including some SQL specific extensions, that are also supported by the debugger of the present invention. The debugger of the present invention is able to support at least the following debug reports sent by the debugger engine managing the stored procedures being debugged, and retrieved by the debugger manager via the debugger router GetStatus stored procedure: Add Routine, Update Call Stack, Define Variable, Variable Value, Large Variable Value, Set Variable Visibility, At Line, At Breakpoint, At Exception, and End Run.
[0121] Add Routine status command is used to inform the debugger manager to load a new routine source due to a routine entry event. Update Call Stack status command is used to inform the client debugger manager of the current execution call stack. Define Variable status command is used to add a new routine variable that has now been declared. Variable Value status command is used to report a change in the current value of a variable. Large Variable Value status command is used to report a large variable value range due to a variable value change. Set Variable Visibility status command is used to toggle a variable visibility due to nesting of blocks that have DECLARE statements. At Line status command is used to report current execution line. At Breakpoint status command is used to report breaking due to encountering a line or a variable breakpoint. At Exception command is used to report encountering an exception. End Run status command is used to indicate that the routine has run to completion and debugging has been terminated.
[0122] The debugger of the present invention will soon be implemented under the name PSM Debugger in DB2's latest addition to the application development tool suite, in the DB2 UDB version V7.2, providing PSM debugging support for UNIX, Windows and other platform support. It will preferably be used for developing applications for DB2 servers in SQL PSM language, using stored procedures, UDF and triggers. The PSM debugger gives a user the ability to perform source-level debugging of PSM code. The DB2 Stored Procedure Builder will also be provided with this product, which includes the debugger manager user interface to the PSM Debugger, allowing the user to remotely debug server-side SQL stored procedures and other resources. The debugger manager user interface will be used to display the debugging session states, including all of the debugger views (such as, source code, variables, call stack, and break points), received from the server-side debugger engine, and to forward user commands to the debugger engine.
[0123] The present invention works with any of the IBM database manager products, such as DB2 for VM!VSE, DB2 for OS/390, DB2 for AS/400, DB2 Common Server, DB2 Universal Database. However, the technology may be applied to any other database manager products, such as Oracle, Informix, Sybase, SQL Anywhere, and Microsoft SQL Server, and other relational and non-relational products. The present invention allows for rapid and timely remote site software debugging, and minimizes the load on the network to initialize and maintain the remote site debugging operation. It may be applied to multivendor sources and targets, including Oracle, Sybase, Informix, Microsoft SQL Server, and others. It may be used with multidatabase servers that provide a single-site image to all data, relational and non-relational, local and remote, from IBM and non-IBM platforms, as though the data were local, regardless of the differences in SQL dialects, data access methods, networking protocols, and operating systems, in truly heterogeneous environments.
[0124] The foregoing description of the preferred embodiment of the invention has been presented for the purposes of illustration and description. It is not intended to be exhaustive or to limit the invention to the precise form disclosed. Many modifications and variations are possible in light of the above teaching. It is intended that the scope of the invention be limited not by this detailed description, but rather by the claims appended hereto.
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A method, apparatus and article of manufacture is provided for SQL debugging within a computer system network. The method uses stored procedures via a console for debugging of SQL instructions located in a server, wherein preferably only one database communication line exists between the server and the console. The server has a database management system for retrieving data from a database stored in an electronic storage device coupled to the server. The method uses a debugger manager at the console for commanding and monitoring debugging operations of the server-side SQL instructions performed by a debugger engine, and uses stored procedures of a debugger router as a database communication interface for receiving commands and sending status reports between the debugger manager and the debugger engine.
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BACKGROUND
[0001] The invention relates to a camshaft adjuster for an internal combustion engine according to the preamble of claim 1 .
[0002] From DE 102 11 607 A1, a camshaft adjuster for adjusting and fixing the relative rotational angle position of a camshaft relative to the crankshaft of an internal combustion engine is known. A hydraulic adjustment device here consists of an external rotor, which is allocated to a drive wheel, and also an internal rotor, which is connected to a camshaft via a driven element. Pressure chambers are formed between the external rotor and the internal rotor. Charging these chambers hydraulically can change the angular relationship between the drive wheel and driven element.
[0003] In the mentioned publication, it is proposed to produce the drive wheel and at least one of the other functional parts integrally from a high load capacity plastic. According to a first embodiment, the drive wheel and the external rotor and also two other components are produced integrally from plastic. For an alternative construction, the external rotor is produced as a separate component from plastic or from a conventional material, such as metal, and is set in a cover formed integrally with the drive wheel.
[0004] The outer rotor, which forms the radially outer boundaries, as well as boundaries in the peripheral direction of the pressure spaces, is screwed to a cover, which surrounds the outer rotor with a hollow cylindrical peripheral surface and which has brackets projecting radially outwardly from the peripheral surface and connected to the toothed ring by means of screws passing through the brackets.
[0005] The invention is based on the objective of providing a camshaft adjuster, which is improved in terms of radial installation size and/or the hydraulic pressure charge.
SUMMARY
[0006] According to the invention, the objective is met by the features of the independent claim 1 .
[0007] The invention is based on the knowledge that for a camshaft adjuster according to DE 102 11 607 A1, the radial installation size of the camshaft adjuster depends on the sum of the following dimensions:
The radial installation size of the outer rotor or the radius of the radial boundary of the pressure spaces, The required radial installation space for the attachment elements and also the brackets of the outer rotor and optionally allocated brackets or flanges, which extend radially inwardly from the toothed ring, and also The radial dimension of the toothed ring and the associated components.
[0011] According to the invention, the mentioned sum is reduced in that the attachment elements are arranged at least partially at a distance from a longitudinal axis of the camshaft adjuster, which is smaller than an outer radius of the pressure spaces. In this way, the dimensions according to b) and c) are not summed. Instead, the dimensions related to b) and c) overlap, so that the total radial installation size is reduced.
[0012] The use of the knowledge according to the invention produces new shaping possibilities:
For a given outer radius of the drive wheel required, for example, as a result of the gear transmission of the camshaft gearing, according to the invention the outer radius of the pressure spaces can be enlarged. For an unmodified hydraulic design, an inner radius of the pressure spaces can be enlarged, so that open installation space is produced in the camshaft adjuster radially on the inside. On the other hand, for a constant inner radius of the pressure spaces, the active surface for a hydraulic charge can be enlarged, whereby an improved adjustment effect and/or a reduced design of additional hydraulic components can be produced. For a constant outer diameter of the pressure spaces, the outer radius of the drive wheel can be reduced, whereby the radial installation size of the drive wheel and the camshaft adjuster can be reduced. Mixtures of the two mentioned alternatives are also possible, which produces expanded structural design possibilities and new installation space possibilities.
[0016] In the sense of the invention, attachment elements are understood to be attachment elements themselves, such as screws, rivet connections, or other positive or non-positive attachment elements, and also associated regions of the components to be connected, such as the flanges, brackets, or the like. According to the teaching according to the invention, the previously mentioned attachment elements are arranged at least partially in the radial direction at the height of the pressure spaces. Here, the attachment elements can be arranged at any position in the longitudinal direction of the camshaft adjuster and can be arranged arbitrarily over the peripheral direction.
[0017] According to a special construction of the invention, the attachment elements are arranged in the peripheral direction between pressure spaces and also in the direction of the longitudinal axis of the camshaft adjuster between axial boundaries of the pressure spaces. This construction is based on the knowledge that material clusters, which represent unused installation space and which cause additional weight in the outer rotor, are provided in the outer rotor between the pressure spaces in the peripheral direction according to the state of the art, whereby the mass moment of inertia of the camshaft adjuster is increased. According to the invention, this installation space can be advantageously used, in that the attachment elements are arranged within this space.
[0018] For this purpose, it can be advantageous according to an improvement of the invention if the outer rotor has radial bulges between adjacent pressure spaces, wherein the radial bulges mean material savings for the outer rotor and simultaneously create the installation space for the attachment elements. Radially inwardly oriented brackets, which can be connected rigidly to the toothed ring of the drive wheel, project into the radial bulges.
[0019] The invention is further based on the knowledge that for an embodiment of DE 102 11 607 A1, between the outer rotor and inner rotor, a bearing surface is formed with plastic, which is not optimum both for a contact partner made from metal and also for such an element made from plastic in terms of bearing properties, sliding properties, and wear as well as operational strength. For example, if a plastic in the form of a duroplastic is used for an external rotor, then it has been shown that such duroplastics can contain minerals. These minerals lead to increased wear and increased friction on sliding surfaces, also those made from steel, and in the worst case to failure of the camshaft adjuster. On the other hand, it has been shown for a second embodiment of DE 102 11 607 A1 that a use of a metallic bearing surface requires an additional mounting step, in some circumstances unnecessarily, in a surrounding plastic body. Furthermore, through such a placement, under some circumstances another degree of freedom or play and production inaccuracy for the bearing surface is produced, which can negatively affect the operation of the camshaft adjuster.
[0020] Therefore, according to the invention the bearing surface of the external rotor is formed with a metallic insert body, which is held with a non-positive fit in a carrier body made from plastic. Through this non-positive hold, the undesired degrees of freedom, play, and unnecessary mounting steps can be avoided. Nevertheless, according to the invention a metallic insert body can be used, so that a metallic bearing surface is given, whereby the increased wear and increased friction on the sliding surfaces can be avoided. The carrier body according to the invention can involve either the drive wheel itself or another component, such as a flange, which is connected to the drive wheel via corresponding attachment elements with a friction, positive, and/or firmly bonded fit, possibly under the intermediate connection of additional components.
[0021] According to one improvement of the invention, the insert body is constructed extending in the peripheral direction and also forms a limit for the pressure spaces in addition to the bearing surface. Accordingly, the insert body has a multifunction construction with the function of the bearing and the operating-fixed shape of the pressure spaces. Here, the insert body can limit the pressure spaces radially outwards and/or in the peripheral direction and, under some circumstances, can form limits or stops for the internal rotor. Through the formation of the insert body running in the peripheral direction, a rigid, closed ring structure is formed. In addition, the insert body thus correlates the position and orientation of several pressure spaces distributed over the periphery.
[0022] In one preferred camshaft adjuster according to the invention, the drive wheel is produced from a composite material. In the sense of the invention, a composite material is understood to be a material containing several sub-materials. These sub-materials can be formed, for example, as a carrier material with reinforcement elements arranged in the carrier material. The material can involve a fiber-composite material or a body formed from different layers of different materials. Examples here can be thermoplastics or duroplastics or materials made from thermoplastics and duroplastics together. In this way, according to the material selection and material combination, the mechanical properties of the drive wheel can be influenced in a suitable way.
[0023] According to another aspect of the invention, the internal rotor is also formed with plastic. The internal rotor has at least one bearing surface made from metal connected to this rotor with a firmly bonded fit. Accordingly, advantages known for a construction made from plastic and named, for example, in DE 102 11 607 A1 can be used for the rotor. In addition, both the internal rotor and also the external rotor have bearing surfaces made from metal, which has proven advantageous in terms of sliding properties and operating strength.
[0024] For the case that the attachment elements are not to interact with the material of the drive wheel or the flange otherwise used, it is advantageous when the attachment elements interact with reinforcement inserts of the drive wheel and/or the flange. Such reinforcement inserts can involve, for example, metal intermediate layers such as inserts, which are supported, for example, with their casing surface opposite the other material of the drive wheel or the flange while guaranteeing good a force introduction. Possible receptacle recesses of the reinforcement inserts can be shaped selectively for connecting to the attachment elements. For example, they can be inserted into the threading, with which the attachment elements are screwed. In this way, an especially compact construction of the camshaft adjuster is allowed for simultaneously good force introduction and transmission.
[0025] For a further improved camshaft adjuster, insert bodies and carrier bodies are connected to each other with a positive fit by means of an injection molding process. Accordingly, the insert bodies can be used in addition to their functions in operation during the production as shaping surfaces for an injection molding process, in that injection molding is performed on this material. The injection molding process simultaneously guarantees an especially good positive-fit connection between the contact body and carrier body.
[0026] Furthermore, the toothed ring can be formed in one piece with the brackets and with a composite material, wherein a reinforcing material of the composite material is arranged in the region of the brackets. In this way, the mechanical properties of the brackets can be improved.
BRIEF DESCRIPTION OF THE DRAWINGS
[0027] Additional features of the invention emerge from the following description and the associated drawings, in which embodiments of the invention are presented schematically. Shown are:
[0028] FIG. 1 a cross-sectional view of a part of a camshaft adjuster with an outer rotor and a carrier body made from plastic with a firmly bonded fit connected insert body and also an inner rotor supported rotatably in the outer rotor;
[0029] FIG. 2 a half longitudinal cross-sectional view of a camshaft adjuster in which the drive wheel made from plastic or an attachment element is attached to a flange;
[0030] FIG. 3 a view of a drive gearwheel made from plastic with radially inwardly pointing brackets for receiving attachment elements;
[0031] FIG. 4 a half longitudinal cross-sectional view of a drive wheel with a connecting piece or a bracket and inserts inserted into the connecting piece or bracket;
[0032] FIG. 5 a partial cross-sectional view of a drive gearwheel with radially inwardly pointing brackets and inserts arranged in these brackets;
[0033] FIG. 6 a cross-sectional view of a camshaft adjuster, wherein attachment elements are drawn radially inwardly, so that their spacing from the longitudinal axis of the camshaft adjuster is smaller than the outer diameter of the pressure chambers, and
[0034] FIG. 7 a view of a drive gearwheel made from plastic, which is attached to a housing of the camshaft adjuster via a carrier element.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0035] The invention relates to a hydraulic camshaft adjuster 1 in a known construction. The camshaft adjuster has a drive wheel 2 , which is formed as a pulley in the shown embodiments. An outer rotor 3 , which is arranged, in particular, radially inwardly from the drive wheel 2 , is connected rigidly to the drive wheel 2 . The outer rotor 3 is formed with bearing surfaces 4 , which correspond to segments of a casing surface of a cylinder, and also radial bulges for pressure chambers 5 . According to the embodiment shown in FIG. 1 , four bearing surfaces 4 and also four pressure chambers 5 are provided, which are distributed uniformly over the periphery. An inner rotor 6 , which can be locked or is locked in rotation with the camshaft, is arranged in the outer rotor 3 so that it can rotate relative to this outer rotor about a longitudinal axis of the camshaft adjuster 1 . The inner rotor 6 has bearing surfaces 7 formed corresponding to the bearing surfaces 4 of the outer rotor 3 and also has vane-like radial projections 8 , wherein four bearing surfaces 7 and four projections 8 are provided, which are distributed uniformly across the periphery of the inner rotor, according to the embodiment shown in FIG. 1 . The bearing surfaces 4 and 7 form a seal in the peripheral direction and the end faces of the projections 8 contact the associated pressure chambers 5 forming a seal radially on the outside, so that in the peripheral direction pressure spaces 9 , 10 are formed on both sides of the projections. Through suitable charging of the pressure spaces 9 , 10 , the relative angular position between the outer rotor 3 and the inner rotor 6 can be changed, whereby the angular relationship between the drive wheel 2 and a camshaft can be changed for adjusting the opening times of valves.
[0036] According to FIG. 1 , both the pressure chambers 5 and also the bearing surfaces 4 are both formed with a metallic insert body 11 , which extends in the peripheral direction and which has an approximately constant wall thickness. The insert body 11 is held with a firmly bonded fit in a carrier body 12 , which according to the embodiment shown in FIG. 1 is formed integrally with the drive wheel 2 or is formed as a separate component, which can be connected rigidly to the drive wheel 2 .
[0037] FIG. 2 shows a camshaft adjuster 1 ′ in longitudinal section. For this camshaft adjuster, the drive wheel 2 ′ is formed integrally with inwardly projecting brackets 13 , which are arranged approximately in the middle in the axial direction, which extend in the direction of a longitudinal axis X-X of the camshaft adjuster 1 ′ over one third to one fourth of a width of the running gearing of the drive wheel 2 ′, and which are distributed uniformly over the periphery, cf. FIG. 3 . A flange 14 , which is formed integrally with the outer rotor 3 ′, contacts an end of the brackets 13 . The brackets 13 and the flange 14 are connected to each other with a friction, positive, and/or firmly bonded fit and/or via attachment elements 15 , which are formed as screws according to FIG. 2 . Here, the brackets 13 and also the flange 14 have suitable bores 16 with or without threading. The bores 16 with or without threading can here be formed directly in the material forming the drive wheel or are prepared according to FIG. 4 by reinforcement intermediate layers 17 , especially inserts, for example, made from metal, which are attached preferably with a firmly bonded fit to the other integral elements of the drive wheel 2 .
[0038] In terms of the drive wheel 2 , the outer rotor 3 , the bearing surface 4 , the inner rotor 6 , the bearing surface 7 , the projections 8 , the insert body 11 , the carrier body 12 , the brackets 13 , and/or the flange 14 , there are the following shaping possibilities:
The components named above can be made from any plastic or from a fiber composite material. In particular, a thermoplastic or a duroplastic of any composition can be used. Furthermore, any composite material can be provided, for example, a plastic with an iron metal or a non-iron metal. In terms of the thermal expansion coefficients, these can be adapted to each other mutually, so that, for example, plastic, fiber composite materials, or composite materials have equal thermal expansion coefficients, such as adjacent components made from different materials. In particular, components arranged on the driven side, that is, components connected rigidly to the camshaft, can have a greater thermal expansion coefficient than components arranged on the drive side. The components named above can be joined to form units in one or more pieces. For example, the drive wheel 2 , the outer rotor 3 , the bearing surface 4 with insert body 11 , bracket 13 , and carrier body 12 , as well as flange 14 are formed as an integral, installation space-optimized component made from one or more materials or composite materials. For weight reduction and for improving the mounting possibilities, pockets can be provided in the components named above. The drive wheel 2 and insert body 11 can be connected to each other optionally through the intermediate connection of additional (sub) bodies with a positive fit, for example, by screws, with a form fit, for example, by rivets, or with a firmly bonded fit, for example, by adhesive, injection molding, or integral production, wherein combinations of the connection possibilities named above are conceivable. Non-plastic elements can be used as aids for the screw connection, for example, based on a “mold-in” or “after-molding” technology. A “mold-in” technology involves, for example, a metal bushing with threading, which is injection molded in a die, while as an example for an “after-mold” technique, a metal bushing with threading is conceivable, which is inserted in a plastic part after the injection-molding process. Metallic elements or sub-bodies can be formed as reinforcement material in other materials, for example, for homogenizing the expansion and/or for bracing, for forming support material, and for increasing the component stiffness. A selection of materials and their orientation can be used as thermal construction parameters, in which the expansion coefficient can be set to a desired target according to the element and its volume percentage. The use of reinforcement intermediate layers or inserts can be used, in particular, for minimizing setting force losses and for permitting direct screw connections. According to FIG. 1 , the outer rotor can be embedded directly into a plastic material. Assembling this plastic material with the outer rotor can be realized directly, for example, in an injection molding process or else by means of a later assembly.
[0049] FIG. 6 shows a partial cross section allocated to the embodiment according to FIG. 2 . Here, the casing surface of the outer rotor 3 with the pressure spaces 5 has a back-and-forth or meander-shaped construction with different radii, wherein, in the region of the pressure spaces 5 , the outer radius is at a maximum and the radius is reduced in the peripheral region between adjacent pressure spaces 5 through radial bulges or recesses 18 . The brackets 13 , which are connected to the toothed ring 19 rigidly or with a firmly bonded fit, project into the recesses 18 and are connected to the outer rotor 3 in the region of the recesses 18 . In this way, the attachment elements 15 can be “pulled down” to smaller radii, so that the attachment elements 15 act at a radius that lies in the region of the outer diameter 35 of the pressure chamber 5 or that is smaller than this. Here, the attachment elements 15 , the brackets 13 , an optional flange 14 , and the recesses 18 are provided preferably axially between the end faces 33 , 34 of the drive wheel 2 or corresponding end faces of the pressure spaces 5 , so that a small axial installation size is also produced.
[0050] FIG. 7 shows an example construction for a drive wheel 2 ″ with allocated components, here a toothed ring 19 , a carrier element 20 , and a housing 21 .
[0051] The housing 21 is formed especially as a sheet-metal part with an approximately cylindrical casing surface 22 and includes additional components of the camshaft adjuster 1 ″. The carrier element 20 is supported rigidly on the casing surface 22 , especially by a firmly bonded connection. Here, the carrier element 20 has a hollow cylindrical contact connecting piece 23 , which contacts the casing surface 22 radially at the inside and is connected to the housing 21 with a firmly bonded fit on at least one axial end face. The contact connecting piece 23 transitions, especially under the intermediate connection of a transition radius, into a circular disk-shaped carrier body 24 , which is oriented coaxial to the longitudinal axis X-X and which, in turn, transitions in a hollow cylindrical outer body 25 with a surrounding shoulder 26 or collar in the end region opposite the carrier body 24 .
[0052] The toothed ring 19 contacts the shoulder 26 in the region of an axial end face, while the opposite end of the toothed ring 19 has a radially inwardly projecting radial projection 27 , which contacts the carrier body 24 or the transition region between the carrier body 24 and outer body 25 . The toothed ring 19 has radially on the inside, especially approximately in the middle, a surrounding projection or connection region 29 provided across sub-peripheries, which extends approximately over half the width of the toothed ring 19 . The connection region 29 is connected to the outer casing surface of the outer body 25 with a firmly bonded fit.
[0053] For the toothed ring 19 , the carrier element 20 , and the housing 21 , all of the previously mentioned materials or material combinations can be used. As an example embodiment, a production of the toothed ring 19 from plastic, especially a duroplastic, is conceivable, while the carrier element 20 and the housing 21 are produced from a metal.
[0054] The shoulder 26 can be used alternatively or additionally for simplifying the mounting of a guide of a drive element like a toothed belt or a control chain in the direction of the longitudinal axis X-X.
[0055] The outer body 25 has on its outer casing surface preferably recesses 31 or depressions or grooves, which can be formed as pockets in the outer body or can pass through this body. For the shown embodiment, the recesses 31 are formed with an approximately rectangular cross section. Radially inwardly oriented projections 32 or a surrounding collar extend radially inwardly from the toothed ring 19 , especially from the projection 30 . These projections are held with a positive fit at least in the longitudinal direction X-X and/or in the peripheral direction in the recess 31 , depression, or groove. In the radial direction, the toothed ring 19 can be guided opposite the carrier element 20 through the projection 30 and/or projection 32 .
LIST OF REFERENCE SYMBOLS
[0000]
1 Camshaft adjuster
2 Drive wheel
3 Outer rotor
4 Bearing surface of outer rotor
5 Pressure chamber
6 Inner rotor
7 Bearing surface of inner rotor
8 Projections
9 Pressure space
10 Pressure space
11 Insert body
12 Carrier body
13 Bracket
14 Flange
15 Attachment element
16 Bore
17 Reinforcement insert
18 Recess
19 Toothed ring
20 Carrier element
21 Housing
22 Casing surface
23 Contact connecting piece
24 Carrier body
25 Outer body
26 Shoulder
27 Projection
28 First connection region
29 Second connection region
30 Projection
31 Recess
32 Projection
33 Axial end face
34 Axial end face
35 Outer radius of pressure chamber
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A camshaft adjuster ( 1 ) for an internal combustion engine is provided, in which the relative angular position between a driving gear ( 2 ) and an output element that is allocated to the camshaft can be adjusted by hydraulically impinging pressure chambers located between an inner and outer rotor. The outer rotor and the gear ring of the driving gear ( 2 ) are joined to each other via fastening elements ( 15 ). In order to create a particularly compact camshaft adjuster ( 1 ), the fastening elements are located at least in part at a distance from the longitudinal axis of the camshaft adjuster ( 1 ) which is smaller than the external radius ( 35 ) of the pressure chambers.
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BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to a structure and method for configuring a field programmable gate array (FPGA).
2. Description of the Prior Art
An FPGA typically includes configuration memory cells, configuration control elements and a matrix of logic blocks and I/O blocks. To create a desired circuit, the user writes a data bit to each of the configuration memory cells. The configuration control elements are configured in response to the data bits stored in configuration memory cells. The user selects the data bits such that the configuration control elements properly configure the logic and I/O blocks to form the circuitry required by the user's design.
FIG. 1 is a schematic diagram of a prior art configuration memory cell 100 and an associated configuration control element 110. Configuration memory cell 100 includes programming transistor 101 and inverters 102 and 103. Configuration memory cell 100 is programmed using means external to the FPGA. In programming configuration memory cell 100, an enable (EN) signal is provided to the gate of transistor 101 on lead 106 and a programming (PRG) signal is provided to the source of transistor 101 on lead 107. The PRG signal is thereby transmitted through transistor 101 and stored in the latch formed by inverters 102 and 103. After the PRG signal is stored by inverters 102 and 103, the EN signal is de-asserted. As a result, the PRG signal is provided to configuration control circuit 110 on lead 104 and the inverse of the PRG signal (PRG) is provided to configuration control circuit 110 on lead 105. In response, configuration control circuit 110 provides (or prevents) an interconnection between other elements (such as logic and/or I/O blocks) in the FPGA.
The PRG signal used to program configuration memory cell 100 is a bit which is typically stored in an EEPROM, EPROM, ROM, floppy disk or hard disk which is part of the external programming means. A conventional FPGA may contain thousands of configuration memory cells like configuration memory cell 100. Programming all of these configuration memory cells requires thousands of bits. These bits are all loaded by the external programming means. When the FPGA is configured, the external programming means transmits the required bits to the FPGA in the form of a bit stream. Because this bit stream travels along a physical path from the external programming means to the FPGA, the bit stream can be accessed fairly easily by tapping into this physical path. Although copyright protection may be obtained for the bit stream, an unscrupulous copyist can nonetheless reproduce the user's device by recording the bit stream, reproducing the bit stream, and applying the bit stream to an identical FPGA. The copyist can generally obtain an identical FPGA "off the shelf" because, within a product line, FPGA's are typically manufactured in a generic manner.
Because the costs associated with designing the configuration of an FPGA-based device are significant, it would be desirable to have an FPGA which is more difficult to copy, without substantially adding to the complexity of the FPGA.
SUMMARY OF THE INVENTION
Accordingly, the present invention provides a structure and method for configuring a field programmable gate array (FPGA). In one embodiment of the invention, a programming signal is transmitted to a configuration memory cell within the FPGA. In response, the configuration memory cell provides a signal to a configuration control circuit which is used to configure the FPGA. The configuration memory cell includes an input lead, a storage device and a selectable configuration circuit. The input lead carries the programming signal to the storage device. The storage device stores the programming signal and the inverse of the programming signal. The selectable configuration circuit is coupled to the storage device. The selectable configuration circuit can be selectably configured to provide the programming signal or the inverted programming signal to a first input lead of the configuration control circuit. The configuration control circuit couples (or decouples) various elements of the FPGA in response to the signal provided on the first input lead.
In an alternate embodiment, the selectable configuration circuit is coupled between the input lead and the storage device. Again, the selectable configuration circuit can be selectably configured to provide the programming signal or the inverted programming signal to the first input lead of the configuration control circuit.
The above described configuration memory cells provide several advantages. In one embodiment, all of the selectable configuration circuits of the FPGA are selectably configured such that the FPGA is placed in the desired configuration when all of the programming signals are at logic low level. In such an embodiment, the FPGA is internally programmed by connecting all of the configuration memory cells to a logic low signal during start up of the FPGA.
In an alternate embodiment, the selectable configuration circuits of an FPGA are randomly fabricated to have either a first or a second configuration. The random order of the selectable configuration circuits is user specific. That is, the FPGAs utilized by a particular user are identical, with each FPGA having the same random order of selectable configuration circuits. The order of the selectable configuration circuits is known only to the user, and only the user can readily obtain an FPGA having the particular random order of selectable configuration circuitry. Thus, while the user still provides a bit stream to program the FPGA, this bit stream will only properly program FPGA's available to the user. In this manner, the invention provides an additional level of security within the FPGA.
The invention will be more fully understood in view of the following drawings taken together with the detailed description.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a schematic diagram of a prior art FPGA configuration memory cell;
FIG. 2 is a schematic diagram of an FPGA configuration memory cell in accordance with one embodiment of the invention;
FIG. 3 is a schematic diagram of one embodiment of the configuration control circuit of FIG. 2;
FIGS. 4-6 are schematic diagrams illustrating various applications of configuration memory cells and configuration control circuits of the invention; and
FIG. 7 is a schematic diagram of an FPGA configuration memory cell in accordance with another embodiment of the invention.
DETAILED DESCRIPTION OF THE INVENTION
FIG. 2 is a schematic diagram of a configuration memory cell 200 in accordance with one embodiment of the invention. Configuration memory cell 200 includes transistor 201, inverters 202 and 203 and selectable configuration circuit 206. The gate of transistor 201 receives an enable (EN) signal from a programming device on lead 208. The source of transistor 201 receives a programming (PRG) signal from the programming device on lead 209. The PRG signal is a bit having either a logic high or a logic low value. To program configuration memory cell 200, the EN signal is asserted high. The high EN signal turns on transistor 201, thereby allowing the PRG signal to be transmitted through transistor 201 to the latch 207 formed by inverters 202 and 203. In one embodiment, inverters 202 and 203 are conventional CMOS inverters. Latch 207 stores the PRG signal even after the EN signal is de-asserted low.
Latch 207 is coupled to selectable configuration circuitry 206. Selectable configuration circuitry 206 includes nodes 221-224. Latch 207 provides the PRG signal to node 221. Similarly, latch 207 provides the inverse of the programming signal (PRG) to node 223. Conductive paths are selectively formed to connect nodes 221 and 223 to nodes 222 and 224 in one of two configurations.
In a first configuration, an electrically conductive path connects nodes 221 and 222, and another conductive path connects nodes 223 and 224. In this first configuration, the PRG signal is provided to node 222 and the PRG signal is provided to node 224. Consequently, the PRG and PRG signals are provided to input leads 204 and 205, respectively, of configuration control circuit 210.
In a second configuration, a conductive path is formed between nodes 221 and 224, and another conductive path is formed between nodes 223 and 222. In this configuration, the signal is provided to node 222 and the PRG signal is provided to node 224. Consequently, the PRG and PRG signals are provided to input leads 205 and 204, respectively, of configuration control circuit 210.
Because the first and second configurations transpose the manner in which the PRG and PRG signals are provided to configuration control circuit 210, the response of the configuration control circuit 210 is dependent upon the configuration of selectable configuration circuit 206. As described in more detail below, configuration control circuit 210 provides a first response when selectable configuration circuit 206 is in the first configuration, and a second response, which is opposite to the first response, when selectable configuration circuit 206 is in the second configuration.
The signals on nodes 222 and 224 are provided to configuration control circuit 210 on leads 204 and 205, respectively. Configuration control circuit 210 is a conventional circuit which is responsive to the signals on leads 204 and 205. In one embodiment, configuration control circuit 210 is a transmission gate that controls the interconnection of segments 230 and 240 of the FPGA.
FIG. 3 is a schematic diagram of an embodiment in which configuration control circuit 210 is a transmission gate formed by n-channel transistor 301 and p-channel transistor 302. The gate of n-channel transistor 301 is connected to lead 204 and the gate of p-channel transistor 302 is connected to lead 205. Consequently, if selectable configuration circuitry 206 has the first configuration described above (i.e., the PRG signal applied to lead 204 and the PRG signal applied to lead 205), a logic high PRG signal causes transistors 301 and 302 to turn on, thereby connecting routing segments 230 and 240. Routing segments 230 and 240 connect logic blocks and other circuitry within the FPGA.
Conversely, if selectable configuration circuitry 206 has the previously described second configuration (i.e., the PRG signal applied to lead 204 and the PRG signal applied to lead 205), a logic high PRG signal causes transistors 301 and 302 to turn off, thereby isolating interconnect routing segments 230 and 240.
By controlling the configuration of memory cell 200, several advantages are obtained. As previously discussed, each FPGA may contain thousands of configuration memory cells which must be programmed from an external programming source to properly configure the FPGA. However, in accordance with the invention, the configuration memory cells may be programmed internally when the FPGA is powered-up. To accomplish this, the selectable configuration circuitry of each configuration memory cell in the FPGA is fabricated such that when a low PRG signal is applied to the associated configuration control circuit, the configuration control circuit is placed in the desired configuration. During power-up of the FPGA, the EN signal is asserted high and the PRG signal provided to each configuration memory cell is de-asserted low, resulting in the desired FPGA configuration.
For example, if the desired FPGA configuration requires that transistors 301 and 302 (FIG. 3) are turned off to disconnect segments 230 and 240, the selectable configuration circuitry 206 is fabricated such that node 221 is connected to node 222 and such that node 223 is connected to node 224. When a low PRG signal is applied to latch 207 via transistor 201, a low signal is applied to lead 204 and a high signal is applied to lead 205. As a result, transistors 301 and 302 are turned off to provide the desired configuration.
In the above-described embodiment, even though the FPGA is placed in a default configuration when logic low PRG signals are provided to the configuration memory cells, the FPGA remains programmable. To create a different configuration, an external bit stream is used to program the configuration memory cells of the FPGA. This bit stream includes logic high signals which are provided to the configuration memory cells which are to be reprogrammed and logic low signals which are provided to the configuration memory cells which are to remain unchanged.
In a variation of the invention, the selectable configuration circuits of the configuration memory cells of an FPGA are randomly fabricated to have either the first or second configuration. The random order of the selectable configuration circuits is user specific. That is, the FPGAs utilized by a particular user are identical, with each FPGA having the same random order of selectable configuration circuits. The order of the selectable configuration circuits is known only to the user. The user still provides a bit stream to program the FPGA. However, this bit stream will only properly program an FPGA which has the random order of selectable configuration circuitry found on the user's FPGA. Consequently, a copyist can no longer replicate the user's device by copying the bit stream provided to the user's FPGA, buying an identical, conventional FPGA off the shelf, and programming the conventional FPGA by reproducing the user's bit stream. Thus, the invention provides an additional level of security within the FPGA.
Selectable configuration circuit 206 can be realized in a number of different ways. In one embodiment, the interconnection of selectable configuration circuit 206 is determined by appropriately patterning the masks which are used to fabricate the interconnects between latch 207 and configuration control circuit 210.
In an alternate embodiment, the masks which are used to fabricate the interconnects between latch 207 and configuration control circuit 210 are patterned to provide connections between nodes 221 and 223, nodes 221 and 224, nodes 222 and 223, and nodes 222 and 224. A laser is then used in accordance with conventional techniques to eliminate the undesired connections. The lasing may be performed by the manufacturer or designer of the FPGA.
In yet other embodiments, conventional programmable fuses, EPROM cells or EEPROM cells are fabricated between nodes 221 and 223, nodes 221 and 224, nodes 222 and 223, and nodes 222 and 224. These elements are then programmed using conventional methods to form the desired connections between nodes 221-224.
FIG. 4 is a schematic diagram illustrating another application of the invention. Configuration memory cells 400a and 400b control the configuration of multiplexers 411a and 411b, respectively. Configuration memory cells 400a and 400b are similar to configuration memory cell 200 (FIG. 2). Leads 421 and 422 connect the output terminals of configuration memory cell 400a to the control input terminals of multiplexer 411a. When configuration memory cell 400a provides a logic low signal on lead 421 and a logic high signal on lead 422, a logic low signal is transmitted through multiplexer 411a to the reset input terminal of flip flop 401. Consequently, flip flop 401 is operated such that the flip flop 401 is not reset.
Conversely, when configuration memory cell 400a provides a logic high signal on lead 421 and a logic low signal on lead 422, a RESET input signal is transmitted through multiplexer 411a to the reset input terminal of flip flop 401. The RESET input signal controls whether flip flop 401 is reset.
In a similar manner, configuration memory cell 400b controls the signal provided to the clock enable (CLKEN) input terminal of flip flop 401. When a logic low signal is provided to lead 423 and a logic high signal is provided to lead 424, the signal provided to the CLKEN input of flip flop 401 is a logic high signal. In this case, flip flop 401 is always enabled. When a logic high signal is provided to lead 423 and a logic low signal is provided to lead 424, a CLKEN input signal is provided to the CLKEN input terminal of flip flop 401.
In another application, configuration memory cells and configuration control circuits in accordance with the invention are used to create a ROM look up table. FIG. 5 is a schematic diagram of an 8-bit ROM look up table which utilizes configuration memory cells 500a-500h. Configuration memory cells 500a-500h are similar to configuration memory cell 200 (FIG. 2). Output leads 501a-501h couple one of the output terminals of configuration memory cells 500a-500h to input terminals of 8-to-1 multiplexer 503. Configuration memory cells 500a-500h are programmed such that the output leads 501a-501h carry a logic high or a logic low signal, depending upon the desired look up table values. Multiplexer 503 connects the output terminal of one of configuration control circuits 510a-510h to output terminal 504 in response to a 3-bit control signal received from function generator 502. Although this application has been described in connection with an 8-bit look up table, it is understood that this application is easily modified to include look up tables having other numbers of bits.
In yet another application, a configuration memory cell and configuration control circuit of the invention can be used to control whether signals within the FPGA will be interpreted as active-high or active-low. FIG. 6 is a schematic diagram illustrating how configuration memory cell 600 can be used to control the active-high/active-low status of a CLKEN input signal. Leads 621 and 622 connect the output terminals of configuration memory cell 600 to the control terminals of multiplexer 601. When configuration memory cell 600 is programmed such that a logic low signal is provided on lead 621 and a logic high signal is provided on lead 622, the CLKEN input signal is transmitted through multiplexer 601 to the CLKEN input terminal of flip flop 602. In this configuration, the CLKEN input signal is active-high.
Conversely, when configuration memory cell 600 is programmed to provide a logic high signal on lead 621 and a logic low signal on lead 622, the CLKEN input signal is inverted by inverter 603, and passed through multiplexer 601 to the CLKEN input terminal of flip flop 602. In this configuration, the CLKEN input signal is active-low.
FIG. 7 is a schematic diagram of a configuration memory cell 700 in accordance with the invention. Configuration memory cell 700 includes transistor 701, inverters 702 and 703 and selectable configuration circuit 706. Configuration memory cell 700 operates in a manner similar to configuration memory cell 200. However, selectable configuration circuit 706 is connected between transistor 701 and the latch 707 formed by inverters 702 and 703.
Selectable configuration circuit 706 is connected in one of two configurations. In a first configuration, node 721 is connected to node 722. In this configuration, the PRG signal transmitted through transistor 701 to latch 707 is provided to configuration control circuit 710 on lead 704 and the signal is provided to configuration control circuit 710 on lead 705.
In a second configuration, node 721 is connected to node 723. In this configuration, the PRG and PRG signals are transmitted to configuration control circuit 710 on leads 704 and 705, respectively.
Configuration memory cell 700 can be fabricated in accordance with any of the methods previously described in connection with configuration memory cell 200.
While the invention has been described in connection with particular embodiments, it is understood that the invention is not limited to the embodiments disclosed, but is capable of various modifications which would be apparent to one of ordinary skill in the art. Thus, the invention is limited only by the following claims.
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A structure and method for configuring a field programmable gate array (FPGA). A configuration memory cell within the FPGA receives a programming signal. In response, the configuration memory cell provides a signal to a configuration control circuit to configure the FPGA. The configuration memory cell includes an input lead, a storage device and a selectable configuration circuit. The input lead carries the programming signal to the storage device. The storage device stores the programming signal and an inverted programming signal which is the inverse of the programming signal. The selectable configuration circuit can be selectably configured to provide the programming signal or the inverted programming signal to a first input lead of the configuration control circuit. The configuration control circuit couples (or decouples) various elements of the FPGA in response to the signal provided on the first input lead.
In an alternate embodiment, the selectable configuration circuit is coupled between the input lead and the storage device. Again, the selectable configuration circuit can be selectably configured to provide the programming signal or the inverted programming signal to the first input lead of the configuration control circuit.
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This is a division of application Ser. No. 743,902, filed June 12, 1985, pending.
BACKGROUND OF THE INVENTION
The strengthening of yarn spun from anisotropic-melt forming polyesters is taught in Luise U.S. Pat. No. 4,183,895. The Patentee acknowledges that heat treatment may cause fusion between the filaments which can make it impractical to rewind the yarn. It is suggested in said patent that useful results have been obtained if the filaments are precoated with a thin layer of an inert substance, for example, talc, graphite or alumina. Further improvements are, however, desired to prevent sticking of filaments to each other during heat treatment. The use of anisotropic-melt polyester fiber has been suggested for composite reinforcement. The need to promote the adhesion of such fiber to matrices in composites has also been recognized. This invention provides improvements in these areas.
SUMMARY OF THE INVENTION
The present invention provides a process for heat strengthening a yarn spun from an anisotropic-melt forming polyester without substantial interfilament or intrafilament fusion. The yarn is coated with a dispersion of hydrophobic silica having an average primary particle size below about 50 nanometers in a liquid carrier and heated in a substantially inert atmosphere below the filament melting point for a time sufficient to increase yarn tenacity. The precursor and end-product yarn as well as certain resin matrix composites reinforced with such yarns are also part of the invention.
DETAILED DESCRIPTION OF THE INVENTION
A class of wholly aromatic polyesters that form optically anisotropic melts from which oriented filaments can be melt spun is described in Schaefgen U.S. Pat. No. 4,118,372. Other anisotropic-melt forming polyesters are disclosed in U.S. Pat. Nos. 4,083,829; 4,153,779 and in many other patents and applications. The as-spun oriented fibers from such polyesters are strengthened by heating while essentially free from tension and in an essentially inert atmosphere. The conditions of heat treatment are fully described in U.S. Pat. No. 4,183,895.
In accordance with this invention as-spun anisotropic-melt forming polyester filament yarn is first coated with a hydrophobic silica having an average primary particle size below about 50 nanometers (nm). The term primary refers to the non-agglomerated particle. The filament yarn may be a multifilament yarn or a heavy denier monofilament yarn.
The hydrophobic silicas used in the examples below are fumed silicas referred to as Aerosil® R-972 or R-976 produced by Degussa Corporation. They are identified and described in Degussa trade literature of 6/26/84. Aerosil® R-972, for example, is produced by treating a standard Aerosil type 130 which has 3-4 hydroxyl groups per square nanometer and a surface area of about 130 m 2 /gm with dimethyl dichlorosilane at above 500° C. in a continuous process. It is believed that other hydrophobic silicas should also be useful. Some are described in the aforementioned Degussa publication. Other particulate materials disclosed in the prior art are distinguishable from the hydrophobic silica employed herein. Thus, graphite is not as effective in preventing interfilament adhesion and presents housekeeping problems due to flaking of the graphite off the filaments. Further, neither graphite nor hydrophilic silica provides the high adhesion levels of the fiber to epoxy matrix materials as does hydrophobic silica. Hydrophilic silica also tends to agglomerate, making it less effective in preventing filament sticking. One disadvantage of alumina is the fact that it is abrasive and can present wear problems on rolls. Thus, the hydrophobic silica presents many advantages over products heretofore suggested in the art.
The hydrophobic silica is preferably applied from a dispersion in an organic liquid carrier although any compatible liquid carrier may be used. The preferred liquid carrier is a polar fluid preferably one having a high density. Chlorinated hydrocarbons, such as perchloroethylene are useful. Methylene chloride and methanol mixtures have also been used with good results. The particular carrier employed is not believed to be critical. The dispersion is applied to uniformly deposit at least about 2 μg and up to 100 μg of hydrophobic silica per square centimeter of filament surface area. Greater amounts may be used but no advantage is expected in the use of such larger amounts.
After the yarn is coated, it is subjected to a heat treatment to strengthen the yarn. This treatment is described in the aforementioned U.S. Pat. No. 4,183,895. If desired, an accelerator can be used as described in U.S. Pat. No. 4,424,184. The yarn is heated, preferably without tension, at a temperature in excess of 250° C. but below the filament melt temperature, preferably in an inert atmosphere and for a time sufficient to increase tenacity, preferably by at least 50%, over the as-spun yarn. In the course of this process, the hydrophobic silica particles are firmly attached to the filament surface and remain substantially uniformly distributed along the surface. Interfilament and intrafilament fusion appears to be substantially avoided. Thus, in the case of the heavy denier monofilament yarn, fusion between contacting segments of the filament will be reduced during the heat treatment while in the case of multifilament yarn fusion is avoided between adjacent filaments and contacting yarn segments.
Yarns produced in accordance with this invention are useful in epoxy resin matrix composites as reinforcement. In such applications they have been shown to exhibit improved adhesion. The reinforcement is ordinarily employed in proportions between 5 and 70 volume percent based on fiber reinforced matrix composite. Improved adhesion to rubber is found where the yarns are given an epoxy subcoat.
TEST PROCEDURES
Tensile properties for multifilament yarns were measured with a recording stress-strain analyzer at 21° C. and 65% relative humidity using 3 turns-per-inch twist and a gauge length of 5 in (12.7 cm). Results are reported as T/E/M, where T is break tenacity in grams per densier, E is elongation-at-break expressed as the percentage by which the initial length increased, and M is the initial tensile modulus in grams per denier (gpd). Average tensile properties for at least three specimens are reported.
When considering the examples that follow, it should be understood that the results reported are believed to the representative and may not constitute all of the runs performed.
EXAMPLE 1
A coating dispersion is prepared from 10 gm of fumed, hydrophobic silica (Aerosil® R-972 from Dugussa with a 16 nanometer average primary particle size) and 600 gm of perchloroethylene by stirring until a homogeneous, white, colloidal dispersion is obtained. Several meters of an 870-denier, anisotropic-melt polyester yarn (ca. 8.7 dpf) prepared in accordance with the general techniques of U.S. Pat. No. 4,183,895 from a polymer of the following composition--chlorohydroquinone (40 mole %), 4,4'-dihydroxydiphenyl (10 mole %), terephthalic acid (40 mol %) and isophthalic acid (10 mol %)--are immersed in the dispersion for several minutes. The coated yarn sample was gently removed from the dispersion and placed on Fiberfrax® (a batted ceramic insulation of the Carborundum Company) in a perforated metal basket. A control yarn without coating from the same source was placed in a similar basket. The yarn samples were then heat strengthened in an oven purged with nitrogen following a programmed, 16 hr., heating cycle with a maximum temperature of about 306° C. In the cycle the oven is purged with nitrogen at room temperature (RT), for about 1/2 hr, and then the temperature is gradually elevated from RT to 200° C. in 2 hr, 200° C. to 306° C. in 7.3 hr, held at 306° C. for 7.5 hr, and then cooled to RT. After heat treatment, the control yarn was fused while individual filaments could be easily separated from the fumed-silica-coated yarn. The silica particles appear to be strongly adhered to the fiber surface. About 50 μg per cm 2 of yarn is determined to be present. Observations in a scanning electron microscope showed a uniform distribution of silica particles on the fiber surface.
EXAMPLE 2
A 60 denier, 10-filament yarn spun from polymer of the same composition as Example 1 was immersed in a hydrophobic silica dispersion as in Example 1 and then removed. Samples of this coated yarn and an uncoated control yarn from the same source were heat strengthened in 3.0-meter tube oven as described in Example 5 of U.S. Pat. No. 4,424,184. The sample yarns were placed on a continuous, glass-fiber belt and moved through the oven with about a 45 minute residence time. The oven was continuously purged with nitrogen flowing at about 0.3 SCF/min. A typical temperature profile, determined by use of thermocouples spaced about 30 cm apart starting 30 cm within the oven from the entrance, was 178°, 240°, 270°, 284°, 294°, 300°, 299°, 302° and 295° C. The uncoated yarn was fused while the coated yarn was not. (T/E/M of the fused yarn was 4.7 gpd/1.5%/282 gpd and the T/E/M of the coated yarn was 8.2 gpd/1.9%/473 gpd.)
EXAMPLE 3
A 60 denier, 10-filament yarn spun from polymer of the same composition as Example 1 was treated with a 1% aqueous KI solution (containing 0.1% Triton® X-100 as surfactant) to accelerate heat-strengthening. A sample of the yarn was coated as in Example 1. Another sample was left uncoated. Both were heat strengthened following the procedure of Example 2. The uncoated yarn was fused while the coated yarn was not. (T/E/M of the fused yarn was 21.4 gpd/3.3%/527 gpd and the T/E/M of the coated yarn was 18.7 gpd/3.0%/531 gpd).
EXAMPLE 4
This example demonstrates the improvement in cord-to-rubber adhesion achieved with yarn of the invention as compared with similar yarn coated with graphite prior to heat treatment.
Hydrophobic silica was applied to 1500 denier, 400-filament, as-spun yarn from the same polyester composition as in Example 1 from a 2% Aerosil® R-972 dispersion in methanol/methylene chloride (75/25) at such a rate that 1.2% silica was deposited based on dry-yarn weight. The liquid medium was evaporated and the yarn piddled into a perforated metal basket. Similarly, graphite was applied to 1500 denier, 400-filament, as-spun yarn from a 12% Microfyne flake graphite (Joseph Dixon Crucible Co.) dispersion in methanol/methylene chloride (75/25). The yarns were heat strengthened in an oven purged with nitrogen using at 16 hr. programmed heating cycle with a maximum temperature of about 306° C. as in Example 1. They were backwound with the application of a lubricating finish and twisted to 1500/1/2, 6.5 TM (twist multiplier) cords.
A commercial, single-end, cord-treating unit (Litzler Co.) was used to apply and cure an epoxy subcoat and resorcinol formaldehyde latex (RFL) topcoat to the cords. The epoxy subcoat was cured at 450° F./60 sec/7 lb tension: the RFL topcoat was cured at 475° F./90 sec/3.5 lb tension.
A 120° C., 2-ply, strap-adhesion test (ASTM D-2630-71) was used to evaluate the cord-to-rubber adhesion. The results below show that the silica coating improves both the peel strength and the appearance rating.
______________________________________ AppearanceItem Coating Peel Strenqth (lb/in) Rating*______________________________________A Silica 51 4.5B Graphite 38 1.9______________________________________ *5 = all rubber tear, no cord visible, to 1 = no rubber on cords.
EXAMPLE 5
This example demonstrates the improvement in cord-to-rubber adhesion achieved with yarn of the invention as compared with similar yarn coated with hydrophilic silica (Aerosil® 200).
In separate runs, hydrophobic silica Item A and hydrophilic silica Item B were applied to yarns as in Example 4 and the yarns were similarly treated and incorporated into a rubber matrix and then tested (ASTM D-2630-71). The results were as follows:
______________________________________ AppearanceItem Coating Peel Strength (lb/in) Rating*______________________________________A Hydrophobic Silica 40 4.3B Hydrophilic Silica 36 2.3______________________________________ *As in Example 4.
EXAMPLE 6
A 200 filament, approximately 760 denier yarn was prepared from an anisotropic melt polyester of the following composition--chlorohydroquinone (50 mole %), terephthalic acid (35 mole %) and 2,6-dicarboxynaphthalene (15 mole %). Samples of the yarn were coated with hydrophobic silica and then heat strengthened as in Example 4. The yarn was essentially free of fused filaments.
EXAMPLE 7
This example demonstrates the improvement in fiber-to-matrix adhesion achieved with yarn of the invention compared to similar yarn coated with graphite prior to heat treatment.
Hydrophobic silica and graphite were applied to 940 denier, 200-filament, as-spun yarn from dispersions in methanol/methylene chloride (75/25) as in Example 4. The yarns were heat strengthened in an oven purged with nitrogen using a 16 hr. programmed heating cycle with a maximum temperature of about 306° C. as in Example 1.
Unidirectional composite bars were prepared for testing using these heat-strengthened coated yarns and an epoxy matrix following the procedures found in U.S. Pat. No. 4,418,164 for filament winding (except as otherwise indicated). The bars were wound using undried yarn and a mixture of 100 parts of diglycidyl ether of bisphenol-A (Epon 826 Shell), 25 parts of 1,4-butanediol diglycidyl ether (Araldite RD-2 Ciba-Geigy) and 30 parts aromatic diamine curing agent (Tonox, Uniroyal). They were cured for 1.5 hr. at 120° C. followed by 1 hr. at 175° C.
Short-beam-shear test (ASTM D-2344-76 with samples tested at a 4:1 span to depth ratio) results on these bars indicated a substantial improvement in adhesion between fiber and matrix for the hydrophobic silica-coated yarn compared to the graphite-coated yarn (6430 vs. 4500 psi. respectively).
EXAMPLE 8
Hydrophobic silica (Aerosil® R-976 with a 7 nanometer average primary particle size) was applied from a 5% dispersion in methanol/methylene chloride (75/25) using a finish application roll to about a 400-denier monofilament yarn spun from a polymer with the composition of Example 1. The coated monofilament was wound on a six-inch-diameter, perforated metal bobbin wrapped with Fiberfax®. The bobbin of monofilament yarn was heat strengthened in an oven purged with nitrogen using a 16-hr programmed heating cycle with a maximum temperature of about 306° C. similar to Example 1. The heat-treated monofilament yarn was not fused and could be easily backwound from the bobbin.
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Application of hydrophobic silica to an anisotropic-melt forming polyester yarn reduces interfilament and intrafilament fusion during heat-strengthening. Improvements in adhesion of yarn to certain matrices are noted.
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BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention relates generally to processes for the treatment mercaptans. More specifically this invention relates to processes for the removal of mercaptans from normally gaseous hydrocarbons streams.
2. Description of the Prior Art
The sweetening of sour hydrocarbons streams by the conversion or removal of mercaptan sulfur is well known. Mercaptans present in such feedstreams are converted by the sweetening process to disulfide compounds. In the sweetening process the mercaptan containing hydrocarbon contacts a mercaptan oxidation catalyst carried by an alkaline solution in the presence of an oxygen supply stream. Typically in the performance of the sweetening process the disulfides remain in the hydrocarbon stream and are, therefore, not removed but converted to an acceptable form.
A wide variety of processes are known for the sweetening of distillates. U.S. Pat. No. 4,490,246 and the references cited therein set forth a number of flow schemes for the sweetening process. A number of different separation arrangements can be used to recover the treated distillate and the catalyst containing alkaline stream. The '246 patent seeks to reduce the separation of dissolved disulfide gases from a liquid product and teaches the use of a settler and a low pressure separator to remove a gaseous phase of disulfides from the product effluent of the sweetening process. As demonstrated by U.S. Pat. No. 2,988,500 a single settler can be used to withdraw excess gases overhead, a product stream from an intermediate section of the settler and a bottoms stream of an alkaline catalyst solution.
Extraction processes are typically used when treating light hydrocarbons and gas streams for mercaptan removal. In the extraction process the feed first contacts a caustic solution in an extraction column. The caustic solution contains a mercaptan oxidation catalyst. Feed depleted in mercaptans passes overhead from the extraction column and the mercaptan containing caustic passes countercurrently from the bottom of the column. The mercaptan rich caustic receives an injection of air and catalyst as it passes from the extraction column to an oxidizer for the conversion of mercaptans to disulfides. A disufide settler receives the disulfide rich caustic from the oxidizer. The disulfide settler vents excess air and decants disulfides from the caustic before the caustic is returned to the extractor.
The above described extraction flow scheme can be used to remove mercaptans from fuel gas streams in refineries. In such arrangements the feed is contacted under gaseous conditions. However, such schemes have been found to be unsatisfactory in reducing sulfur concentrations to very low levels when the feed streams have a continuous or intermittent oxygen concentration. The presence of oxygen in the feed leads to oxidation of the mercaptans to disulfides in the extractor. These disulfides are stripped from the caustic by the volatile fuel gas and raise the total sulfur concentration of the fuel gas product to unacceptable levels for environmental standards.
Other methods are known to reduce the sulfur concentration of mercaptan containing gas streams. U.S. Pat. No. 4,808,341 issued Feb. 28, 1989 discloses a process for the separation of gases from mercaptans, the process uses a lean oil to absorb mercaptans in a first contacting zone and regenerates the absorption oil by contacting the mercaptan rich oil with an aqueous oxidizing agent to produce a sulfuric acid solution and a hydrocarbon absorption oil.
SUMMARY OF THE INVENTION
Accordingly, it is an object of this invention to provide an extraction process for the treatment of mercaptan containing gas streams that have a continuous or intermittent oxygen concentration.
It is a further object of this invention to provide a process that uses an aqueous alkaline catalyst solution to extract mercaptans from a mercaptan and oxygen-containing gas stream.
This invention provides a process that removes mercaptans from an oxygen-containing gas stream without sulfur contamination of the gas product or the regeneration of an absorbent stream. The process of this invention removes mercaptans from the gas stream by converting them to disulfides in the presence of an aqueous alkaline solution containing a mercaptan oxidation catalyst and a liquid hydrocarbon stream that acts as a disulfide acceptor. By using the liquid hydrocarbon stream in the mixing zone, the mercaptans in the gas stream can be converted to disulfides and absorbed into a liquid phase without contaminating the gas stream product. The gaseous stream, the alkaline solution and the liquid hydrocarbon stream enter a settler that separates the gaseous product, the liquid hydrocarbon stream and the catalyst containing alkaline solution. The use of a single settler and a liquid hydrocarbon stream as a disulfide acceptor provides a simple process arrangement for the production of a very low sulfur gas stream.
Accordingly in one embodiment, this invention is a process for desulfurizing a gaseous feedstock containing mercaptans, hydrocarbons and oxygen. The process comprises mixing the gaseous feedstock, a low vapor pressure liquid hydrocarbon stream and an aqueous alkaline solution containing a mercaptan oxidation catalyst in a mixing vessel to convert the mercaptans to disulfides and absorb disulfides in the liquid hydrocarbon stream. The mixture of the feedstock, the aqueous alkaline solution, the oxidation catalyst and the disulfide containing liquid hydrocarbon stream are passed to a settler vessel. An upper gaseous phase, an intermediate liquid hydrocarbon phase and a lower aqueous phase are maintained in the settler vessel. A gaseous phase containing hydrocarbons and having a reduced concentration of mercaptans relative to the gaseous feedstock is withdrawn from the upper phase of the settler vessel. A disulfide containing liquid hydrocarbon is withdrawn from an intermediate phase of the settler vessel and removed from the process. The aqueous alkaline solution is withdrawn from the lower phase and returned to the mixing vessel.
In a more specific embodiment, this invention is a process for desulfurizing a gaseous feedstock that contains mercaptans, hydrocarbons and oxygen. The process includes the steps of admixing the gaseous feedstock, a naphtha boiling range hydrocarbon stream and an aqueous alkaline solution containing a mercaptan oxidation catalyst. The admixture is passed to a mixing vessel at conditions to maintain the naphtha stream in liquid phase, to convert the mercaptans to the disulfides and absorb disulfides in the naphtha. An oxygen concentration of at least 20 vol. % more than the theoretical mercaptan demand is maintained in the mixing vessel. A mixing vessel effluent comprising the feedstock, the aqueous alkaline solution, oxidation catalyst and a disulfide containing naphtha stream are passed to a settler vessel. An upper gaseous phase, an intermediate liquid naphtha phase, and a lower aqueous phase is maintained in the settler vessel. A gaseous hydrocarbon stream having a total sulfur concentration of less than 40 mol ppm is withdrawn from the gaseous phase of the settler vessel. Naphtha from the intermediate naphtha phase is withdrawn from the settler vessel and removed from the process. The aqueous alkaline solution is removed from the lower phase of the settler vessel and returned for admixture with the feedstock and naphtha stream.
Other objects, embodiments and details of this invention are disclosed in the following detailed description of the invention.
BRIEF DESCRIPTION OF THE DRAWING
The FIGURE shows a schematic representation of a process flowscheme for practicing the process of this invention.
A general understanding of the process of this invention can be obtained by reference to the drawing. The drawing has been simplified by the deletion of a large number of apparatus customarily employed in a process of this nature such as vessel internals, temperature and pressure control systems, flow control valves, recycle pumps, etc. which are not specifically required to illustrate the performance of the subject process. Furthermore, the illustration of the process of this invention in the embodiment of a specific drawing is not intended to limit the invention or preclude other embodiments set out herein, or reasonably expected modifications thereof. Referring then to the drawing, a hydrocarbonaceous gas stream containing mercaptan sulfur and possibly oxygen enters the process through line 10. A line 12 carries an aqueous alkaline stream that contains a mercaptan oxidation catalyst which is introduced into line 12 by a catalyst addition line 14. A line 16 carries a relatively low vapor pressure hydrocarbon stream. The contents of lines 12 and 16 along with air from a line 18 pass into admixture with the contents of line 10 and are charged to a mixing vessel 20. After sufficient contacting and residence time in vessel 20 to convert mercaptans in the feedstream to disulfides, a line 22 carries the mixture of gaseous feed, a disulfide containing liquid hydrocarbon stream, and the aqueous soltuion of mercaptan oxidation catalyst into a settle vessel 24. Quiescent conditions are maintained in the settler vessel to establish an upper gaseous phase 26, an intermediate liquid hydrocarbon phase 28 and an aqueous phase 30. The treated gas stream having a low concentration of mercaptan and disulfide sulfur is withdrawn from the gaseous phase by a line 32 and recovered as a product. The aqueous phase containing the alkaline contacting medium is withdrawn from the bottom of the settler vessel by a line 34 and pressured by pump 36 back into contact with the gaseous feed via line 12. The low pressure liquid hydrocarbon phase now containing an increased concentration of disulfides is withdrawn from phase 28 by a line 38. A portion of the liquid hydrocarbon phase is withdrawn from the process by a line 40 for use as an intermediate or product in other processes, a pump 42 circulates the remaining portion of the liquid hydrocarbons from line 38 back into contact with the gaseous feed by a line 16. Additional amounts of low vapor pressure liquid hydrocarbons are added to line 16 by a line 44. Fresh caustic and spent caustic are added as make up or withdrawn from the unit batchwise via line 33.
DETAILED DESCRIPTION OF THE INVENTION
This invention is used to remove mercaptan sulfur and any derivative sulfur compounds from gaseous feedstocks. These feedstocks will be primarily composed of C 4 and lower carbon number hydrocarbons. In most instances, suitable feedstreams will comprise C 3 and lighter hydrocarbons. In particular, the feedstreams will primarily compose fuel gas streams having a gross heating value of more than 300 BTU per standard cubic feet. Feedstreams of this type will often be subject to environmental regulations for a reduction in the total amount of sulfur emitted by the combustion of such fuel gas streams. This invention will be used to reduce the sulfur in the gaseous product stream to a range of from 10 to 100 mol ppm and more preferably to below 40 mol ppm sulfur calculated as H 2 S. It is anticipated that refinery flare gas streams, refinery product off gas streams, tank vapor recovery systems, and other typical refinery fuel gas sources will provide the primary source of the gaseous feedstock when practicing this invention. Another characteristic of suitable feedstocks for this invention is that they contain oxygen in an amount of from 0 to 5 vol. % on a continuous or intermittent basis. It is the presence of this oxygen that makes other mercaptan extraction systems unsuitable for treating such feedstocks and provides the operational benefits of this invention.
The feedstocks will also contain mercaptans. The relatively lighter mercaptans contained in the gaseous feedstock can be readily converted to disulfides by the sweetening reaction of this invention. The sweetening reaction is promoted in the usual manner by the contact of the mercaptans with an aqueous alkali solution in which the mercaptans are soluble. The alkaline solution can comprise any alkaline hydroxide but is preferably sodium hydroxide in a concentration of from 1 to 25 wt %. The aqueous alkaline solution will usually be added to the unit in an amount equal to 1 to 25 wt. % of NaOH and preferably 5 to 10 wt. % of NaOH.
As in most sweetening operations, the aqueous alkaline solution will also contain a mercaptan oxidation catalyst. This invention does not require the use of a specific mercaptan oxidation catalyst. Many suitable catalysts are known in the art. One preferred class of catalysts comprise a sulfonated metal phthalocyanine. A particularly preferred sulfonated metal phthalocyanine is a highly monosulfonated cobalt phthalocyanine prepared by the method of U.S. Pat. No. 4,049,572, the teachings of which are herein incorporated by reference. Other phthalocyanine catalysts are described in U.S. Pat. No. 4,897,180. Additional dipolar type catalyst that are suitable for use in an alkaline contacting solution are described in U.S. Pat. Nos. 4,956,324; 3,923,645; 3,980,582 and 4,090,954. Usually a relatively small concentration of oxidation catalyst is required in the aqueous alkaline solution. Any method can be used to add the oxidation catalyst to the aqueous alkaline solution including such devices as a blow case or an injection pump. Typically, the oxidation catalyst in the aqueous alkaline solution will have a concentration of from 10 to 500 wt. ppm and preferably a concentration of 200 wt. ppm.
Sweetening of the mercaptans in the mixing vessel is done in the presence of a relatively low vapor pressure liquid hydrocarbon stream that can act as a disulfide acceptor. The disulfides must be removed from the normally gaseous phase portion of the treating admixture in order to reduce the final sulfur concentration of the product. The liquid hydrocarbon stream will function as an absorbent to retain the disulfides that are produced from the sweetening of the mercaptans. The liquid hydrocarbon stream must be present in a sufficient concentration and with a sufficiently low disulfide partial pressure in order to prevent the volatilization of disulfides into the product gas stream. In order to prevent volatilization of mercaptans, the liquid hydrocarbon stream will comprise C 5 and higher hydrocarbon fractions having boiling points of at least 100° F. or more. More preferably, the streams will comprise 200°-400° F. boiling range hydrotreated naphthas. Reforming and alkylate product streams are also preferred. When using a typical naphtha stream as the liquid hydrocarbon, the aqueous alkaline solution to the naphtha can usually range from 100:1 to 1:100 and preferably will be in a ratio of from 5:1 to 10:1. Suitable liquid hydrocarbon streams will also be streams that can readily accept disulfides without deterioration of the value or utility of such streams. For most refiners, low vapor pressure liquid hydrocarbon products will be available in sufficient quantity and with allowable product specifications for disulfide concentration to meet the disulfide adsorption requirements of this invention.
While this invention is particularly suited to treating oxygen-containing gaseous hydrocarbon streams, in some cases the oxygen concentration of such streams will be insufficient to completely convert all mercaptans to disulfides. In order to allow a complete regeneration of mercaptans from the aqueous alkaline solution, an additional amount of oxygen-containing gas may be required as a reactant. The oxygen-containing gas may be added at any point where it can react with soluble mercaptans in the aqueous alkaline stream. Preferably any needed oxygen-containing gas, typically air, will be added to the mixture of gaseous feed, aqueous alkaline solution and liquid hydrocarbons.
Complete conversion of mercaptans to disulfide and absorption of disulfides into the normally liquid hydrocarbon stream is assured by contact of feedstock and feed inputs in a mixing zone. The mixing zone would normally comprise a vertical contacting vessel. The aqueous alkaline stream and the liquid hydrocarbon streams would normally flow upwardly through the vessel, but downward flow may be preferable in some cases. The mixing vessel is designed to provide sufficient residence time and contacting of the reactants and absorbents to provide the necessary conversion of mercaptans and removal of disulfides from the normally gaseous components. A broad range of operating conditions can be used to promote the sweetening reaction in the mixing vessel. Typically, these conditions will include a temperature of from 50°-150° F. and a pressure of from 2 to 2000 psig. Those skilled in the art are aware of a variety of such mixing devices that can be used to provide contact and residence time for the sweetening reaction to occur. Suitable devices for this invention would include orifice plate columns, trayed contactors, packed contactors or fiber film contactors as described in U.S. Pat. No. 3,754,377. Although the drawing shows the process operating with a concurrent flow of gaseous and liquid phase components, the invention can also be practiced with countercurrent flow of the liquid components to the gaseous feedstock.
A separation zone receives a product containing mixture from the mixing vessel. The mixture comprises the catalyst containing alkaline solution, a liquid hydrocarbon stream, and the product gases. In this invention the separation zone provides a three-phase settling operation which separates the product gases, liquid hydrocarbon, and catalyst containing alkaline solution into three distinct phases. For the purposes of this description, the term "phase" refers to the different physical states of the gas and liquid portions as well as the different immiscible components of the liquid portion. The settler vessel is arranged with appropriate baffling to provide quiescent conditions that will allow a stable formation of the three phases. The settler vessel is preferentially arranged horizontally and operates at a pressure and temperature similar to that in the mixing vessel. Product gases form the uppermost phase in the settler vessel. A product line at the top of the vessel withdraws the product gases. Below the uppermost gas phase, the liquid hydrocarbon stream forms an intermediate phase. An inlet located in a mid portion of the settler vessel withdraws the liquid hydrocarbon from an intermediate point of the settler vessel. The alkaline solution fills the bottom portion of the settler vessel with an aqueous phase that drains from the vessel. Regulation of the withdrawal rates for the three output streams from the settler vessel in conjunction with monitoring of the different phase levels maintains the intermediate phase within definite vertical limits to assure the continuous availability of all three streams from the settler vessel.
A portion of the liquid hydrocarbon withdrawn from the intermediate phase of the settler vessel usually leaves the process. Usually some proportion of the liquid phase returns as a recycle to the inlet of the mixing vessel. An influx of additional liquid hydrocarbons replaces the liquid hydrocarbons withdrawn from the process and keeps the disulfide partial pressure in the circulating liquid hydrocarbon stream at a desired level. The removal and replacement of the liquid hydrocarbon stream from the process provides a primary mechanism for controlling the disulfide concentration of the product stream. Thus, the relative proportion of recycled liquid hydrocarbon will vary with the disulfide concentration of the liquid hydrocarbon stream entering the process and the amount of mercaptans to be removed from the feed gas. Therefore, the amount of liquid hydrocarbon recycled to the process can vary with any wide range of limits depending on the liquid hydrocarbon and the gaseous feedstock. However, for a typical naphtha stream and fuel gas feed from 5 to 95 vol. % of the liquid hydrocarbons will return as a recycle.
EXAMPLE
In order to further demonstrate a typical operation of this process, the following example shows the process of this invention treating a gaseous feedstock having the composition described in the Table. This example is further described with reference to the specific flowscheme shown in the Figure. This example has been generated from a computer simulation of the process of this invention using correlations and data from experimental results and actual operating units.
In the mixing operation, an air stream in an amount of 700 standard cubic feet per hour, a 1.85 molar NaOH solution containing 200 wt. ppm of a cobalt phthalocyanine catalyst and a recirculating naphtha stream in an amount of 14 gallons per minute combined with 6300 standard cubic feet per minute of the gaseous feedstock enter the mixing vessel. The mixing vessel operates at a temperature of 100° F. and a pressure of 100 psia. After an average residence time of about 2 minutes, the triple phase effluent from the mixing vessel flows into a settler vessel.
The settler vessel separates the mixed phase effluent into the three components previously described. Caustic removed from the bottom of the settler vessel returns for admixture with the feed. Periodically, an additional amount of fresh caustic containing approximately 200 wt. ppm of the oxidation catalyst is added to the recycle stream. Approximately, 50 vol. % of the naphtha removed from the settler vessel leaves the process. Fresh hydrotreated naphtha having a boiling point of 300°-500° F. replaces all of the naphtha that exits the process and flows in combination with the remainder of the naphtha from the settler vessel into admixture with the gas feed. A product gas stream having the composition given in the table flows out of the top of the settler vessel.
As demonstrated by this example, the process of this invention reduces the mercaptan and disulfide concentration of the gaseous feed to very low levels. This reduction of sulfur compounds uses very little processing equipment and a relatively simple process scheme. The simple flowscheme and process operation makes this invention particularly useful in meeting the sulfur removal requirements of oxygen-containing fuel gas streams.
TABLE______________________________________ Feed Gas Product GasComponent Mol % Mol % (ppm)______________________________________Hydrogen 28.00 28.02Methane 28.00 27.96Nitrogen 5.00 4.99Oxygen 0.08 0.08Ethane 22.92 22.84Propane 10.00 9.90Isobutane 5.96 5.80Mercaptans 0.04 (5)Disulfides -- (13)Naphtha -- 0.41 100.00 100.00______________________________________
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Fuel gas streams containing oxygen are treated by a process that performs simultaneous sweetening and absorption of mercaptan compounds. The mercaptan oxidation catalyst and an aqueous alkaline solution and a low vapor pressure liquid hydrocarbon stream contact the fuel gas feed in a mixing vessel to sweeten the mercaptans and absorb resulting disulfides from the gas stream into the liquid hydrocarbon stream. A separation vessel receives the dual phase effluent from the mixing vessel and settles the effluent into three component phases. An upper gas phase provides a treated fuel gas stream, an intermediate hydrocarbon phase provides liquid hydrocarbons containing disulfides for removal from the process, and recycle to the mixing vessel and an alkaline solution drains from the bottom of the settler. The aqueous alkaline solution is pumped back to the mixing vessel in combination with the mercaptan oxidation catalyst.
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FIELD OF THE INVENTION
[0001] The present invention relates generally to a reusable cardboard insert that will support the structure and use of a standard size (34″×16″×12″) lawn and garden refuse bag. More particularly the invention relates to the ability to shape the cardboard insert to the fit the inner dimensions of the lawn and garden refuse bag to facilitate keeping the lawn and garden refuse bag fully open and accessible to the user while it is yet without sufficient refuse inside of it to keep the lawn and garden refuse bag from collapsing. Claimant makes no claim to lawn and garden refuse bag(s) that are currently and commonly in use in commerce as of this application.
BACKGROUND OF THE INVENTION
[0002] The invention will be described with reference to its ability to be folded along perforated lines that have the dimensions that are shown on the renderings provided.
[0003] It is desirable for persons gathering lawn and garden refuse to be able to collect said refuse in a lawn and garden refuse bag(s) without said lawn and garden refuse bag(s) collapsing from an open usable position to a closed, unusable position allowing a portion of the gathered refuse to fall outside the internal collection area of the lawn and garden refuse bag's potential storage area. What is needed is a structurally stabilizing insert to hold the lawn and garden refuse bag in the full and open position allowing greatest access to the internal storage area.
[0004] Although cardboard is used for many purposes in our everyday lives, there is (are) no specific use(s) of cardboard for the purpose of rendering lawn and garden refuse bags fully open, accessible and usable in the initial stages of its storage use.
SUMMARY OF THE INVENTION
[0005] The present invention provides for a flat rectangular piece of cardboard with overall dimensions of 36″×32″×¼″ to be stamped and perforated according to the drawings provided. The invention is made of:
[0000] 69 pound weighted corrugated cardboard; although other weights and type of cardboard and other materials may be used.
BRIEF DESCRIPTION OF THE FIGURES
[0006] FIG. 1 is a front view of the flat rectangular piece of cardboard A, including its dimensions according to a first embodiment of the present invention in the fully open/flat position.
[0007] FIG. 2 is a top view of the flat rectangular piece of cardboard A including dimensions in the fully open/flat position.
[0008] FIG. 3 is the front view of the rectangular piece of cardboard A with the left leaf folded inward. The invention is no longer flat as a portion o the invention has been folded on itself. This figure demonstrates the ability to shape the invention as needed.
[0009] FIG. 4 is a top view of the rectangular piece of cardboard A with the left leaf folded inward.
[0010] FIG. 5 is the front view of the rectangular piece of cardboard A with both the left leaf and the right leaf folded inward. This further demonstrates its capability to be shaped.
[0011] FIG. 6 is the top view of the rectangular piece of cardboard A with both leafs folded inward.
[0012] FIG. 7 is a front view of the rectangular piece of cardboard A in the fully deployed position so it may act as a structurally stable insert for the lawn and garden refuse bag that it will serve. Please note the left and right leafs are at 90 degrees to the main body of the invention.
[0013] FIG. 8 is a top view of the rectangular piece of cardboard A in the fully deployed position so it may act as a structurally stable insert for the lawn and garden refuse bag that it will serve.
[0014] FIG. 9 is a top view of the rectangular piece of cardboard A in the fully deployed position inserted into a standard 34″×16″×12″ lawn and garden refuse bag.
[0000] **Please note that item # 9 on FIG. 9 demonstrates the borders of the lawn and garden refuse bag.**
DETAILED DESCRIPTION
[0015] The present invention provides for a flat, rectangular reusable piece of cardboard A (a.k.a. insert or the insert) to be shaped to fit the inner dimensions of a standard 34″×16″×12″ lawn and garden refuse bag.
[0016] A piece of cardboard may be cut, sized, perforated, stamped and molded for many different, useful purposes. The purpose of this invention is to be cut, sized, perforated and stamped for the purpose of folding it—thus giving it the ability to be shaped—to fit the interior dimensions of a standard 34″×16″×12″ lawn and garden refuse bag. The purpose of this invention is to give structural support to the lawn and garden refuse bag while the lawn and garden refuse bag is being used and utilized in the collection and accumulation of refuse.
[0017] The insert A is made of 69 pound weight corrugated cardboard (although cardboard of other weight and material may also be substituted.) The dimensions of the insert A—in the fully open/flat position is 36″ along the top horizontal edge 3 and 36″ along the bottom horizontal edge 4 . Furthermore it is 32″ along the left outer vertical edge 1 and 32″ along the right outer vertical edge 2 . The insert is ¼″ thick uniformly throughout.
[0018] The insert A contains two (2) perforations 5 and 6 to its rear outer layer allowing for bending, molding and shaping of the insert A to fit the interior dimensions of a standard 34″×16″×12″ lawn and garden refuse bag. The perforations 5 and 6 are both 32″ perforated runs in overall length vertically from the top horizontal edge 3 to the bottom horizontal edge 4 and occur exactly 10.5″ from the entire run of the left outer vertical edge 1 toward the entire run of the vertical midline of the insert A and exactly 10.5′ from the entire run of the right outer vertical edge 2 toward the entire run of the vertical midline of the insert A. The perforations 5 and 6 are parallel to the left outer vertical edge 1 of the insert A and they are parallel to the right outer vertical edge 2 of the insert A and run the entire height (32″) of the insert A. These perforations 5 and 6 segment the insert into 3 distinct regions or areas of the insert A. These regions or areas are referred to on the drawing page as the left leaf B, the right leaf C and the main body D. The area of the insert A from the left outer vertical edge 1 to the left perforation 5 is known as the left leaf B. The size of the area of the left leaf B measures 10.5″×32″. The area of the insert A from the right outer vertical edge 2 to the right perforation 6 is known as the right leaf C. The size of the area of the right leaf C measures 10.5″×32″. The area from the left perforation 5 to the right perforation 6 is known as the main body D. The size of the area of the main body D measures 15″×32″.
[0019] The perforations 5 and 6 do not cut through the insert A completely, rather they score the rear outer layer of the corrugated cardboard thereby allowing bending, molding and shaping of the insert A rather than causing detachment of the two areas known as the left leaf B and right leaf C from the main body D of the insert A.
[0020] As best shown in FIG. 4 , FIG. 6 and FIG. 8 the insert A may be bent, molded or shaped in a variety of ways. As depicted in FIG. 9 , the insert A is fully deployed and is bent, molded and shaped in its intended use position for the purpose of providing stability and structure to the lawn and garden refuse bag as it is being inserted into the interior dimensions of the lawn and garden refuse bag. FIG. 6 best illustrates the insert A fully folded and is best positioned to be initially inserted into the inner dimensions of the lawn and garden refuse bag prior to the full deployment of the insert A for which its purpose is intended.
[0021] The insert A has two (2) stamped out areas 7 and 8 . The stamped out areas 7 and 8 are portions of the corrugated cardboard insert A that have been fully cut through both front and rear outer layers of the insert A and removed from the overall area of the insert A. The cardboard that has been removed is no longer a part of the insert A or the invention. The purpose of the stamped out areas 7 and 8 are to serve as hand holds for the ease of moving, folding, carrying, removing or in general handling the insert A whether during use or in storing the insert A away for storage. The stamped out areas 7 and 8 are located on both the left leaf B and the right leaf C (one (1) stamped out area per leaf B and C.) The positioning of the stamped out areas 7 and 8 are as follows:
[0022] The left leaf B stamped out area 7 has the overall dimension of 2″×5.5″. The left leaf B stamped out area 7 has two (2) horizontal borders that allow the cardboard cutout. The superior horizontal border of the stamped out area 7 of the left leaf B is 3″ inferior of the top horizontal edge 3 as well as 29″ superior of the bottom horizontal edge 4 . The inferior horizontal border of the stamped out area 7 of the left leaf B is 5″ inferior to the top horizontal edge 3 as well as 27″ superior to the bottom horizontal edge 4 . The left leaf B stamped out area 7 has two (2) vertical borders that allow the cardboard cutout of the stamped out area 7 . The left vertical border of the stamped out area 7 of the left leaf B is 2.5″ medial to the left outer vertical edge 1 as well as 8″ lateral of the left perforation 5 . The right vertical border of the stamped out area 7 of the left leaf B is 2.5″ lateral to the left perforation 5 as well as 8″ medial to the left outer vertical edge 1 .
[0023] The right leaf C stamped out area 8 has the overall dimension of 2″×5.5″. The right leaf B stamped out area 8 has two (2) horizontal borders that allow the cardboard cutout. The superior horizontal border of the stamped area 8 of the right leaf C is 3″ inferior of the top horizontal edge 3 as well as 29″ superior of the bottom horizontal edge 4 . The inferior horizontal border of the stamped out area 8 of the right leaf C is 5″ inferior to the top horizontal edge 3 as well as 27″ superior to the bottom horizontal edge 4 . The right leaf C stamped out area 8 has two (2) vertical borders that allow the cardboard cutout. The right vertical border of the stamped out area 8 of the right leaf C is 2.5″ medial to the right outer vertical edge 2 as well as 8″ lateral of the right perforation 6 . The left vertical border of the stamped out area 8 of the right leaf C is 2.5″ lateral to the right perforation 6 as well as 8″ medial to the right outer vertical edge 2 .
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A flat rectangular, reusable piece of cardboard having dimensions of (32″×36″×¼″) with two (2) vertical perforations, and two (2) stamped out areas for hand holds. This flat, rectangular, reusable piece of cardboard may be shaped to fit the inner dimensions of a standard (34″×16″×12″) lawn and garden refuse bag for the purpose of providing said lawn and garden refuse bag with sufficient support to hold it in the fully open and usable position, preventing lawn and garden refuse bag from collapsing during use.
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RELATED APPLICATIONS
[0001] This application claims priority from Indian Application 1650/CHE/2010 filed on Jun. 14, 2010.
FIELD OF THE INVENTION
[0002] The present invention relates to a solid dosage form comprising fenofibrate. The present invention also relates to a process for preparation of solid dosage form comprising fenofibrate.
BACKGROUND OF THE INVENTION
[0003] Fenofibrate is a lipid regulating agent, chemically known as 2-[4-(4-chlorobenzoyl) phenoxy]-2-methyl-propanoic acid, 1-methylethyl ester and is disclosed in U.S. Pat. No. 4,058,552. Fenofibrate is currently marketed in the United States under the tradenames TRICOR®, FENOGLIDE® and TRIGLIDE® in the form of tablets and with the tradenames ANTARA® and LIPOFEN® in the form of capsules.
[0004] Bioavailability is the degree to which a drug becomes available to the target tissue after administration. Many factors can affect bioavailability including the dosage form and various properties, e.g., dissolution rate of the drug. Poor bioavailability is a significant problem encountered in the development of pharmaceutical compositions, particularly those containing an active ingredient that is poorly soluble in water. Poorly water soluble drugs, those having solubility less than about 10 mg/ml, tend to be eliminated from the gastrointestinal tract before being absorbed into the circulation.
[0005] The solubility of an active pharmaceutical ingredient influences the bioavailability of the drug. Fenofibrate is a poorly soluble drug. Due to its poor hydrosolubility, fenofibrate poses problem of low dissolution. It is also poorly absorbed in the digestive tract and consequently its bioavailability is incomplete and irregular. Clearly, there is a need for improved compositions in which the fenofibrate exhibits better dissolution properties.
[0006] There are several prior art references which discloses various attempts to improve the solubility of fenofibrate.
[0007] U.S. Pat. No. 4,800,079 and U.S. Pat. No. 4,961,890 discloses granules with controlled release of fenofibrate, each granule comprising an inert core, a layer based on fenofibrate and a protective layer, wherein the improvement comprises the layer based on fenofibrate containing the fenofibrate in the form of crystalline microparticles of dimensions not greater than 30 microns, said microparticles being included in the pores of an inert matrix soluble in water.
[0008] U.S. Pat. No. 4,895,726 discloses a composition containing a co-micronized mixture of particles of fenofibrate and a solid surfactant, wherein the mean particle size of said co-micronized mixture is less than 15 μm.
[0009] U.S. Pat. No. 5,145,684 discloses particles consisting essentially of a crystalline drug substance having a solubility in water of less than 10 mg/ml, said drug substance having a non-crosslinked surface modifier adsorbed on the surface thereof in an amount sufficient to maintain an effective average particle size of less than about 400 nm.
[0010] U.S. Pat. No. 6,027,747 discloses a solid dispersion comprising fenofibrate in a hydrophilic polymer and a surfactant prepared by co-precipitation.
[0011] U.S. Pat. No. 6,074,670, U.S. Pat. No. 6,596,317 and U.S. Pat. No. 7,037,529 discloses fenofibrate composition comprising inert hydrosoluble carrier covered with at least one layer containing a fenofibrate active ingredient in a micronized form having a size less than 20 μm, a hydrophilic polymer and, optionally, a surfactant and further processing them into a suitable dosage form.
[0012] U.S. Pat. No. 6,375,986 discloses solid dose nanoparticulate composition comprising at least one poorly soluble active agent, at least one polymeric surface stabilizer adsorbed to the surface of the drug, DOSS, and a pharmaceutically acceptable carrier, as well as any desired excipients. The patent further discloses the use of solid dose nanoparticulate composition for the preparation of suitable dosage form.
[0013] U.S. Pat. No. 6,696,084 discloses a process for the preparation of small particles or microparticles containing fenofibrate and a phospholipid surface stabilizing substance comprising the steps of: a) mixing at high shear an admixture of fenofibrate and a phospholipid in an aqueous carrier in the absence of an organic solvent within a temperature range at or above the melting point of the fenofibrate to form a heated suspension containing the fenofibrate, then b) homogenizing said heated suspension in a pressure range and within said temperature range to form a heated homogenate containing the fenofibrate then c) spray drying the heated homogenate to form dried small particles.
[0014] U.S. Pat. No. 6,180,138 discloses a process for preparing a dosage form comprising the steps of premixing the lipid-regulating agent with an excipient, micronizing the powdered mixture, suspending the micronized powdered mixture in a surfactant solution, drying the mixture, wet or dry granulating the mixture, and optionally forming a finished oral dosage form of the resulting formulation.
[0015] U.S. Pat. No. 6,368,622 discloses a process for preparing a solid formulation comprising the steps of forming a mixture of the lipid-regulating agent with a solid surfactant, and granulating the mixture by melting, mixing, and congealing, then optionally forming a finished dosage form.
[0016] U.S. Pat. No. 6,383,517 discloses a process for preparing a solid formulation comprising the steps of dissolving the lipid-regulating agent in a surfactant solution, premixing an excipient, wet granulating the lipid-regulating agent/surfactant solution and the premix, drying the resulting mixture, and optionally sizing the dried granules and forming a finished dosage form.
[0017] U.S. Pat. No. 6,444,225 discloses a process of making a composition comprising a solid dispersion of a disintegrant dispersed in fenofibrate, which comprises the steps of melting the fenofibrate, blending the disintegrant into the molten fenofibrate, and solidifying the mixture.
[0018] U.S. Pat. No. 6,465,011 discloses a solid formulation comprising the lipid-regulating agent dispersed in a hydrophilic, amorphous polymer in which said lipid-regulating agent is present as a metastable, amorphous phase.
[0019] U.S. Pat. No. 6,531,158 discloses a drug delivery system comprising micronized fenofibrate and an inert substrate of suitable particle size, selected from microcrystalline cellulose or lactose, which when orally administered as a single 67 mg dose in adults maintains post ingestion blood plasma levels of fenofibric acid of: at least about 100 mg/ml at one hour; at least about 350 mg/ml at two hours; at least about 750 mg/ml at four hours; at least about 850 mg/ml at five hours; and at least about 650 mg/ml at twenty-four hours.
[0020] U.S. Pat. No. 6,555,135 discloses a composition comprising a comicronized mixture of fenofibrate, and a solid non-toxic amount of a pharmaceutically acceptable excipient having no therapeutic activity that is not a surfactant.
[0021] U.S. Pat. No. 7,101,574 discloses a pharmaceutical composition in the form of granules, wherein each granule comprises a neutral microgranule on which is a composition comprising: micronized fenofibrate, a surfactant, and a binding cellulose derivative as a solubilization adjuvant.
[0022] U.S. Pat. No. 7,255,877 discloses a method of preparing fenofibrate microparticles, comprising the steps of: (1) mixing the fenofibrate particles with (a) a natural or synthetic phospholipid and (b) at least one non-ionic, anionic, or cationic surfactant to form a mixture, prior to or during a reduction of particle size, and (2) subjecting the mixture of step (1) to size reduction by an energy input procedure selected from one or more of sonication, milling, homogenization, microfluidization, or precipitation from solution using antisolvent and solvent precipitation in the presence of the mixture to produce fenofibrate microparticles having a volume-weighted mean particle size that is about 50% smaller than particles produced without the presence of the surfactant using the same energy input procedure.
[0023] U.S. Pat. No. 7,276,249 and U.S. Pat. No. 7,320,802 discloses a composition comprising nanoparticulate fibrate, preferably fenofibrate particles have an effective average particle size of less than about 500 nm and at least one surface stabilizer adsorbed on the surface of the fibrate particles.
[0024] U.S. Pat. No. 7,927,627 discloses a nanoparticulate fibrate composition comprising: (a) particles of a fibrate or a salt thereof having an effective average particle size of less than about 2000 nm; and (b) associated with the surface thereof hypromellose, dioctyl sodium sulfosuccinate, and sodium lauryl sulfate as surface stabilizers; wherein the composition is phospholipid-free.
[0025] US 2003/0224059 a drug delivery vehicle comprising at least one pharmaceutical carrier bearing microparticle of a drug, wherein the microparticles have a mean particle size of about 100 nm to about 10 μm.
[0026] US 2004/0115264 discloses fenofibrate tablet, characterized in that it is obtained by compressing a mixture comprising: a) granules containing: 1 to 5% of a surfactant; micronized fenofibrate; and at least one solid excipient selected from starch, cellulose and derivatives thereof, with the exception of C 12 disaccharides, said granules being obtained by granulating the mixture with the aid of an aqueous solution of polyvinylpyrrolidone; b) crosslinked polyvinylpyrrolidone; and c) optionally flow aids or lubricants, the amount of fenofibrate being greater than 50% by weight, expressed relative to the weight of the tablet.
[0027] US 2005/0112192 and US 2006/0177512 discloses a process for preparing a drug formulation comprising the steps of: dissolving a lipid-regulating drug in a solvent free of surfactant to form a drug solution; premixing an excipient to generate an admixture; wet granulating the admixture and the drug solution to form a granulated drug admixture; and drying the granulated admixture.
[0028] US 2006/0177499 discloses a dry granulation process for preparing composition comprising co-micronised mixture of fenofibrate and solid surfactant.
[0029] US 2007/0014853 discloses a dosage form comprising a granulate, wherein the granulate comprises an active pharmaceutical ingredient having a poor water solubility intimately associated with at least one pharmaceutically acceptable sugar, and wherein when the active pharmaceutical ingredient is fenofibrate, the at least one acceptable sugar is not lactose.
[0030] US 2007/0048384 discloses a composition comprising at least one active agent, at least one pharmaceutically acceptable surfactant and at least one pharmaceutically acceptable polymer, wherein the active agent is primarily amorphous fenofibrate.
[0031] US 2007/0148245 discloses a process for making a pharmaceutical composition of a drug having low aqueous solubility, the process comprising (a) fixing the drug in a strong matrix comprising at least one at least partially amorphous sugar to obtain a sugar-drug matrix; and (b) milling the sugar-drug matrix to obtain a milled sugar-drug matrix as the pharmaceutical composition, the composition being optionally further processed into a pharmaceutical formulation.
[0032] US 2008/0050450 discloses a composition comprising fenofibrate nanoparticles having an effective average particle size of less than 2000 nm, and a particle sequestrant.
[0033] US 2008/0095838 discloses a solid pharmaceutical composition for oral administration; which comprises, within one and the same phase: at least one solid and micronized lipophilic active principle, at least one surfactant, at least one cationic polymer insoluble in water at pH greater than or equal to 5, and at least one organic or inorganic acid.
[0034] US 2009/0202649 discloses formulation comprising a dispersion containing fenofibrate and at least one surfactant, optionally combined with one or more solid organic or inorganic excipients. The patent publication also discloses formulations of fenofibrate prepared by spray drying an emulsion comprising fenofibrate, at least one hydrophilic polymer and at least one surfactant onto inert substrate cores, or optionally collecting spray dried solid to obtain a pharmaceutical composition.
[0035] US 2010/0151037 discloses a composition comprising nanoparticles of fibrate, surfactant, co-surfactant, bulking agent and water and further discloses a method for the preparation of nanoparticles of a poorly water soluble drug.
[0036] US 2010/0166857 discloses a solid dispersion comprising: a plurality of coated particles comprising inert particles with a coating, wherein the coating comprises fenofibrate dispersed in a hydrophilic polymer, and wherein the inert particles comprise nonpareils; and a plurality of granules comprising micronized fenofibrate with at least one pharmaceutically acceptable excipient.
[0037] US 2011/0020455 discloses a solid dispersion comprising an active ingredient having a low solubility in water and a powdery porous carrier impregnated with and supporting the active ingredient, wherein the porous carrier comprises a porous silicon-containing carrier having a heating loss of not more than 4% by weight at a temperature of 950° C. for 2 hours.
[0038] EP 0 793 958 B1 discloses a process for the preparation of fenofibrate preparation using fenofibrate, surface-active agents and polyvinyl pyrrolidone and optionally one or more further auxiliary or auxiliaries and using mixing and granulation and subsequent drying, characterized in that firstly fenofibrate particles are mixed with polyvinylpyrrolidone particles and crosslinked polyvinylpyrrolidone particles and optionally further auxiliary particles, and the resultant mixture is then granulated with an aqueous solution of one or more surface-active agent(s) in a proportion of at least 1.5% by weight, based on the dry granules to be produced and the granules are dried.
[0039] WO 00/16749 discloses a method for preparing novel galenic formulations for providing fenofibrate with enhanced bioavailability when it is orally absorbed, and consisting in: (a) micronizing fenofibrate; (b) granulating the fenofibrate in the presence of a liquid medium comprising a surfactant, water and water-miscible alcohol; and (c) drying the resulting granular material.
[0040] WO 01/34119 discloses a solid dispersion formulation comprising a pharmaceutical compound, a water soluble carrier, such as polyethylene glycol (PEG), and a crystallization inhibitor, such as polyvinylpyrrolidone (PVP) or hydroxypropyl methylcellulose (HPMC).
[0041] WO 2004/028506 discloses an immediate release composition comprising an inert hydro-insoluble carrier with at least one layer containing fenofibrate in a micronized form, a hydrophilic polymer and a surfactant; and optionally one or several outer phases or layers.
[0042] WO 2008/016260 discloses solid dispersion comprising an amorphous fenofibrate dispersed in a water-soluble polymer.
[0043] WO 2008/075320 discloses a process for preparing a composition comprising fenofibrate, wherein the process comprises the steps of: (i) preparing a solution comprising fenofibrate, a surfactant and a hydrophilic polymer, (ii) homogenizing the solution of step (i) with one or more solvents, (iii) spraying the homogenized solution of step (ii) over one or more inert carriers, (iv) drying the granules of step (iii) and blending with one or more pharmaceutically acceptable excipients, (v) compressing the mixture of step (iv) into tablets or filling into capsules.
[0044] WO 2008/104846 discloses composition comprising unmicronized fenofibrate or a salt thereof in admixture with one or more wetting agents and one or more pharmaceutically acceptable excipients, wherein the admixture is not co-micronized before processing.
[0045] WO 2008/104852 discloses a composition comprising fenofibrate adsorbed on a pharmaceutically acceptable adsorbent optionally, along with one or more pharmaceutically acceptable excipients.
[0046] WO 2008/110534 discloses a process for the preparation of a pharmaceutical composition containing poorly soluble drug comprising the steps of: a) dissolving the drug, or a pharmaceutically acceptable salt thereof, and at least one polymer in a suitable solvent, to form a solution; b) spraying the solution onto inert pellets; and c) drying the inert pellets to remove the solvent.
[0047] WO 2009/016608 discloses composition comprising non-micronised fenofibrate and one or more pharmaceutically acceptable vehicles comprising one or more of polyethylene glycol or derivatives thereof, poloxamer, Cremophore RH 40 and vitamin E. The patent publication further discloses composition comprising non-micronized fenofibrate and cyclodextrin.
[0048] WO 2010/033179 discloses granule for a pharmaceutical composition, comprising a core, which comprises at least one active pharmaceutical ingredient intimately associated with at least one hydrophilic polymer, wherein the active pharmaceutical ingredient has a solubility in water of less than about 1 mg/ml.
[0049] WO 2010/075065 discloses a method of making microparticles comprising: (a) dissolving, melting, or suspending at least one water-insoluble active agent in at least one fatty acid or conjugated fatty acid, surfactant, hydrophilic polymer, or combinations thereof to form a mixture, and (b) mixing the mixture of step (a) with a hydrophilic or lipophilic carrier to form microparticles.
[0050] WO 2010/081623 discloses an aqueous suspension comprising crystalline fenofibrate or fenofibric acid having an average particle size of D(50) less than 250 nm, cellulose derivative, solubilizing adjuvant and a surfactant.
[0051] WO 2010/115886 discloses an adsorbate comprising an active pharmaceutical ingredient (API) being practically insoluble in water associated with a particulate and/or porous carrier, wherein the adsorbate is prepared by using a non-polar solvent or a mixture of non-polar solvents, and wherein essentially no API is in the form of precipitates, particles or crystals.
[0052] WO 2010/146606 discloses a stable nanodispersion comprising nanoparticles having a mean size less than 300 nm dispersed in a vehicle comprising a water miscible solvent and water, said nanoparticles comprising one or more drugs having a polymer and a surfactant comprising a mixture of fatty acids or its salts and sterol or its derivatives or its salts.
[0053] IN 770/MUM/2007 discloses an immediate release composition comprising an inert core with at least one layer containing fenofibrate in non-micronized form in admixture with pharmaceutically acceptable excipients and optionally one or more layers.
[0054] IN 599/MUM/2008 discloses a composition comprising micronized fenofibrate, one or more surfactants other than dioctylsulfosuccinate along with pharmaceutically acceptable excipients.
[0055] IN 1384/MUM/2008 discloses a formulation of fenofibrate with enhanced oral bioavailability, simplicity of design and manufacture and absence of food effect. The formulation comprises fenofibrate dissolved in a lipophilic surfactant, with a hydrophilic surfactant optionally added.
[0056] IN 1820/DEL/2009 discloses a fenofibrate composition in the form of capsules or tablets, comprising fenofibrate, surfactant, hydrophilic polymer and anti-foaming agents.
[0057] IN 1888/CHE/2009 discloses a pharmaceutical composition comprising a high drug load of fenofibrate, wherein the fenofibrate is present in more than 70% by weight of total composition and further discloses a process for preparing fenofibrate composition using extrusion process.
[0058] The above prior art references disclose various approaches to improve the solubility as well as bioavailability of fenofibrate. Still, there exists a need for improved formulations in which the fenofibrate exhibits better dissolution properties. The inventors of the present invention have developed a solid dosage form comprising fenofibrate which increases the rate of dissolution of fenofibrate as well as its bioavailability.
OBJECTIVE OF THE INVENTION
[0059] The main objective of the present invention is to provide a solid dosage form comprising fenofibrate and one or more pharmaceutically acceptable excipients.
[0060] Another objective of the present invention is to provide a process for the preparation of solid dosage form comprising fenofibrate having better dissolution properties, content uniformity and equivalent bioavailability w.r.t commercialized fenofibrate dosage form.
SUMMARY OF THE INVENTION
[0061] The present invention relates to a solid dosage form comprising:
a) tablet core comprising one or more pharmaceutically acceptable excipients, b) a layer surrounding the tablet core comprising fenofibrate and one or more pharmaceutically acceptable excipients, and c) optionally a film coating.
[0065] The present invention further relates to a solid dosage form comprising:
a) tablet core comprising one or more pharmaceutically acceptable excipients, b) a layer surrounding the tablet core comprising fenofibrate, hydrophilic polymer/s, a hydrophilic carrier, optionally one or more surfactants and one or more pharmaceutically acceptable excipients, and c) optionally a film coating.
[0069] The present invention further relates to a solid dosage form comprising fenofibrate prepared by the process comprising the steps of
a) preparing a tablet core, b) preparing dispersion of fenofibrate in a suitable solvent, c) coating the tablet core with fenofibrate dispersion, and d) optionally film coating the coated tablet.
DETAILED DESCRIPTION OF THE INVENTION
[0074] The present invention relates to a solid dosage form comprising fenofibrate and one or more pharmaceutically acceptable excipients.
[0075] The present invention relates to a solid dosage form comprising:
a) tablet core comprising one or more pharmaceutically acceptable excipients, b) a layer surrounding the tablet core comprising fenofibrate and one or more pharmaceutically acceptable excipients, and c) optionally a film coating.
[0079] The present invention further relates to a solid dosage form comprising:
a) tablet core comprising one or more pharmaceutically acceptable excipients, b) a layer surrounding the tablet core comprising fenofibrate, hydrophilic polymer and one or more pharmaceutically acceptable excipients, and c) optionally a film coating.
[0083] The present invention further relates to a solid dosage form comprising:
a) tablet core comprising one or more pharmaceutically acceptable excipients, b) a layer surrounding the tablet core comprising fenofibrate, hydrophilic polymer, a hydrophilic carrier, optionally one or more surfactants and one or more pharmaceutically acceptable excipients, and c) optionally a film coating.
[0087] The present invention further relates to a solid dosage form comprising:
a) tablet core comprising one or more pharmaceutically acceptable excipients, b) a layer surrounding the tablet core comprising fenofibrate, hydrophilic polymer, a hydrophilic carrier, surfactants and one or more pharmaceutically acceptable excipients, and c) a film coating.
[0091] “Tablet core” according to the present invention may be an inert tablet core comprising one or more pharmaceutically acceptable excipients. The tablet core may further contain fenofibrate along with one or more pharmaceutically acceptable excipients.
[0092] “Fenofibrate” according to the present invention includes, but not limited to, fenofibrate free base, its pharmaceutical acceptable salts, esters, ethers, solvates, hydrates, polymorphs and the like. Fenofibrate may be used in the range of 1-70% by weight of the composition.
[0093] “Pharmaceutically acceptable excipient/s” are the components added to pharmaceutical formulation to facilitate manufacture, enhance stability, control release, enhance product characteristics, enhance bioavailability, enhance patient acceptability, etc. Pharmaceutically acceptable excipients includes, but not limited to, diluents/fillers, binders, disintegrants, sugars, lubricants, glidants, compression aids, colors, sweeteners, preservatives, surfactants, phospholipids, suspending agents, dispersing agents, film formers, flavors, printing inks, etc.
[0094] Binders hold the ingredients in the composition together. Exemplary binders include, but not limited to, cellulose and its derivatives including, ethyl cellulose, hydroxypropyl cellulose, hydroxypropyl methylcellulose, methylcellulose and hydroxyethyl cellulose, carboxymethyl cellulose; starch and its derivatives; hydrocolloids; sugars; polyvinyl pyrrolidone and combinations comprising one or more of the foregoing binders. The binder may be used in the range of 1-15% by weight of the composition.
[0095] Diluents increase the bulk of the composition. Diluents according to the present invention include, but not limited to, sugars such as lactose, sucrose, dextrose; sugar alcohols such as mannitol, sorbitol, xylitol, lactitol; Starlac® (co-processed mixture of Starch and lactose), Microcelac® (co-processed mixture of microcrystalline cellulose and lactose), starch, modified starches, pregelatinized starch, dibasic calcium phosphate, tribasic calcium phosphate, powdered cellulose, microcrystalline cellulose, silicified microcrystalline cellulose and the like or combinations thereof. The diluent may be used in the range of 5-80% by weight of the composition.
[0096] Disintegrants according to the present invention include, but not limited to, water swellable substances, for example, cellulose and its derivatives including low-substituted hydroxypropyl cellulose; cross-linked polyvinylpyrrolidone; cross-linked sodium carboxymethylcellulose, sodium carboxy methylcellulose, microcrystalline cellulose; sodium starch glycolate; ion-exchange resins; starch and modified starches including pregelatinized starch; formalin-casein; and combinations comprising one or more of the foregoing water swellable substances. The disintegrant may be used in the range of 1-20% by weight of the composition.
[0097] Lubricants and glidants aids in the processing of powder materials. Exemplary lubricants include, but not limited to, calcium stearate, glycerol behenate, magnesium stearate, mineral oil, polyethylene glycol, sodium stearyl fumarate, stearic acid, talc, vegetable oil, zinc stearate, and combinations comprising one or more of the foregoing lubricants. Exemplary glidants include, but not limited to, talc, silicon dioxide, cornstarch and the like. The lubricant may be used in the range of 0.1-5% by weight of the composition.
[0098] Surfactants are compounds which are capable of improving the wetting of the drug and/or enhancing the dissolution. The surfactants can be selected from hydrophilic surfactants or lipophilic surfactants or mixtures thereof. The surfactants can be anionic, nonionic, cationic, and zwitterionic surfactants. Surfactants according to the present invention include, but not limited to, polyoxyethylene alkylaryl ethers such as polyoxyethylene lauryl ether, polyoxyethylene cetyl ether, polyoxyethylene stearyl ether; polyethylene glycol fatty acid esters such as PEG monolaurate, PEG dilaurate, PEG distearate, PEG dioleate; polyoxyethylene sorbitan fatty acid ester such as polysorbate 40, polysorbate 60, polysorbate 80; sorbitan fatty acid mono esters such as sorbitan monolaurate, sorbitan monooleate, sorbitan sesquioleate, sorbitan trioleate, polyoxyethylene castor oil derivates such as polyoxyl castor oil, polyoxyl hydrogenated castor oil, sodium lauryl sulphate, monooleate, monolaurate, monopalmitate, monostearate, sodium dioctyl sulfosuccinate (DOSS), lecithin, stearylic alcohol, cetostearylic alcohol, cholesterol, polyoxyethylene ricin oil, polyoxyethylene fatty acid glycerides, poloxamer, cremophore RH 40, and the like or combinations thereof. The surfactant may be used in the range of 0.0001-10% by weight of the composition.
[0099] Phospholipids according to the present invention include, but not limited to, phosphatidylcholine, phosphatidylethanolamine, phosphatidylserine, phosphatidylinositol, phosphatidylglycerol, phosphatidic acid, lysophospholipids, sphingomyelin, egg or soybean phospholipid, lecithin or combination thereof. The phospholipid may be used in the range of 0-5% by weight of the composition.
[0100] The expression “hydrophilic polymer” in the invention should be taken to mean any high molecular weight substance (greater, for example, than 300) having sufficient affinity towards water to dissolve therein or to form a gel. Examples of such polymers include, but not limited to, polyvinylpyrrolidone, copovidone, poly(vinyl alcohol), hydroxypropyl cellulose, hydroxyethyl cellulose, hydroxymethyl cellulose, hydroxypropyl methylcellulose, gelatin and the like or combinations thereof. The hydrophilic carrier may be used in the range of 0.1-20% by weight of the composition.
[0101] “Hydrophilic carrier” according to the present invention means, but not limited to, any excipient, generally hydrophilic, pharmaceutically inert, crystalline or amorphous. Examples of such excipients are derivatives of sugars, such as lactose, saccharose, sucrose, mannitol, sorbitol, cellulose and its derivatives, inorganic salts, starch or hydrolyzed starch (maltodextrin), or the like and mixtures thereof. The hydrophilic carrier may be used in the range of 5-80% by weight of the composition.
[0102] Suitable sugars according to the present invention include, but not limited to, one or more of sucrose, glucose, fructose, galactose, maltose, isomaltose, cellobiose, melibiose, gentiobiose, lactose, sorbitol, mannitol, xylitol, lactitol and the like or combinations thereof.
[0103] The tablet core according to the present invention may be prepared by any method known in the art such as wet granulation, dry granulation or direct compression of the pharmaceutically acceptable excipients. Preferably the tablet core is prepared by direct compression.
[0104] The present invention further relates to a solid dosage form comprising fenofibrate prepared by the process comprising the steps of:
a) preparing a tablet core, b) preparing dispersion of fenofibrate in a suitable solvent, c) coating the tablet core with fenofibrate dispersion, and d) optionally film coating the coated tablet.
[0109] The present invention further relates to a solid dosage form comprising fenofibrate prepared by the process comprising the steps of:
a) preparing a tablet core, b) preparing dispersion of fenofibrate along with one or more pharmaceutically acceptable excipients in a suitable solvent, c) coating the tablets with fenofibrate dispersion, and d) filling the tablets in the hard gelatin capsules.
[0114] The present invention further relates to a solid dosage form comprising fenofibrate prepared by the process comprising the steps of:
a) preparing a tablet core, b) preparing dispersion of fenofibrate along with one or more pharmaceutically acceptable excipients in a suitable solvent, c) coating the tablets with fenofibrate dispersion, and d) optionally film coating the coated tablet.
[0119] The present invention further relates to a solid dosage form comprising fenofibrate prepared by the process comprising the steps of:
a) blending one or more pharmaceutically acceptable excipients, b) compressing the blend of step (a) into a tablet, c) dispersing fenofibrate and hydrophilic polymer in a suitable solvent, d) coating the tablets of step (b) with fenofibrate dispersion of step (c), and e) optionally film coating the coated tablet
[0125] The present invention further relates to a solid dosage form comprising fenofibrate prepared by the process comprising the steps of:
a) blending one or more pharmaceutically acceptable excipients, b) compressing the blend of step (a) into a tablet, c) dispersing fenofibrate, hydrophilic polymer and a hydrophilic carrier in a suitable solvent, d) coating the tablets of step (b) with fenofibrate dispersion of step (c), and e) optionally film coating the coated tablet.
[0131] The present invention further relates to a solid dosage form comprising fenofibrate prepared by the process comprising the steps of:
a) blending one or more pharmaceutically acceptable excipients, b) compressing the blend of step (a) into tablet, c) dispersing fenofibrate and hydrophilic polymer in a suitable solvent, d) milling the fenofibrate dispersion, e) dissolving sugar in the dispersion of step (d), f) coating the tablets of step (b) with fenofibrate dispersion of step (e), and g) optionally film coating the coated tablet.
[0139] Dosage form according to the present invention can be selected from the group comprising tablets, capsules, minitablets or the like or combinations thereof.
[0140] “Suitable solvent” according to the present invention can be any solvent wherein the drug can be either dissolved or dispersed such as isopropyl alcohol, ethanol, water, acetone, methylene chloride and the like or mixtures thereof.
[0141] “Dispersion” according to the present invention can be microdispersion or nanodispersion. The dispersion can be prepared and milled by methods known in the art.
[0142] Film coating composition includes one or more polymeric carriers along with one or more pharmaceutically acceptable excipients such as plasticisers, opacifier, anti-sticking agent, colorants, sugars, pore forming agent, surfactants and the like. More particularly the film coating is Opadry.
[0143] Suitable film coating polymers according to the present invention include, but not limited to, ethyl cellulose, hydroxypropyl cellulose, hydroxypropyl methylcellulose, hydroxyethyl cellulose, polyvinylpyrrolidone, polyvinyl alcohol, polyethylene oxide and the like or combinations thereof.
[0144] Suitable plasticizers according to the present invention include, but not limited to, polyethylene glycol, acetyl triethyl citrate, acetyl tributyl citrate, triethyl citrate, acetylated monoglycerides, glycerol, triacetin, propylene glycol, dibutyl phthalate, diethyl phthalate, isopropyl phthalate, dimethyl phthalate, dactyl phthalate, dibutyl sebacate, dimethyl sebacate, castor oil, glycerol monostearate, fractionated coconut oil and the like or combinations thereof.
[0145] Suitable opacifiers according to the present invention include, but not limited to, water insoluble pigments comprising titanium dioxide, calcium carbonate, calcium sulfate, magnesium oxide, magnesium carbonate, aluminum silicate, aluminum hydroxide, talc, iron oxide and the like or combinations thereof.
[0146] Suitable colorants include water soluble dyes, water insoluble pigments and natural colorants.
[0147] Suitable anti-sticking agents used according to the present invention are selected from talc, magnesium stearate and the like or a mixture thereof.
[0148] In another embodiment of the present invention, the weight of the tablet core may be in the range of 50 mg to about 1000 mg.
[0149] In another embodiment, the particle size of fenofibrate is in the range of about 10 nm to about 200 microns, preferably in the range of about 100 nm to about 100 microns and more preferably in the range of about 100 nm to about 1 microns.
[0150] In yet another embodiment, the amount of fenofibrate used may be in the range of about 10 to about 300 mg.
[0151] In another preferred embodiment of the present invention, the solid dosage form comprises:
a) tablet core comprising 30-50% w/w of lactose, 1-20% w/w of crospovidone, 30-50% w/w of silicified microcrystalline cellulose, 0.0001-10% w/w of sodium lauryl sulphate and 0.1-5% w/w of magnesium stearate, b) a layer surrounding the tablet core comprising 1-70% w/w of fenofibrate, 1-20% w/w of hydroxypropyl methylcellulose, 0-5% w/w of lecithin and 5-30% w/w of sucrose, and, c) film coating over the coated tablet,
wherein the % w/w is based on total weight of the dosage form.
[0155] In another preferred embodiment, the solid dosage form comprising fenofibrate is prepared by a process comprising the steps of:
a) blending lactose, sodium lauryl sulphate, crospovidone and silicified microcrystalline cellulose, b) lubricating the blend of step (a) with magnesium stearate, c) compressing the blend of step (b) into tablet, d) dispersing fenofibrate and hydroxypropyl methylcellulose in purified water and stirring to get uniform dispersion, e) milling the fenofibrate dispersion to get fenofibrate having an average particle size above 600 nm, f) dissolving sucrose and/or lecithin in the dispersion of step (e), g) coating the tablets of step (c) with fenofibrate dispersion of step (f), and h) applying a film coating over the coated tablets of step (g).
[0164] The following examples further exemplify the invention and are not intended to limit the scope of the invention. It is obvious to those skilled in the art to find out the composition for other dosage forms and substitute the equivalent excipients as described in this specification or with the one known to the industry.
Example 1
[0165]
[0000]
S. No
Ingredients
mg/tablet
Inert Tablet Core
1
Lactose
258.95
2
Sodium lauryl sulfate
10.57
3
Crospovidone
13.05
4
Silicified microcrystalline cellulose
151.65
5
Magnesium stearate
0.91
Drug nano-dispersion coating
6
Fenofibrate
145
7
Hydroxypropyl methylcellulose
14.5
8
Sucrose
145
9
Purified water
q.s
Drug loaded tablet weight
739.5
Film coating
10
Opadry
15
11
Purified water
q.s
Film coated tablet weight
754.5
[0166] The processing steps involved in manufacturing fenofibrate tablets are given below:
i) lactose, sodium lauryl sulphate, crospovidone and silicified microcrystalline cellulose were sifted separately and blended, ii) the blend of step (i) was lubricated with magnesium stearate and iii) the lubricated blend of step (ii) was compressed into tablets, iv) fenofibrate and hydroxypropyl methylcellulose were dispersed in water and stirred to get a uniform dispersion, v) the dispersion of step (iv) was nanonized to get fenofibrate having an average particle size above 600 nm, vi) sucrose was added to the nanodispersion of step (v), vii) the tablets prepared in step (iii) were coated with nanodispersion of step (vi) and dried, and viii) the coated tablets obtained in step (vii) were coated with Opadry coating.
Example 2
[0175]
[0000]
S. No
Ingredients
mg/tablet
Inert Tablet Core
1
Lactose
229.39
2
Sodium lauryl sulfate
40.00
3
Crospovidone
13.05
4
Silicified microcrystalline cellulose
151.65
5
Magnesium stearate
0.91
Drug nano-dispersion coating
6
Fenofibrate
145
7
Hydroxypropyl methylcellulose
14.5
8
Sucrose
145
9
Purified water
q.s
Drug loaded tablet weight
739.5
Film coating
10
Opadry
15
11
Purified water
q.s
Film coated tablet weight
754.5
Example 3
[0176]
[0000]
S. No
Ingredients
mg/tablet
Inert Tablet Core
1
Lactose
223.10
2
Sodium lauryl sulfate
40.00
3
Crospovidone
20.00
4
Silicified microcrystalline cellulose
151.00
5
Magnesium stearate
0.90
Drug nano-dispersion coating
6
Fenofibrate
145
7
Hydroxypropyl methylcellulose
14.5
8
Sucrose
145
9
Purified water
q.s
Drug loaded tablet weight
739.5
Film coating
10
Opadry
15
11
Purified water
q.s
Film coated tablet weight
754.5
Example 4
[0177]
[0000]
S. No
Ingredients
mg/tablet
Inert Tablet Core
1
Lactose
258.82
2
Sodium lauryl sulphate
10.57
3
Crospovidone
13.05
4
Silicified microcrystalline cellulose
151.65
5
Magnesium stearate
0.91
Drug nano-dispersion coating
6
Fenofibrate
145.00
7
Hydroxypropyl methylcellulose
14.50
8
Sucrose
145.00
9
Lecithin
1.00
10
Purified water
q s
Drug loaded tablet weight
740.5
Film coating
11
Instacoat
15.50
12
Purified water
q s
Film coated tablet weight
756.00
Example 5
[0178]
[0000]
S. No
Ingredients
mg/tablet
Inert Tablet Core
1
Lactose
258.85
2
Sodium lauryl sulfate
10.57
3
Crospovidone
13.05
4
Silicified microcrystalline cellulose
151.65
5
Magnesium stearate
0.91
Drug nano-dispersion coating
6
Fenofibrate
145
7
Hydroxypropyl methylcellulose
29
8
Sucrose
141.81
9
Microcrystalline cellulose
3.19
10
Purified water
q.s
Drug loaded tablet weight
754
Film coating
11
Opadry
20
12
Purified water
q.s
Film coated tablet weight
774
Example 6
[0179]
[0000]
S. No
Ingredients
mg/tablet
Inert Tablet Core
1
Lactose
258.85
2
Sodium lauryl sulfate
10.57
3
Crospovidone
13.05
4
Silicified microcrystalline cellulose
151.65
5
Magnesium stearate
0.91
Drug nano-dispersion coating
6
Fenofibrate
145
7
Hydroxypropyl methylcellulose
29
8
Sucrose
135.43
9
Microcrystalline cellulose
3.19
10
Crospovidone
6.38
11
Purified water
q.s
Drug loaded tablet weight
754
Film coating
12
Opadry
20
13
Purified water
q.s
Film coated tablet weight
774
Example 7
[0180]
[0000]
S. No
Ingredients
mg/tablet
Inert Tablet Core
1
Lactose
258.85
2
Sodium lauryl sulfate
10.57
3
Crospovidone
13.05
4
Silicified microcrystalline cellulose
151.65
5
Magnesium stearate
0.91
Drug nano-dispersion coating
6
Fenofibrate
145
7
Hydroxypropyl methylcellulose
29
8
Sucrose
100.34
9
Microcrystalline cellulose
31.9
10
Crospovidone
12.76
11
Purified water
q.s
Drug loaded tablet weight
754
Film coating
12
Opadry
20
13
Purified water
q.s
Film coated tablet weight
774
[0181] The compositions given in Examples 2 to 7 were prepared using the similar procedure described in Example 1.
[0182] Table 1 given below shows the comparative dissolution profile of fenofibrate tablets according to the present invention (Examples 1-3) and Tricor® Tablets carried out in 1000 ml medium (water+0.05M sodium lauryl sulphate) using Apparatus USP II (Paddle), at 50 rpm speed.
[0000]
TABLE 1
% Drug released
Time in min
Example-1
Example-2
Example-3
Tricor ® 145 mg
10
85
81
76
92
30
93
95
97
96
45
94
96
98
96
60
96
96
98
96
|
An improved solid dosage form of fenofibrate which exhibits improved dissolution properties leading to increased bioavailability of fenofibrate. A novel core-shell approach to the composition is provided as well as a process for the preparation of the improved solid dosage forms.
| 0
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CROSS REFERENCE TO RELATED APPLICATION(S)
[0001] This application claims the benefit of Korean Patent Application No. 10-2005-0133753, filed Dec. 29, 2005, entitled “Device for sensing position of camera and mobile phone comprising the same”, which is hereby incorporated by reference in its entirety into this application.
BACKGROUND OF THE INVENTION
[0002] 1. Field of the Invention
[0003] The present invention relates, in general, to a camera position sensing device for a mobile communication terminal such as a mobile phone, and more particularly, to a camera position sensing device which is installed in a phone body and a hinge capable of being rotated relative to the phone body to sense the rotation angle of a camera, and to a mobile phone having the same.
[0004] 2. Description of the Prior Art
[0005] As is generally known in the art, in a mobile communication terminal, a magnet is installed in a camera module, and a sensor (for example, a hall element) for sensing the density of magnetic flux generated in the magnet (for example, a change in a magnetic field) is installed in a terminal body. When the camera module is rotated relative to the terminal body, the rotation angle thereof can be sensed by the sensor.
[0006] That is to say, a camera position sensing device comprises a magnet which is installed in a relatively rotatable member and a hall element which is installed in a relatively fixed member. The rotated state of a camera is detected using the magnetic flux density of the magnet which is sensed by the hall element.
[0007] FIG. 1 is a front view illustrating a conventional mobile phone 10 having a camera position sensing device. The construction of the mobile phone 10 will be described with reference to FIG. 1 .
[0008] The general structure of the mobile phone 10 having a camera module 50 includes a phone body 20 which has a key pad 22 , and a folding part 30 which is coupled to the phone body 20 through a hinge 40 and has an LCD module 32 . In FIG. 1 , the camera module 50 is illustrated as being coupled to the hinge 40 .
[0009] A sensor 24 such as a hall element is installed in the phone body 20 , which is relatively fixed, and a magnet 34 is installed in a member (for example, the folding part 30 in FIG. 1 ) which is rotated relative to the phone body 20 . The rotation angle of the camera module 50 , that is, the rotation angle of the lens of the camera module 50 , is sensed using the sensor 24 and the magnet 34 . In FIG. 1 , the rotation angle of the camera module 50 can be utilized, for example, to allow a display screen on the LCD module 32 of the folding part 30 to be reversed depending upon the rotated state of the camera module 50 (the direction of the camera lens).
[0010] FIGS. 2A through 2C illustrate a typical example in which the rotated state of a camera module 50 is sensed by a magnet 54 which is rotated about a hinge and the hall element (the sensor) 24 of a phone body 20 which is relatively fixed.
[0011] In FIG. 2A through 2C , the magnet 54 is directly attached to the camera module 50 such that the magnet 54 can be rotated together with the camera module 50 about the hinge with respect to the relatively fixed phone body 20 .
[0012] Referring to FIG. 2A , when the lens 52 of the camera module 50 faces forward (in the direction indicated by the arrow A), the magnet 54 is positioned farthest from the sensor 24 of the phone body 20 . The magnet 54 is arranged on a reference line C which connects the rotation center of the camera module 50 (that is, the center axis of the hinge) with the sensor 24 , and at this time, the angle between the magnet 54 and the sensor 24 is determined as θ 1 . Actually, the angle θ 1 is defined perpendicularly to the direction of the arrow A.
[0013] Next, FIG. 2B illustrates the state in which the camera module 50 is rotated by a quarter turn, that is, 90°, so that the lens 52 faces away from the phone body 20 . At this time, the magnet 54 is positioned perpendicular to the reference line C, and the angle between the magnet 54 and the sensor 24 is determined to be θ 2 .
[0014] Finally, FIG. 2C illustrates the state in which the camera module 50 is rotated by a half turn, that is, 180°, so that the lens 52 faces rearward (in the direction indicated by the arrow B). At this time, the magnet 54 is positioned nearest to the sensor 24 of the phone body 20 , and the angle between the magnet 54 and the sensor 24 is determined to be θ 3 .
[0015] As can be readily seen from the above descriptions, in the camera position sensing structure as shown in FIGS. 2A through 2C , with the rotation of the camera module 50 , as the magnet 54 is rotated from the farthest position toward the nearest position with respect to the sensor 24 , the rotation angle of the camera module 50 is sensed in conformity with a change in the position of the camera module 50 .
[0016] However, in the structure for sensing the rotation of the camera module 50 using the magnet 54 and a sensor 24 such as a hall element, since the rotated state of the camera module 50 is sensed using only the relative distance between the magnet 54 and the sensor 24 , erroneous operation of the mobile phone may result.
[0017] For example, referring to FIG. 3 , assuming that the angle at the forward facing position (the direction indicated by the arrow A in FIG. 2A ) is 0° and that the angle at the rearward facing position (the direction indicated by the arrow B in FIG. 2C ) is 180°, by analyzing the measurement results obtained from the sensor 24 while the camera module 50 is rotated from 0° to 180°, it was confirmed that the sensor 24 doubly passes through an optional operation point (for example, the point having a magnetic flux density of 40 gauss).
[0018] In other words, in the case of the mobile phone having the conventional camera position sensing structure, when the folding part is fully rotated from 0° to 180°, the sensor 24 passes an optional operation point twice, and therefore, it is difficult to precisely sense the rotated state of the camera module 50 .
[0019] Of course, this phenomenon can be prevented by limiting the rotation angle of the folding part to an angle (for example, about 135°) which is immediately before the camera module 50 secondarily passes through the optional operation point, but in this case, the design of the mobile phone cannot but be negatively impacted.
SUMMARY OF THE INVENTION
[0020] Accordingly, the present invention has been made keeping in mind the above problems occurring in the prior art, and an object of the present invention is to provide a camera position sensing device which employs a magnet and a sensor to sense the rotated state of a camera module so that a linear sensing result is obtained from the sensor throughout the entire rotation range of the camera module.
[0021] Another object of the present invention is to provide a mobile phone which has a camera position sensing device capable of linearly sensing the position of a camera.
[0022] In order to achieve the first object, according to one aspect of the present invention, there is provided a camera position sensing device comprising a magnet installed in a first member which is mounted with a camera module; and a hall element installed in a second member which is relatively rotatably coupled to the first member, to sense the position of the camera module depending upon the relative position of the hall element with respect to the magnet, wherein an initial offset is afforded to an installation position of the magnet in the relative rotating direction of the magnet.
[0023] According to another aspect of the present invention, the hall element senses the position of the camera module based on the relative position of the hall element from the magnet and the direction of the magnetic flux of the magnet.
[0024] According to another aspect of the present invention, as the initial offset is afforded to the magnet, the hall element linearly senses the position of the camera module.
[0025] According to another aspect of the present invention, the camera module is rotatably mounted to the first member, and the magnet is directly installed on the camera module.
[0026] According to another aspect of the present invention, the camera module includes a lens, and the position of the camera module indicates the orientation of the lens.
[0027] In order to achieve the second object, according to another aspect of the present invention, there is provided a mobile phone having a camera position sensing device, comprising a first member having a camera module mounted thereon; a second member relatively rotatably coupled to the first member; and a camera position sensing device having a magnet which is installed in one of the first and second members and a hall element which is installed in the other of the first and second members, wherein the hall element senses the position of the camera module depending upon the relative position of the hall element with respect to the magnet, and an initial offset is afforded to an installation position of the magnet in the relative rotating direction of the magnet.
[0028] According to another aspect of the present invention, the second member comprises a phone body which has a key pad, and the first member comprises a hinge shaft which is rotatably coupled to one side of the phone body.
[0029] According to another aspect of the present invention, the mobile phone further comprises a folding part connected to the phone body by the medium of the hinge shaft and attached with an LCD module.
[0030] According to still another aspect of the present invention, as the initial offset is afforded to the magnet, the hall element linearly senses the position of the camera module.
[0031] According to a still further aspect of the present invention, the camera module is rotatably mounted to the first member, and the magnet is directly installed on the camera module.
BRIEF DESCRIPTION OF THE DRAWINGS
[0032] The above and other objects, features and other advantages of the present invention will be more clearly understood from the following detailed description when taken in conjunction with the accompanying drawings, in which:
[0033] FIG. 1 is a front view illustrating a conventional mobile phone having a camera position sensing device;
[0034] FIGS. 2A through 2C are diagrammatic views illustrating the operation of a conventional camera position sensing device;
[0035] FIG. 3 is a graph illustrating the measurement results of the camera position sensing device of FIG. 2 depending upon rotation angles;
[0036] FIGS. 4A through 4C are diagrammatic views illustrating the operation of a camera position sensing device in accordance with an embodiment of the present invention;
[0037] FIG. 5 is a graph illustrating the measurement results of the camera position sensing device of FIG. 4 depending upon rotation angles; and
[0038] FIG. 6 is a perspective view illustrating a mobile phone in accordance with another embodiment of the present invention.
DETAILED DESCRIPTION OF THE INVENTION
[0039] Reference will now be made in greater detail to a preferred embodiment of the invention, an example of which is illustrated in the accompanying drawings. Wherever possible, the same reference numerals will be used throughout the drawings and the description to refer to the same or like parts.
[0040] FIGS. 4A through 4C are diagrammatic views illustrating the constructions and operations of a magnet and a hall element in accordance with an embodiment of the present invention.
[0041] Referring to FIG. 4A , a camera position sensing device in accordance with the embodiment of the present invention comprises the pair of a magnet 154 attached to a camera module 150 and a sensor 124 such as a hall element attached to a phone body 120 . According to the present invention, the magnet 154 has a predetermined initial offset angle θ off in the rotating direction of a camera, which is measured from a reference line C connecting the center of the camera module 150 (for example, the rotation axis of a hinge) with the sensor 124 .
[0042] Concretely speaking, referring to FIG. 4A , when the lens 152 of the camera module 150 faces forward (in the direction indicated by the arrow A), as the magnet 154 is initially offset by the angle θ off in the direction opposite the rotating direction of the camera module 150 , the initial offset angle θ off is afforded. That is to say, when the lens 152 of the camera module 150 faces forward (in the direction indicated by the arrow A), the magnet 154 is initially offset from the conventional position θ 1 in the direction opposite the rotating direction of the camera module 150 by an angle corresponding to the initial offset θoff.
[0043] Referring to FIGS. 4B and 4C , as the camera module 150 is rotated with the initial offset θ off afforded, when compared to the conventional positions θ 2 and θ 3 (see FIGS. 2B and 2C ), the magnet 154 is rotated while it is offset by the initial offset angle θ off In other words, when the lens 152 of the camera module 150 faces away from the phone body 120 and faces rearward (in the direction indicated by the arrow B), when compared to the conventional positions θ 2 and θ 3 , the magnet 154 is rotated while maintaining the initial offset θ off .
[0044] By affording the initial offset θ off to the installation position of the magnet 154 , the hall element 124 can precisely sense a change in a magnetic field which is generated in the magnet 154 .
[0045] In the conventional art, since the magnet is simply positioned based on the relative distance between the magnet and the hall element, the sensor doubly passes through an operation point. However, in the camera position sensing device according to the present invention, the magnetic flux density is linearly sensed, as shown in FIG. 5 . That is to say, while the folding part is rotated from 0° to 180°, the rotated state of the camera depending upon the magnetic flux density of the magnet is linearly detected, whereby the rotated state of the folding part can be precisely sensed.
[0046] This is based on the fact that the portion of the magnet for sensing the magnetic flux density is not the portion 124 a of the hall element 124 which faces the hinge but the portion 124 b of the hall element 124 which is perpendicular to the reference line C. That is to say, in order to measure the density of the magnetic flux generated in the magnet, a magnetic field M must perpendicularly pass through the portion of the hall element 124 . To this end, as can be readily seen from FIG. 4A , the magnetic flux density is detected from the portion 124 b of the hall element 124 which is perpendicular to the reference line C.
[0047] For reference, each of FIGS. 3 and 5 illustrates an analyzing graph which is obtained by programming the relative positional relationship between the magnet and the hall element in each of the conventional art and the present invention, and calculating sensing results using a technique such as a finite element method (FEM). Concretely speaking, each of FIGS. 3 and 5 illustrates magnetic flux densities which are sensed while rotating the lens of the camera module from 0° (in the example, the direction indicated by the arrow A) to 180° (in the example, the direction indicated by the arrow B).
[0048] As a consequence, in the camera position sensing device according to the embodiment of the present invention, as the magnet is offset by the initial offset angle θ off , the magnetic flux densities of the magnet, which are sensed by the hall element, are linearly obtained, and thus, it is possible to prevent misoperation of the mobile phone which is otherwise caused in the conventional art due to double passage through an operation point. Also, in the present invention, since the linear sensing results can be obtained by affording the initial offset, it is possible to reverse a display screen by setting an optional operation point as desired.
[0049] In the conventional art, in order to prevent such misoperation, a specific operation point having a predetermined value (for example, 40 gauss) must be set. However, in the present invention, since the magnetic flux density is linearly measured, even when an optional operation point is set, the misoperation is not caused. Consequently, it is possible to freely set an operation point to conform with a desired rotation angle (a desired rotation angle of the camera module) when designing the mobile phone.
[0050] FIG. 6 is a perspective view illustrating a mobile phone 110 in accordance with another embodiment of the present invention. The construction of the mobile phone 110 according to this embodiment of the present invention will be described with reference to FIG. 6 .
[0051] The mobile phone 110 according to this embodiment of the present invention includes a phone body 120 which has a key pad 122 , a folding part 130 which is rotatably coupled to the phone body 120 through a hinge 140 and has an LCD module 132 , and a camera module 150 which is provided adjacent to an end of the hinge 140 and can be rotated with respect to the phone body 120 irrespective of the hinge 140 . A magnet 154 is installed on one side of the camera module 150 at an initial offset angle θ off , and a hall element 124 capable of sensing the magnetic flux density of the magnet 154 is installed on a side of the phone body 120 .
[0052] The pair of the magnet 154 of the camera module 150 and the hall element 124 of the phone body 120 constitutes a camera position sensing device 160 according to the present invention.
[0053] The mobile phone according to the present invention has the camera position sensing device which comprises the magnet and the hall element. In the mobile phone, by using the camera position sensing device, the position of the camera can be linearly sensed in conformity with the rotated state of the camera (between the forward direction indicated by the arrow A and the rearward direction indicated by the arrow B), and the sensing result can be reflected on the LCD module of the folding part. That is to say, the image displayed on the LCD module can be reversed as the occasion demands depending upon the rotated state of the camera module (the lens of the camera module).
[0054] While it was explained with reference to FIG. 6 that the magnet and the hall element were respectively installed in the camera module disposed in the hinge and the phone body, the present invention is not limited to this arrangement. Namely, while not shown in a separate drawing, it can be envisaged that a camera module is disposed in a folding part which has an LCD module, and a magnet which is afforded with an initial offset θ off according to the feature of the present invention is installed in the folding part.
[0055] As is apparent from the above description, the camera position sensing device according to the present invention comprises the pair of a hall element and a magnet. Specifically, due to the fact that the position of the magnet has an initial offset angle θ off in the rotating direction, the magnetic flux density of the magnet can be linearly sensed within the rotation range (from 0° to 180°) of a camera. By using the camera position sensing device, the problem of the rotated state of the camera being erroneously sensed due to the misoperation of the camera position sensing device can be solved.
[0056] Although a preferred embodiment of the present invention has been described for illustrative purposes, those skilled in the art will appreciate that various modifications, additions and substitutions are possible, without departing from the scope and spirit of the invention as disclosed in the accompanying claims.
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A camera position sensing device comprises a magnet installed in a first member which has a camera module mounted therein, and a hall element installed in a second member which is relatively rotatably coupled to the first member, to sense a position of the camera module depending upon a position of the hall element relative to the magnet, wherein an initial offset is afforded to an installation position of the magnet in a relative rotating direction of the magnet.
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RELATED APPLICATION
[0001] This application is based on and claims the benefit of U.S. Provisional Application No. 60/316,371, filed Aug. 31, 2002.
FIELD OF THE INVENTION
[0002] This invention relates to an article for supporting, organizing and protecting elongated items, particularly optical fibers.
BACKGROUND OF THE INVENTION
[0003] It is advantageous to provide relatively delicate, elongated items such as optical fibers with an external structure which supports, protects and organizes them. Support of the fibers prevents or mitigates mechanical stresses on the fibers which can cause degradation of fiber performance or even outright fiber failure. Stresses in the fibers which adversely affect transmission of optical signals may be caused by tensile or compressive forces, as well as by merely bending the fibers. Protection is necessary because the fibers are also generally subject to physical damage due to impact, shock and abrasion which can result from rough handling during installation, as well as conditions of service. Organization of the optical fibers permits ends to be readily identified and properly and quickly terminated regardless of the length or number of fibers being considered. Such organization is an invaluable time saver when the fibers are connected to other fibers or a device because it allows the ends to be connected to the appropriate mating fiber or terminal without the need for testing and identifying each fiber before the connection is completed.
[0004] Currently, it is the practice to ensheath bundles of optical fibers within a tubular cable comprising a thin-walled outer jacket formed of flexible plastic such as PVC, PTFE, polyethylene or polypropylene. Alternatively, optical fibers are also protected in a flat ribbon of flexible plastic with the fibers arranged in spaced relation adjacent to one another across the width of the ribbon.
[0005] The jackets, tubes and ribbons used with current optical fiber cables and ribbons tend to be relatively stiff as compared with the optical fibers and, thus, may impart significant forces on the optical fibers when the cable or ribbon is handled, twisted and bent during installation and servicing. Furthermore, optical fibers within a tubular cable are substantially disorganized and must be coded for identification to enable the ends to be properly terminated. Although the fibers remain organized and easily identifiable when flat ribbon is used to protect them, there are practical considerations limiting the width of the ribbon and thereby the number of optical fibers which can be supported with a particular ribbon. There is clearly a need for improvements in the support, protection and organization of optical fibers.
SUMMARY AND OBJECTS OF THE INVENTION
[0006] The invention concerns a flexible carrier for supporting, protecting and organizing elongated items such as optical fibers. The carrier comprises a substrate formed of a plurality of interlaced filamentary members. The elongated items are captured within the substrate during interlacing of the filamentary members and are thereby fixed in position relatively to one another within the substrate.
[0007] In a preferred embodiment, the elongated items are received within the substrate at a plurality of positions by being interlaced with the filamentary members. A group of the filamentary members is oriented transversely to and engageable with the elongated items at a plurality of crossing points positioned on opposite sides of the elongated items to fix the positions of the elongated items within the substrate. The filamentary members are preferably interlaced by weaving a first portion of them in a warp direction and a second portion of them in a fill direction. The elongated items are oriented substantially parallel to the first portion of filamentary members in the warp direction. The group engageable with the elongated items comprises a plurality of the filamentary members woven in the fill direction. These filamentary members are positioned in spaced relation to one another lengthwise along the substrate.
[0008] In an alternate embodiment, the filamentary members are interlaced by weaving and are woven about the elongated items to form a plurality of elongated tubes positioned side-by-side and connected lengthwise, the tubes capturing the elongated items.
[0009] It is an object of the invention to provide a device for supporting, organizing and protecting delicate elongated items.
[0010] It is an object of the invention to provide a device which will support elongated items without subjecting the items to harmful stress.
[0011] It is another object of the invention to provide a device in which the elongated items can be integrated during manufacture of the device.
[0012] These as well as other objects and advantages of the invention will become apparent upon further consideration of the following drawings and detailed description of preferred embodiments.
BRIEF DESCRIPTION OF THE DRAWINGS
[0013] [0013]FIG. 1 is a perspective view of a flexible, elongated carrier adapted to receive elongated filaments such as optical fibers;
[0014] [0014]FIG. 2 is a perspective view of an alternate embodiment of the carrier shown in FIG. 1;
[0015] [0015]FIG. 3 is a perspective view of a second alternate embodiment of the carrier shown in FIG. 1;
[0016] [0016]FIG. 4 is a perspective view of another embodiment of a carrier according to the invention;
[0017] [0017]FIG. 5 is a perspective view of a second alternate embodiment of the carrier shown in FIG. 1; and
[0018] [0018]FIG. 6 is a plan view of a portion of a knitted substrate according to the invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0019] [0019]FIG. 1 shows a carrier 10 according to the invention. Carrier 10 comprises a flexible, elongated substrate 12 comprising a plurality of filamentary members 14 interlaced together. Elongated items, for example, optical fibers 16 , are positionable lengthwise along the substrate 12 and are engaged and held thereto by filamentary members 18 which are oriented within the substrate substantially transversely to the optical fibers 16 and engage them at a plurality of crossing points 17 positioned on opposite sides of the elongated items. Preferably, the filamentary members 14 comprising the substrate 12 are interlaced by weaving and the transverse filamentary members 18 comprise fill yarns in the weave. Other filamentary members 14 are oriented lengthwise along the substrate to form warp yarns 20 . The optical fibers 16 are arranged substantially parallel to the warp yarns 20 . Although weaving is preferred, the filamentary members 14 may also be interlaced by braiding, as well as knitting.
[0020] In the embodiment of the invention shown in FIG. 1, the optical fibers 16 are interwoven as warp yarns during manufacture of the substrate 12 . The warp and fill yarns 20 and 18 provide support and protection to the interwoven optical fibers 16 , the fill yarns 18 engaging the optical fibers by passing transversely over and under them and thereby retaining them to the substrate 12 . The optical fibers 16 do not need to be interwoven with every fill yarn 18 . Portions 19 of the optical fibers may be permitted to float along the surface of the substrate, and the fill yarns 18 which do engage the optical fibers 16 may be positioned in spaced relation along the length of the substrate 12 . The warp yarns 20 , being substantially parallel to the optical fibers 16 , keep them consistently positioned in spaced relation across the width of the substrate. The spacing is important because it preserves the relative position of the optical fibers to one another in the substrate, allowing them to be readily identified by their position without the need for separate coding. This methodical organization of the optical fibers allows them to be quickly and correctly connected to other optical fibers via mechanical connectors or to optical devices such as optical amplifiers and modulators, without the need for testing to identify each optical fiber.
[0021] [0021]FIG. 2 illustrates an embodiment 22 of the carrier having a relatively wide substrate 24 which can be accordion folded with a plurality of reverse bends 26 forming pleats 27 extending lengthwise along the substrate substantially parallel to the warp direction indicated by arrow 28 . The inherent flexibility of the woven substrate 24 allows the pleats 27 to be formed easily without placing any significant stress on the interwoven optical fibers 16 , providing a relatively high density packing of optical fibers on a compact substrate. Since the substrate 24 is woven or knitted, the width may be varied over as wide a range as desired virtually without a practical limit.
[0022] [0022]FIG. 3 shows another embodiment 30 of the carrier according to the invention, again comprising a substrate 32 preferably woven of fill yarns 18 and warp yarns 20 . Substrate 30 is woven into a plurality of tubes 34 , each tube having an interior space 36 adapted to receive one or more optical fibers 16 . The tubes are positioned side by side and connected lengthwise along a plurality of seams 38 defining and separating each of the tubes 34 . Seams 38 are preferably formed by well known interweaving techniques but could also be sewn, welded or bonded. Preferably, tubes 34 are woven around the optical fibers 16 as the substrate is manufactured thereby capturing the fibers securely within the tubes.
[0023] The carrier according to the invention need not be substantially flat. As shown in FIG. 4, the carrier 40 comprises a substrate 42 which forms the sidewall 43 of an elongated sleeve 44 . Substrate 42 is preferably woven as a sleeve but could also be knitted or braided, or a flat substrate 12 , as shown in FIG. 1, could be formed into a circular shape around its long axis parallel to the warp direction 28 and opposite edges brought together and joined, for example, by sewing, bonding or welding. The carrier embodiment 40 has optical fibers 16 interwoven as warp yarns in the sidewall 43 of the sleeve 44 and also provides an interior space 46 which may be used to house other elongated items such as a wiring harness 48 .
[0024] As shown in FIG. 5, sleeve 44 may also comprise tubes 34 arranged around a common center axis 35 oriented lengthwise along the sleeve, the tubes 34 each having an interior space 36 for receiving one or more optical fibers 16 or other elongated items. Similar to the flat substrate 32 shown in FIG. 3, the tubes are preferably integrally formed with the sleeve 44 and interlaced around the optical fibers 16 which during manufacture.
[0025] [0025]FIG. 6 shows how elongated items such as optical fibers 16 may be integrally positioned within a knitted substrate 50 . Knitted substrate may be formed into a flat, pleated or sleeved configuration as described above for woven substrates. In the knitted substrate 50 , the filamentary members 52 are interlaced in a plurality of loops 54 forming a plurality of wales 56 arranged adjacent to one another in a plurality of courses 58 . The optical fibers 16 are laid into the substrate during knitting, transversely to the wales 56 and are engaged on opposite sides by the loops 54 which fix the optical fibers 16 in position within the substrate.
[0026] The properties of the warp and fill yarns 20 and 18 play a role in determining the characteristics of the various substrate embodiments. Multifilament and monofilament polyester yarns are preferred for most applications since these yarns are readily available, easily woven, knitted or braided and have excellent tensile strength, flexibility and abrasion resistance. For a more flexible substrate, multifilament yarns are preferred. Monofilament yarns provide relatively better abrasion resistance than multifilament yarns but result in a less flexible substrate. Combinations of multifilament and monofilament yarns are feasible to realize both improved abrasion resistance and flexibility.
[0027] Yarns of other materials, such as nylon and aramid fibers, may also comprise the substrate when special properties, such as high-temperature resistance or increased tensile strength are required.
[0028] In addition to varying material properties of the yarns, the properties of the weave, knit or braid can also be adjusted to achieve desirable properties for the substrate. For example, the density of the weave may be set to a relatively high number of picks per inch to provide a substrate having a relatively closed mesh which securely fixes the position of the optical fibers. The mesh may also be relatively open allowing the optical fibers to float within the weave of the substrate.
[0029] Furthermore, the pattern of the weave is another variable which may be used to achieve desired characteristics advantageous to the support and protection of the optical fibers. For example, the optical fibers may be engaged by fewer than all of the fill yarns in the weave, thereby reducing the number of contact points between the yarns and the fibers and providing relatively long runs of optical fibers which are not integrally woven in the substrate. Such a construction allows for the convenient branching of optical fibers at any desired point along the substrate.
[0030] The carrier may be manufactured by interlacing a plurality of filamentary members to form a substrate and interlacing a plurality of the optical fibers or other elongated items with the filamentary members at a plurality of positions. During interlacing, the optical fibers are oriented transversely to a group of the filamentary members which engage the optical fibers at a plurality of crossing points positioned on opposite sides of the optical fibers thereby fixing the relative position of the optical fibers within said substrate. In a woven substrate, the fill yarns comprise the transverse filamentary members which form the crossing points with the optical fibers.
[0031] Carriers comprising a plurality of filamentary members interlaced to form a substrate for the support and protection of elongated items such as optical fibers provide a durable, flexible, versatile and inexpensive means for conveying and organizing the items which is particularly suited to optical fiber applications.
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A flexible carrier for supporting and protecting elongated items such as optical fibers is disclosed. The carrier is formed from a substrate of interlaced filamentary members which may be woven, knitted or braided together. The elongated items are interlaced with or otherwise captured by the substrate during its manufacture. Various configurations of the substrate such as flat, pleated and tubular are feasible. Capture of the elongated members may be effected by integrally woven tubes formed within the substrate, by interweaving the items as warp yarns in a woven substrate or by laying in of the items in a knitted substrate.
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BACKGROUND OF THE INVENTION
Displacement feedback control systems (DFCs) and non-feedback proportional (NFPs) have previously been used for axial piston hydrostatic pumps. The Control Block Diagrams A and B shown in FIGS. 16 and 17 the basic differences between the Feedback (DFC) and non-feedback (NFP) control systems.
The control of the pump necessarily involves controlling the position of the swashplate of the pump. With a DFC mechanism, the swashplate position is primarily a function of only an input signal, manual, electrical or hydraulic. The DFC controls position of a servo piston and swashplate system proportional to the input signal utilizing a mechanical feedback linkage. With an NFP control, the swashplate position is a function of the input signal and the moments imposed on the swashplate which are dependent on the input speed to the pump, the operating pressure for the pump, and the swashplate angle.
The DFC system has several functional advantages, but is expensive to manufacture. The NFP is less expensive but also has certain beneficial characteristics including a softer ride for the vehicle driven by the transmission, and inherent characteristics similar to a low performance anti-stall system. However, on certain types of vehicles, these characteristics can be drawbacks. This is especially true of vehicles requiring constant speed (i.e., constant swashplate position), aggressive performance, responsiveness independent of vehicle load, and applications which use a micro-processor based anti-stall system sensing engine speed. In addition, the NFP control is typically less stable than a DFC due to the lack of compensation provided by the feedback mechanism.
Therefore, it is a principal object of this invention to provide a NFP system to allow improved control for a hydrostatic pump.
More specifically, it is an object of this invention to provide a NFP system to achieve desired operating characteristics which will allow the control of a hydrostatic transmission to closely approximate the control performance provided of a DFC system.
These and other objects will be apparent to those skilled in the art.
SUMMARY OF THE INVENTION
A method is provided for allowing a hydraulic pump with a non-feedback proportional control to closely approximate the performance of a displacement feedback control by taking a hydraulic pump including a rotatable piston group engaging a pivotal swashplate, with the pump having associated therewith an input power shaft and a servo piston mechanically connected to the swashplate to influence a torque imposed on the swashplate when rotational power is imposed on the pump, and a neutral return spring connected to the swashplate and a pump housing; providing a valve plate to control fluid flow between pistons in the group and pressure and return fluid conduits; providing in the valve plate a plurality of elongated arcuate slots extending therethrough concentrically located at a constant radius with respect to a center of the plate and an axis of rotation of the piston group, with each slot having opposite ends, an elongated notch at one end of some of the slots and extending away from the end to form a bottom with sidewalls extending upwardly with respect to the bottom; providing a valve plate index for the valve plate to approximately a −1.5° to −0.5° wherein the valve plate index is defined as the location of a pressure transition zone relative to top or bottom dead center positions of a piston in the rotatable piston group being in either a fully retracted or fully extended position in its operational movement; providing a cylinder block with a piston port for the piston group with fluid inlet and outlet ports in communication with the pistons of the piston group; providing valve plate crossport of approximately 3° to 9° wherein the valve plate crossport is defined as the amount of angle of rotation during which the piston port in the cylinder block is connected to both the inlet and outlet ports at the same time; maintaining the swashplate at a first swashplate offset of −0.015 in. to +0.015 in. in a first direction parallel to axes of rotation of the piston group; maintaining the swashplate at a second swashplate offset of −0.060 in. to +0.060 in. in a second direction perpendicular to a longitudinal axis of the pistons; maintaining the ratio of the volumes of the fluid in the piston bores at a top dead center position of movement of the piston in the bore to the volume at a bottom dead center position of 0.53 to 0.73 and adjusting the spring rate of the return spring to a range of approximately 470-670 pounds/inch; whereby the dependency of the angular position of the swashplate is influenced by less than 50% on operating conditions of the transmission and is increasingly influenced by more than 50% by an input signal acting thereon to ensure stability throughout the transmission's operating range for speed, pressure and swashplate angle.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a perspective view of a hydrostatic transmission adaptable for use with this invention;
FIG. 2 is a schematic cross sectional view of the transmission of FIG. 1 in forward, neutral and reverse modes;
FIG. 3 is a schematic diagram showing the control forces acting on the swashplate;
FIG. 4 is a schematic view of the progressive positions of the servo spring;
FIG. 5 is a plan view of the valve plate;
FIG. 6 is a partial plan view of the valve plate taken on line 6 — 6 of FIG. 5;
FIG. 7 is a partial plan view of the fluid inlet into one of the grooves in the valve plate;
FIG. 8 is a sectional view taken on line 8 — 8 of FIG. 7;
FIG. 9 is a sectional view taken on line 9 — 9 of FIG. 8;
FIG. 10 is a diagram of valve plate indexing;
FIG. 11 is a bottom plan view showing the piston locations associated with inlet and outlet fluid pressures;
FIG. 12 is a perspective view of the bottom of the rotating group showing inlet and outlet ports;
FIG. 13 is a diagram showing the input signal effect on the swashplate with the pivot point of the swashplate being offset with respect to the pivotal axes of the swashplate trunnion;
FIG. 14 is an enlarged scale cross section through a piston in a rotating group at its top dead center position; and
FIG. 15 is a view like FIG. 14 showing the piston in a bottom dead center position.
FIG. 16 is a control block diagram for a feedback (DFC) control system.
FIG. 17 is a control block diagram for a non-feedback (NFP) control system.
DESCRIPTION OF THE PREFERRED EMBODIMENT
The overall goal of this invention is to control the slope and separation of control torque curves as a function of speed, system pressure, and swashplate angle. This includes: (1) reducing the dependency of the swashplate angle on non-input signal parameters (i.e., system pressure and speed; (2) increasing the dependency of the angle of the swashplate on the input signal; (3) ensuring the stability throughout the operating range of the vehicle for speed, pressure and swashplate angle; and (4) reducing the swashplate vibration and noise in conjunction with steps (1)-(3).
The foregoing goal is achieved by bringing together a plurality of known control concepts, fine tuning some or all of these concepts within certain parameters, as discussed hereafter, wherein a control system results which will allow the control of a hydrostatic transmission to approximate the control performance of a DFC system.
With reference to FIG. 1, a hydrostatic transmission 10 for use in a vehicle such as a compact utility tractor has a housing 12 having a Z-shaped configuration with an input shaft 14 parallel to but offset from an output shaft 16 . As seen in FIG. 2, the housing 12 has a center section 18 with internal fluid conduits 20 and 22 which fluidly connect hydrostatic pump 24 with hydrostatic motor 26 . Input shaft 14 is conventionally connected to pump 24 , and output shaft 16 is operatively connected to motor 26 .
The pump 24 has a conventional rotating group 28 mounted on a valve plate 30 and include a plurality of reciprocal pistons 32 with “outer” ends which conventionally engage the flat side of swashplate 34 which is pivotably mounted on a trunnion (not shown). Fluid from conduits 20 and 22 flow through conventional ports in the valve plate 30 to fluidly connect the pump 24 and the motor 26 . The input shaft 14 freely extends through a conventional aperture (not shown) in the swashplate. The angle of the swashplate determines the mode of output shaft 16 . In the neutral position, there is no fluid flow in conduits 20 and 22 between the pump 24 and motor 26 . For positions other than neutral the rotation of output shaft 16 is shown by the arrows F and R in FIG. 2 reflecting forward and rearward directions of travel. The corresponding angular position of the swashplate corresponding to the arrows F and R are also shown in FIG. 2 . The numeral 36 designates an input signal actuated servo piston which is conventionally connected to the swashplate 34 . The movement of the piston in valve 36 is designated by the arrows in FIG. 2 for the forward and reverse directions of rotation of the output shaft 16 . This invention deals essentially with the control of the position of swashplate 34 .
The known control concepts referenced above are (1) the servo spring rate; (2) the valve plate index; (3) valve plate crossport/trap; (4) valve plate porting geometry; (5) swashplate offset; and (6) piston bore volume. Each of these concepts will be discussed below.
Servo Spring Rate
FIG. 3 is a schematic drawing showing the control forces acting on the swashplate 34 . The numeral 38 designates a servo spring which extends between the swashplate 34 and the housing 12 . Every spring has a spring rate which is a measure of its physical makeup. In conjunction with this invention, the spring rate of servo spring 38 should be in the range of 470 to 670 pounds/inch.
The servo spring rate provides a differential load/torque to the swashplate 34 as the servo piston (not shown) of valve 36 and servo spring 38 are moved a given distance. The effect of piston bore pressure (discussed below) to average control torque required can be reduced, by increasing the spring rate so that pressure dependency is reduced. The spring rate overshadows differences due to pressure. The spring rate is also important for obtaining desired resolution of control torque between low and high swashplate angles.
As shown in FIG. 3, spring 38 acts in the direction of the arrow 39 . A more detailed view of spring 38 appears in FIG. 4 . As indicated in FIG. 3, spring 38 acts on swashplate 34 to return it to the neutral position of FIG. 2 . As such, the spring is a part of the input signals acting on the swashplate. With the other criteria set forth herein, it is important to maintain the spring rate of the spring 38 within the range recited above to achieve the optimum utility of the invention. The arrows T 1 -T 4 in FIG. 3 designate the following:
T1 = Total Torque About Trunnion
T2 = Pressure Moment About Trunnion
T3 = Inertia Moment About Trunnion
T4 = Neutral Return Spring Moment About Trunnion
Valve Plate
The valve plate 30 is germane to the concepts of valve plate index, valve plate crossport/trap, and valve plate porting geometry. Each of these features are discussed below.
Valve Plate Index
As previously indicated, valve plates are located adjacent a center section and are in communication with center section conduits to receive or deliver fluid under pressure to the cylinder bores of reciprocating pistons located within the rotating group rotatably mounted on the side of the plate opposite to the center section.
The valve plate 30 is shown in FIGS. 5-10. It is circular in shape and has a center aperture 40 to permit the input shaft 14 to loosely extend therethrough in spaced condition to the aperture. A plurality of arcuate ports 43 appear in spaced relation on a circular axis that is concentrically located with respect to aperture 40 . The ports are separated by lands 47 . FIGS. 7, 8 and 9 show the details of the fluid inlet end 54 of ports 43 . A tapered ramp 56 (FIGS. 7 and 8) having a V-shaped cross section (FIG. 9) is located adjacent certain of the ports 43 . The lower ends 58 of the ramps 56 communicate with an end 54 of the ports 43 (FIG. 8) The ramp 56 increases in width as its elevation decreases towards the port 43 (FIG. 7 ). In lieu of a ramp, a rectangular notch having a bottom and sidewalls can be used. The ends of ports 43 opposite to end 54 has an outlet similar to end 54 .
With reference to FIG. 10 the valve plate index controls the timing of precompression and decompression relative to TDC (top dead center) and BDC (bottom dead center) positions. Valve plate index is conventionally defined as: Index = a Lead - a Trial 2
Valve plate index is the location of the pressure transition zone of a piston 32 in the rotating group 28 relative to the rotational position where the piston is either fully retracted (bottom dead center) or fully engaged (top dead center). Index is defined as positive in direction of cylinder block rotation. A positive index tends to increase neutral-seeking torque while a negative index tends to decrease neutral seeking-torque. Valve plate index affects the dependency of control torque relative to input speed. The valve plate index of this invention is preferably at about a negative 0.870°, and within the range of negative 1.5° to a negative 0.5°, because it relies additionally on crossport, porting geometry, and the X-offset (to be discussed hereafter) to contribute to stroke reducing torque.
Valve Plate Crossport/Trap
Valve plate crossport is defined as the amount of angle of rotation during which the cylinder block piston ports 60 and 62 (FIG. 11) are connected to both the inlet and outlet ports 64 and 66 (FIG. 12) at the same time. Trap occurs when the cylinder block piston ports are blocked and are not connected to either the inlet or outlet ports 64 and 66 .
Ports 60 and 62 (FIG. 11 ), ports 64 and 66 (FIG. 12 ); and ports 43 (FIG. 5) all register with each other at times during the operation of the invention.
Valve plate crossport/trap affects the dependency of control torque relative to input speed and system pressure and affects noise and vibration due to swashplate oscillation. Specifically, it affects the piston bore pressure rise rate which affects the average control torque. A 6° angle crossport works in conjunction with the porting geometry to provide a steeper bore pressure profile and reduce the effect of pressure on the average control torque. The angular range for crossport should be within the range of 3-9°.
Valve Plate Porting Geometry
This geometry was discussed above in relation to FIGS. 5-10 with regard to Valve Plate Index, and particularly in regard to FIGS. 7, 8 and 9 .
Valve plate porting geometry affects the cross sectional area of inlet (FIG. 9) and outlet ports ( 64 and 66 —FIG. 12) and the rise rate of piston bore pressure (discussed below) from the inlet port to the outlet port which has an effect on noise. Porting geometry interacts with valve plate index and crossport/trap to affect the dependency of control torque relative to system pressure, input speed, and swashplate angle. The goal of the porting geometry was to make the inlet area large. This increases the rise rate of the bore pressure profile and reduces the effect of pressure on the average control torque.
Swashplate Offset
Swashplate offset in an “X” direction (described below) is the distance between the trunnion rotation center and point of resolution of torque producing forces (“sweetspot”). See FIG. 13 . Swashplate offset affects the control torque separation between low angle and high angle and is dependent on swashplate angle, system pressure, and speed. This offset should be in the range of −0.015 to 0.015 inches.
Offset in a “Y” direction (described below) should be in the range −0.060 to +0.060 inches. (FIG. 13 ).
As shown in FIG. 13, the “X” offset is in a direction parallel to the axes of the pistons 32 . The “Y” offset is in a direction perpendicular to the axes of the pistons.
Piston Bore Volume
Piston/bore volume of the pumping device is the amount of oil in the piston bore which must be compressed or decompressed during the pumping cycle. Piston/bore volume of the cylinder block bore and piston affects the rise rate of piston bore pressure from the inlet port to the outlet port thus, affecting the separation of the control torques relative to speed, pressure, and angle. FIG. 14 shows a piston 32 in its TDC position showing a piston bore 68 in the block 70 of rotating group 28 . When in the TDC position, the piston 32 creates a volume 72 in the bore 68 . FIG. 15 shows the piston 32 in its BDC position creating a volume 72 A in bore 68 . As can be seen, the volume 72 of FIG. 14 is smaller than the volume 72 A in FIG. 15 . Thus, as indicated above, the ratio of piston bore volumes at TDC to BDC (i.e., volumes 72 to 72 A) should be 0.53 to 0.73. Dotted line 76 shows the position of the end 78 of piston 32 when the piston (and swashplate) are in a neutral position denoting a “neutral” volume within the piston.
While each of the general concepts discussed above have been previously utilized in control systems, they have not been combined within the parameters outlined heretofore. The foregoing concepts used according to these parameters do achieve the stated goals of the invention, and result in the dependency of the angular position of the swashplate being influenced less than 50% on operating conditions of the transmission, and is influenced by more than 50% by the input signal acting thereon to ensure the stability of the transitions operating range for speed, pressure and swashplate angle.
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A non-feedback proportional system is provided to achieve desired operating characteristics which will allow the control of a hydrostatic transmission to closely approximate the control performance of a displacement feedback control system by establishing certain parameters relating to (1) the servo spring rate; (2) the valve plate index; (3) valve plate crossport/trap; (4) valve plate porting geometry; (5) swashplate offset; and (6) piston bore volume.
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This application is a continuation of U.S. patent application Ser. No. 09/504,250 filed Feb. 15, 2000 now U.S. Pat. No. 6,474,850.
FIELD OF THE INVENTION
This invention relates generally to adjuster mechanisms, and more particularly to a sliding headlamp adjuster mechanism for use in motor vehicles.
BACKGROUND OF THE INVENTION
In traditional sealed beam style headlamps; the lamp's aim is adjusted by rotating one or more screws that hold the frame of the lamp to the vehicle. Such adjustment is made from the front of the vehicle by inserting a screwdriver or the like between the lamp frame and the vehicle trim and turning the screws to alter the orientation of the lamp and effectuate the desired adjustment. As the design of motor vehicles has evolved, headlamps have continually been reconfigured to improve the aerodynamics and styling of the front end of the vehicle. Modern headlamps are designed so that their lenses follow the contour of the vehicle to provide an aerodynamically efficient exterior surface. Adjustment of these headlamps must still be performed in order to provide an optimal beam of light and to prevent the aiming of light beams toward oncoming vehicles. Such adjustment is made by moving a reflector within the lamp assembly so that light is directed in the desired manner. Automotive manufacturers+ demand for aerodynamically efficient headlamp designs has lead to modular designs where the headlamp adjustment mechanism is located within the interior of the engine compartment and positioned such that adjustment can easily performed without removing any trim pieces. Thus, the constraints of the installation area and the demands of the automobile manufacturers for aerodynamic headlamp designs dictate the location from which adjustment must be made.
There are many adjuster devices designed for use in connection with aerodynamic headlight designs including, among others, the devices disclosed in U.S. Pat. Nos. 5,707,133 and 5,214,971 to Burton, the inventor of the present invention. Modern automotive headlamp assemblies typically include several basic parts: a support frame, a reflector, a lens, a bulb, and one or more adjusters. The support frame houses the reflector and the bulb on a pivotable mounting to allow the aim of the light to be adjusted using the adjuster and provides a mounting surface for attaching adjusters. The lens seals the front of the support frame to protect it from the elements assailing the front end of the vehicle and provides an aerodynamic shape and attractive appearance. The reflector mounts on one fixed ball joint and is adjustable horizontally and vertically using adjusters that interface with the reflector through moving ball joints. The moving ball joints are moved by actuating the adjusters connected to the moving ball joints by a ball stud. Geared angle style adjusters, such as the ones disclosed in the referenced Burton patents, are often used to adjust the aim of the headlamp. However, such devices are designed to allow adjustment of the headlamp from a location behind the assembly, typically from within the engine compartment and immediately behind and above the lamp assembly. Accordingly, such devices cannot be effectively used in vehicles where the area immediately behind and above the lamp assembly is not accessible. One such vehicle design is shown in FIG. 14 . In that design, the vehicle fender 20 covers the headlamp assembly 22 rendering the area behind and above the assembly substantially inaccessible without removal of the fender 20 of the vehicle. The area below the headlamp assembly 22 is similarly inaccessible because of the bumper 21 and other vehicle components. Thus, existing geared angle style headlamp adjusters have not been found to be effective for use in such vehicle designs.
Conventionally in a vehicle such as the one shown in FIG. 14 , a sealed beam style headlamp is used. However, due to consumer and vehicle manufacturer styling preferences and performance objectives, it is desirable to use a reflector style headlamp in such vehicles. The conventional method for adjusting sealed beam lamps cannot be used to adjust a reflector style lamp and the area immediately above and behind the lamp is inaccessible such that a conventional geared angle style adjuster cannot be used. Accordingly, a need exists for a headlamp adjuster which can be used in connection with a vehicle design where the area behind and above the lamp assembly is substantially inaccessible and the use of a reflector style lamp is desired.
SUMMARY OF THE INVENTION
The present invention relates to a sliding headlamp adjuster that allows for precise adjustment control, can be used where the area above and behind the lamp assembly is inaccessible, ensures smooth operation, can include a vehicle headlamp aiming device (“VHAD”), is cost effective, and which solves the problems raised or not solved by existing headlamp adjuster designs. As described in more detail below and shown in the accompanying drawings, the sliding headlamp adjuster uses a two-piece sliding body construction to meet these objectives.
A headlamp adjuster in accordance with one embodiment of the present invention includes a base housing with a slide disposed at least partially therein. The base housing includes one or more mounting tabs such that the adjuster can be mounted to the back of a headlamp assembly support frame. The base housing has channels along its sides in which rails extending from the slide are disposed. A ball stud is threaded into the slide and protrudes therefrom passing through the base housing into the headlamp assembly. The ball of the ball stud is engaged in a socket in the reflector so that axial movement of the ball stud causes movement of the reflector. The ball stud is caused to axially move by a corresponding sliding of the slide along the channels in the base. Movement of the slide results from rotation of an adjustment screw that is threaded into the sliding piece but held in axial position (free to rotate) in the base. Thus, rotation of the axially-fixed adjustment screw causes movement of the slide and the ball stud with respect to the base housing. Because the base is fixed to the headlamp assembly support frame and the ball is engaged in a socket in the reflector, rotation of the adjusting screw causes changes in the orientation of the reflector within the assembly and the aim of the lamp is thereby adjusted.
In certain applications, the adjuster must include a VHAD. U.S. National Highway Traffic Safety Administration (“NHTSA”) standards require that horizontal adjuster mechanisms be either non-readjustable after the proper aim has been achieved or be equipped with a non-recalibratable VHAD. Currently, VHADs are required for horizontal adjusters but not for vertical adjusters. The VHAD used in the sliding adjuster includes an indicator plate with a post extending therefrom. The post includes a groove with a partial helical twist and is axially fixed (free to rotate) with respect to the base housing. A tab jutting from the slide is disposed in the groove. The indicator plate is positioned on the base near the adjustment screw such that indicator lines on the plate can be seen by the person adjusting the aim of the lamp. The base includes aiming rails behind the plate that, in connection with the indicator lines, allow the person making the adjustment to perceive how much of an adjustment has been made. Because the groove includes a partial helical twist, as the tab jutting from the slide moves along the groove with movement of the slide, the post and indicator plate are caused to rotate. The scale of the movement of the plate as reflected in the indicator lines is designed to reflect the corresponding movement of the reflector. If no VHAD is required, the indicator plate and post are simply not installed in the sliding adjuster.
The new design has numerous benefits that make it advantageous for use in connection with reflector style headlamps. The new design allows precise control of reflector aim, has smooth operational characteristics, can include a VHAD, and effectively maintains adjustment. Further, the new adjuster can be used where the area above and behind the lamp is inaccessible and it is cost effective to manufacture and install.
While the present invention is particularly useful in automotive headlamp assemblies, other applications are certainly possible and references herein to use in a headlamp assembly should not be deemed to limit the application of the present invention. Rather, the present invention may be advantageously adapted for use where similar performance capabilities and characteristics are desired. These and other objects and advantages of the present invention will become apparent from the detailed description, claims, and accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a perspective view of a sliding headlamp adjuster constructed in accordance with one embodiment of the present invention;
FIG. 2 is a front view of a sliding headlamp adjuster constructed in accordance with one embodiment of the present invention;
FIG. 3 is a rear view of a sliding headlamp adjuster constructed in accordance with one embodiment of the present invention;
FIG. 4 is a section detail of the rear view of a sliding headlamp adjuster constructed in accordance with the embodiment of the present invention shown in FIG. 3 ;
FIG. 5 a is cross-sectional view of the adjustment screw shown in FIG. 6 taken generally along the line 5 a — 5 a;
FIG. 5 b is a perspective view of a portion of the adjustment screw shown in FIG. 6 ;
FIG. 5 c is a section detail of the threads of the adjustment screw shown in FIG. 5 b;
FIG. 6 is a partial cross-section of the sliding headlamp adjuster in FIG. 3 taken generally along the line 6 — 6 ;
FIG. 7 is a partial front view of a sliding headlamp adjuster in accordance with one embodiment of the present invention wherein the adjustment screw is being rotated in the direction of arrow 92 resulting in movement of the VHAD indicator plate in the direction of arrow 96 ;
FIG. 8 is a perspective view of a sliding headlamp adjuster in accordance with one embodiment of the present invention with the adjustment screw being rotated in the direction of arrow 92 resulting on movement of the VHAD indicator plate in the direction of arrow 96 and the ball stud in the direction of arrow 94 ;
FIG. 9 is another rending of the cross-section shown in FIG. 6 with the adjustment screw having been rotated such that the slide is in a different position from that shown in FIG. 6 ;
FIG. 10 is partial front view of a sliding headlamp adjuster in accordance with one embodiment of the present invention wherein the adjustment screw is being rotated in the direction of arrow 98 resulting in movement of the VHAD indicator plate in the direction of arrow 100 ;
FIG. 11 is a side view of a sliding headlamp adjuster in accordance with one embodiment of the present invention installed in a headlamp assembly;
FIG. 12 is a schematic representation of the positioning of sliding headlamp adjusters in accordance with the present invention with respect to a headlamp assembly;
FIG. 13 is a front view of a sliding headlamp adjuster in accordance with one embodiment of the present invention shown in an installed position; and
FIG. 14 is a perspective view of a vehicle with which a sliding headlamp adjuster in accordance with the present invention might advantageously be used.
DETAILED DESCRIPTION
As shown in FIGS. 1 and 2 , a sliding headlamp adjuster (identified generally as 24 ) in accordance with one embodiment of the present invention includes a base housing 26 with a slide 28 disposed at least partially therein. The base housing 28 has one or more mounting tabs 30 such that the adjuster 24 can be mounted to the back of a headlamp assembly support frame 32 (see FIG. 11 ). The amount and configuration of the tabs 30 can be configured as necessary for particular installations. Alternatively, a quarter-turn mounting system could be used. The base housing 26 has interior channels 34 running along its sides 36 . When viewed from the exterior, e.g., FIG. 1 , the channels 34 appear rectangular in cross-section. However, as shown in FIG. 3 and in detail in FIG. 4 , on the interior, the channels 34 have a generally sideways T-shaped open cross section with a top T portion 38 , a bottom T portion 40 and a narrower neck T portion 42 .
As shown in FIGS. 3 and 4 , the slide 28 has rails extending from each of its sides. The rails include an upper rail 44 and a lower rail 46 . Each rail includes a leg 48 with a foot 50 extending therefrom. The rails 44 and 46 are disposed within the channels 34 so as to allow the slide 28 to move with respect to the base housing 26 . As shown in FIG. 8 , rails 44 and 46 extend along the side(s) of the slide and provide ample length of engagement to allow a smooth sliding movement and to resist binding. As shown in FIG. 4 , the leg 48 of the lower rail 46 interfaces with the neck portion 42 of the channel 34 . Because this interface is relatively near to the base of the leg 48 , there is little flex of the leg 48 . The foot 50 of upper rail 44 interfaces with the top T portion 38 of the channel 34 such that the leg 48 is flexed at an angle as indicated by arrows 52 which reflect the difference from straight of the leg 48 . The continually flexed engagement of the upper rail 44 with the channel 34 helps reduce any “play” or “slop” in the operation of the adjuster 24 , reduces problematic headlamp “flutter” (flutter is the apparent flickering of a headlamp caused by an improperly secured headlamp that moves when a vehicle hits a bump), and maintains the adjuster 24 in the desired adjustment. This resistance to “flutter” is typically tested by applying a set force to the ball stud 52 in the opposite direction of arrow 94 as shown in FIG. 8 while measuring the resulting deflection of the ball stud 52 in the same direction. In this test, deflection of the ball stud 52 is resisted primarily by the rigidity of the slide 28 , the slide rail 44 and housing channel 34 connection described, and the connection points of adjustment screw 58 . The rail and channel connection is subjected to a bending moment when the test load is applied urging the slide to rock in the rail channel. Minimizing rocking of the slide in the rail channel area as result of this bending moment minimizes deflection of the ball stud 52 . Since the leg 48 in the lower rail 46 resists flex, a greater resistance to rocking and hence to deflection is achieved. While this configuration for the engagement between the rails 44 and 46 and the channels 34 has been found effective, alternative configurations could also be effective. Similarly, while it has been found effective to have two rail/channel engagements, one on each side of the base housing 26 and slide 28 , other numbers and configurations could be used. For example, if additional stability is desired, an additional rail/channel could be provided.
As shown in FIG. 11 , a ball stud 52 extends from the slide 28 passing through the base housing 26 and the assembly support frame 32 and into the headlamp assembly 22 . The ball 54 of the ball stud 52 is engaged in a socket (not shown) in the reflector 56 so that axial movement of the ball stud 52 causes movement of the reflector 56 . The ball stud 52 is caused to move along its axis by movement of the slide 28 along the channels 34 in the base housing 26 . Movement of the slide 28 results from rotation of an adjustment screw 58 that is threaded into the slide 28 .
As shown in FIG. 5 b , the adjustment screw 58 has a head 62 , a narrow neck portion 64 , and a threaded portion 68 . The adjustment screw 58 is free to rotate and is secured in axial position in the base housing 26 by a screw retainer clip 60 ( FIGS. 1 and 2 ) that snap-fits around the narrow neck portion 64 of the adjustment screw 58 . Because the adjustment screw 58 is threaded into the slide 28 but is axially fixed and free to rotate with respect to the base housing 26 , when the adjustment screw 58 is rotated it causes movement of the slide 28 with respect to the base housing 26 . Thus, rotation of the adjustment screw 58 causes movement of the ball stud 52 with respect to the base housing 26 . Because the base housing 26 is fixed to the headlamp assembly support frame 32 and the ball 54 is engaged in a socket in the reflector 56 , rotation of the adjusting screw 58 causes changes in the orientation of the reflector 56 within the assembly 22 and the aim of the lamp is thereby adjusted.
As shown in FIGS. 5 a and 5 b , the adjustment screw 58 may include an anti-thread-stripping plate 66 between the narrow neck portion 64 and the threaded portion 68 . The anti-thread-stripping plate 66 is a disc-shaped protrusion from the shaft of the adjustment screw 58 that has one or more engagement barbs 70 . The purpose of the anti-thread-stripping plate is to reduce the possibility of the threaded portion 66 of the adjustment screw stripping the plastic threads in the slide 28 when an over-adjustment is attempted. As best visualized by referring to FIG. 9 , if the adjustment screw 58 is rotated to the point where the slide 28 abuts the anti-thread-stripping plate 66 , the engagement barbs 70 project into the end of the slide 28 to prevent further rotation of the adjustment screw 58 . Thus, stripping of the threads in the slide 28 in which the adjustment screw 58 is engaged is prevented because the adjustment screw 58 cannot be further rotated. The adjustment screw 58 can be rotated to release the engagement barbs 70 to restore the normal operation of the adjuster 24 .
Preferably, the base housing 26 and slide 28 are manufactured from glass-filled nylon using conventional injection molding processes. The ball stud 52 is preferably made from steel and manufactured in a conventional cold-heading process. Due to the possible exposure to harsh elements, manufacturing the adjustment screw 58 from a zinc alloy using a die casting method is preferably to help prevent corrosion and increase durability. As shown in FIGS. 5 b and 5 c , the threaded portion 68 of the adjustment screw 58 has flattened sides 72 and a forty-five degree thread angle. The flattened sides 72 , while facilitating manufacture of the adjustment screw 58 using a die-cast process, are advantageous in that they facilitate a thread-forming initial threading of the adjustment screw 58 into the slide 28 . Similarly, the forty-five degree thread angle is advantageous in the thread forming because it requires the displacement of a minimal amount of material while maximizing the strength of the threads in the slide 28 . The combined use of a forty-five degree thread angle and flattened sides 72 is helpful in achieving a low drive torque, low prevailing torque, and a resistance to stripping. Of course, other materials and part configurations could be used for particular designs and the description herein of particular materials and configurations should not be deemed to limit the scope of the invention. For example, the ball stud 52 could be manufactured from plastic or a metal other than steel and other plastics or materials could be used to form the base housing 26 and slide 28 .
In certain applications, the adjuster 24 must include a VHAD. Preferably, the VHAD used in the sliding adjuster (identified generally as 74 ) includes an indicator plate 76 with a post 78 extending therefrom. The post 78 includes a groove 80 with a partial helical twist 62 ( FIGS. 6 and 9 ) and is axially fixed (free to rotate) in a snap fit to the base housing 26 . A tab 84 jutting from the slide 28 is disposed in the groove 80 . The indicator plate 76 is positioned on the base 26 near the adjustment screw 58 such that indicator lines 86 on the plate 76 can be seen by the person adjusting the aim of the lamp. The base housing 26 includes aiming rails 88 behind the plate 76 that, in connection with the indicator lines 86 , allow the person making the adjustment to perceive how much of an adjustment has been made. Because the groove 80 includes a partial helical twist 62 , as the tab 84 jutting from the slide 28 moves along the groove 80 with movement of the slide 28 , the post 78 and indicator plate 76 are caused to rotate. The scale of the movement of the indicator plate 76 with respect to the aiming rails 88 is designed to reflect the corresponding movement of the reflector 56 within the assembly 22 . If no VHAD is required, the VHAD 74 is simply not installed in the sliding adjuster 24 . While other materials could be used, manufacture of the VHAD 74 from nylon using an injection molding process is preferable.
As shown in FIGS. 11 , 12 and 13 , the sliding headlamp adjuster 24 is installed to the rear of the headlamp assembly 22 using the mounting tabs 30 . The ball stud 52 extends into the assembly 22 through the support frame 32 where the ball 54 is disposed in a socket in the reflector 56 . An o-ring 57 may be disposed about the ball stud 52 to provide a seal between the shaft of the ball stud 52 and the assembly support frame 32 . A lens 90 covers the front of the support frame 32 and protects the reflector 56 and bulb (not shown) from the elements assailing the front of the vehicle. In FIG. 12 , the left adjuster 24 controls the horizontal movement of the reflector 56 and is thus equipped with a VHAD 74 . The right adjuster 24 controls the vertical movement of the reflector 56 and is not equipped with a VHAD. As shown in detail in FIG. 13 , the adjustment screw 58 and VHAD indicator plate 76 are positioned such that they are visible and accessible from the front of the vehicle between the lens 90 and the bumper 21 . The indicator plate 76 includes indicator lines 86 that are appropriate for reflecting adjustment when the adjuster is installed on either side of a vehicle. A portion of the indicator plate 76 is covered by the assembly support frame 32 or lens 90 such that the indicator lines 86 that are visible through the gap will properly reflect the adjustment being made. Such a covering of the indicator plate 76 allows the manufacturer to supply one adjuster for installation on both sides of the vehicle. Alternatively, the indicator plate 76 could have indicator lines that are specifically arranged for a particular side of the vehicle.
The operation of the sliding headlamp adjuster 24 to effectuate adjustment of the reflector 56 once installed is quite simple. As shown in FIG. 8 and in detail in FIG. 7 , rotation of the adjustment screw 58 in the direction indicated by arrow 92 causes the slide 28 to move toward the head 62 of the adjustment screw 58 . This movement of the slide 28 results in the movement of the ball stud 52 in the direction indicated by arrow 94 . As the tab 84 that extends from the slide 28 into the groove 80 moves with the slide 28 , the tab 84 is caused to move within the groove 80 and along the partial helical twist 82 . Movement of the tab 84 along the partial helical twist 82 causes a rotation of the post 78 and indicator plate 76 of the VHAD 74 in the direction indicated by arrow 96 . The amount that that the ball stud 52 has moved (and caused adjustment of the reflector 56 ) is shown by reference to the indicator lines 86 and aiming rails 88 .
Operation of the adjuster 24 to effectuate movement of the ball stud 52 in the opposite direction of that described in the immediately preceding paragraph is shown in FIG. 10 . In such operation, the adjustment screw 58 is rotated in the direction indicated by arrow 98 which causes the slide 28 to move away from the head 62 of the adjustment screw 58 . This movement of the slide 28 results in the movement of the ball stud 52 in the direction opposite that indicated by arrow 94 in FIG. 8 . As the tab 84 that extends from the slide 28 into the groove 80 moves with the slide 28 , the tab 84 is caused to move within the groove 80 and along the partial helical twist 82 . Movement of the tab 84 along the partial helical twist 82 causes a rotation of the post 78 and indicator plate 76 of the VHAD 74 in the direction indicated by arrow 100 . The amount that the ball stud 52 has moved (and caused adjustment of the reflector 56 ) is shown by reference to the indicator lines 86 and aiming rails 88 .
As illustrated by the foregoing description and shown in the Figures, the present invention is more suitable as a headlamp adjuster than are conventional adjusters. The present invention overcomes the limitations and disadvantages of existing adjusters by utilizing an effective design which allows precise control of reflector aim, has smooth operational characteristics, effectively maintains adjustment, can be used where the area behind and above the lamp is inaccessible, and which is cost effective and efficient to manufacture and install.
Although the invention has been herein shown and described in what is perceived to be the most practical and preferred embodiments, it is to be understood that the invention is not intended to be limited to the specific embodiments set forth above. Rather, it is recognized that modifications may be made by one of skill in the art of the invention without departing from the spirit or intent of the invention and therefore, the invention is to be taken as including all reasonable equivalents to the subject matter of the appended claims.
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A headlamp adjuster for adjusting the position of a reflector includes a base housing with a slide positioned at least partially therein. The base housing has mounting tabs so that the adjuster can be secured to the back of a headlamp assembly support frame. The base housing also has channels along its sides in which rails extending from the slide are disposed. A ball stud extends from the slide, the ball of which engages the reflector within the headlamp assembly such that axial movement of the ball stud causes movement of the reflector. Movement of the slide is caused by rotation of an adjustment screw that is threaded into the slide but held in axial position with respect to the base housing. The adjuster may include a vehicle headlamp aiming device (“VHAD”) if required for the particular application.” A marked-up version showing the changes is enclosed herewith in accordance with 37 CFR §1.121 (b)(iii).
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This application is a continuation of my prior copending provisional applications Ser. No. 60/003,242, filed Sep. 5, 1995 and Ser. No. 60/011,540, filed Feb. 13, 1996.
This application is a continuation of my prior copending provisional applications Ser. No. 60/003,242, filed Sep. 5, 1995 and Ser. No. 60/011,540, filed Feb. 13, 1996.
This invention relates to forms into which concrete is poured in order to erect a concrete wall, and to walls made with the new forms.
BACKGROUND OF THE INVENTION
Generally, forms for building walls have been made of wood or steel but there has been a growing trend to make such forms of a low density foam. There are a number of these low density foam forms in the prior art and on the market. The most widely used type of these forms comprises a pair of parallel vertical foam panels spaced apart by the thickness of the wall. The forms are held in place by plastic or metal support members that extend completely through both of the parallel panels. The panels are protected against outward forces, exerted by the fluid concrete, by backing plates that are adjacent to the exterior walls of the panels and are mechanically interconnected by the tieing means. Examples of such constructions include my U.S. Pat. No. 4,516,372 dated May 14, 1985, and U.S. Pat. No. 4,879,855 to John L. Berrenburg dated Nov. 14, 1989.
One problem with most of the low density forms now on the market is that they are made in a factory some distance from the locations of dealers and builders. Since the more common types of the low density forms on the market have the panels thoroughly braced by rigid tieing means, the dealers and builders must stock a different set of the forms for each width of wall that may be built. Further, when these forms are shipped they take up much space because there is much empty space between the panels. There are foam blocks on the market that avoid the above problems but they are inherently weak since there is nothing embedded in the form and any backing for the forms is minimal.
It is an object of the present invention to overcome all of the problems associated with the above-mentioned low density foam forms.
SUMMARY OF THE INVENTION
My invention has foam panels of about the same size, shape and material as the foam forms referred to above; that is each panel is about four feet long, 1.5 feet high and two inches thick. Each of my panels has an internal structure embedded in the panel, which in combination with backing plates preserves the panel against distortion during the pouring of the fluid concrete. My panels, however, are not interconnected at the factory. The lack of a factory connection permits the panels to be shipped stacked one upon the next without any intervening spaces between panels.
When the panels arrive at the construction site, pairs of panels are joined with the tie member of a length equal to the desired width of the concrete wall. Hence, the panels can be joined by tieing members, by the dealer or builder, avoiding the necessity of stocking a different set of panels for each wall thickness.
The particular form of the tieing means between panels and of the connection of the tieing means to the structural elements in the panels is also part of my invention.
Another feature of this invention is that the backing plates on one form may overlap a small portion of an adjacent form.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is an isometric view of one form of the invention.
FIG. 2 is an isometric view of an inside face of a panel which is part of the invention.
FIG. 3 is a cross section of one of the panels of the invention.
FIG. 4 is an isometric view of a strong structure that is partially embedded in the foam forms of the invention.
FIG. 5 is a tieing means that ties two panels together.
FIG. 6 is a schematic drawing of the mold, the structure that goes in the mold and the pipe for feeding the plastic into the mold.
FIG. 7 is a concrete wall constructed with the formwork of this invention.
FIG. 8 is a partial isometric view of the preferred form of panel, and backing plates, showing in particular the outer surface.
FIG. 9 shows two panels one stacked on the other.
FIG. 10 is a front view of a connecting means.
FIG. 11 is a front view of the tieing means that cooperates with the two strong structures in the two panels to hold them together.
FIG. 12 is a cross-sectional view through the assembled panels showing in particular the two strong structures tied together with the tieing means.
FIG. 13 is an isometric view showing two sockets, one for each of two of said strong structures.
FIG. 14 is an isometric view of a modified form of the invention.
FIG. 15 is a cross-sectional view of a form that embodies the invention.
DETAILED DESCRIPTION
Hereinafter, whenever I refer to foam forms, I will be referring to low density foam materials such as polyurethane may be used, having a density below 4.5 pounds per cubic foot (4.5 p/cf) and preferably has a density in the range of 1.5 to 3 P/CF. Further details of a suitable foam are set forth in column 6 of my patent U.S. Pat. No. 4,516,372. Other low density materials such as polystyrene, may be used. The low density materials will remain a part of the concrete wall and act as an insulator for the wall. If the wall is an outside wall of a building the insulation will reduce heating and cooling costs, as well as reduce sound transmission.
FIG. 1 shows one form of the invention. There are two low density foam panels 10 which were separate from each other during manufacture at the factory and shipping to the dealer or builder. These two panels 10 have inner faces 10a that include sockets 14 as shown in FIG. 2. Each panel has at least one and preferably several strong structures (FIGS. 3 and 4) which comprise a backing plate 12, a socket 14 and strong connecting members 15 that connect the socket to the backing plate. The two sockets 14 on the two panels 10, respectively are interconnected by the inside tie shown in FIG. 5. The inside tie has two strips 11 which are pointed at their lower ends 16, and which are also connected to each other by internal strong members 17. Two or more of the ties of FIG. 5 may be connected by a member 18 so that they can be installed as a unit.
The apparatus shown in FIGS. 4 and 5 is quite strong as compared to the strength of the low density foam panels.
The low density foam forms 10, in the absence of the strong structures of FIGS. 4 and 5 would be destroyed or at least distorted, when used to build a concrete wall. Great force on the panels 10 occurs when the panels are stacked and fluid concrete is poured into the space between the panels 10. The strong structures of FIGS. 4 and 5 are used to not only space the panels apart by a distance equal to the thickness of the concrete wall but to also provide strength to the panels 10. This permits pairs of panels to be installed as a unit and also prevents lateral movement of the panels.
As shown in FIGS. 1 and 2 there are five strong structures . (FIGS. 3 and 4) in each panel 10. Hence there are five tieing member (FIG. 5) for each pair of panels. Each of the five strong structures of FIG. 4 that are in each panel 10, have a backing plate 12, a socket 14 and members 17. The strong structures of FIGS. 3 to 5 perform at least two major functions. First, they strengthen the panels in two ways. The first of these ways is that since the structural elements 15 were molded into the panels and the backing plates 12 and the sockets 14 abut the surfaces of the panels 10, the panels 10 are strengthened. The backing plates act as bearing plates, distributing the stresses over a greater area of the foam panel. Secondly, the backing plates 12 may support wall coverings of all types. If the wall is an outside wall of a building, the exterior face 10b of the panel 10, that is on the outside of the building, may support siding or any other outside wall covering. Inside the building, the outer face 10b of the panel 10 may support dry wall, sheetrock, etc.
The prior art teaches backing plates on (or in indents in the foam panel) foam panels, but my backing plates 12 are an improvement since they have a portions 13 which actually overlap the joints between the panels 10 of first pair of panels and a second pair of panels that are above the first pair. Moreover, my backing plates also act as bearing plates. Moreover, the portions of my backing plates that overlap can be fastened together. That is, the backing plate portion 13 can be fastened by a screw 13a to backing plate 12d (see FIG. 9).
The foam panels 10, with the strong structure of FIG. 4 embedded therein are made at a factory, and are shipped to a dealer or builder at or near the construction site. Prior art forms, which have internal structural support and/or backing plates, have the internal strong supports molded in one piece that goes from a backing plate on one panel, through that panel, through the wall, and through the other panel. As a result, when the form is shipped the several cubic feet of space between the walls takes up room on the truck and limits the number of panels that can be carried by one truck. With my invention, the above waste space is avoided since my inside tie (FIG. 5) is installed at the construction site.
Moreover, the prior art devices now on the market, which have embedded structure, are limited in another way. If they are to be stocked by a local dealer, that dealer must have one set of forms for each thickness of wall that may be called for. With my invention, the panels 10 are the same for every wall thickness. To get various wall thicknesses, the only thing necessary is to stock different ties of the type shown in FIG. 5.
Each of the panels 10 is identical to the other ones. Each panel 10 has an inner face 10a facing the other form 10 and each panel has an outer face 10b. Mounted on each inner face 10a is a connecting means 14 (see FIG. 4) which may be engaged by the tieing means of FIG. 5 as previously explained. Each panel 10 has a connecting wall 10c that connects the inner face 10a to the outer face 10b. The connecting wall 10c has a periphery that runs along the top of wall 10, down the far end of FIG. 1, along the length of the connecting wall 10c that runs along the bottom of panel 10, and thence upwards along the connecting wall 10c at its near end.
Walls made with panels 10 of the shape shown in FIGS. 1 and 2 have a so-called "post and beam configuration". The shape of the panels for making the post and beam construction is old and well known. That configuration is preferred by some architects and I therefore have shown how to apply my invention to it. I prefer, however, that the panels 10 have a uniform rectangular cross-section and panels of that shape are contemplated for all forms of the invention hereinafter described.
In order to provide a form for a concrete wall, the forms of FIG. 1 are stacked on one another, as well as end to end to create a form for a wall. The fact that the backing plates extend high enough to cover the joints as explained above aids in stacking the forms. The extensions 13 on the backing plates 12 make it easier to stack the forms and also maintains the outer wall of the forms smoother and flatter. The extensions 13 also, when attached to backing plates 12d by screws 13a, stabilizes the forms. Moreover, the fact that I employ shiplap joints between stacked forms cooperates with the extensions 13 to improve the flatness of the outer wall (both the wall on the outside of the building that carries the siding and the wall on the interior of the building that carries the dry wall).
FIG. 8 shows the preferred form of the invention. The panels 10 have a uniform rectangular cross-section along the entire length of the panel. Each panel has backing plates 12 with the extensions 13 as explained above. Each backing plate is connected by a strong structure to a connecting means (socket plate) 14a which has two keyhole-shaped sockets 15A (FIG. 10). Since there is a second panel 10 parallel to the first one, the second panel 10 also has a connecting means (socket) 14a with two keyhole sockets 15A. There is a tieing member 16, 17 having four enlarged plugs 18. When the plugs 18 of FIG. 11 are inserted into the keyhole slots 15, and the plugs moved downward to lock the plugs 18 into sockets 15A, the two panels are rigidly attached together as shown in FIG. 12.
FIG. 9 illustrates the overlap of the backing plates. This figure shows the panel 10f stacked on a panel 10e. The panel 10e has an indent 10g which extends inwardly from the outer face 10h of the panel and also extends to the periphery 10j of the panel 10e. The panel 10f has a projection 10k that mates with the indent 10g. The panel 10f has a backing plate 12d which extends along the surface of panel 10f to the lower end of the projection 10k. The backing plate 12e extends along the surface of panel 10e and upwardly to overlap at 13 both said projection 10k and a limited portion of backing plate 12d.
It is evident that when panel 10f has yet to be inserted in mating relation with panel 10e, that the backing plate 12e projects in spaced relation to, and parallel to wall 10m of panel 10e. This results in a short open slot in the upper side of panel 10e as shown in FIG. 1. The presence of this slot makes it easy to guide the projection 10k into the slot that is between wall 10m and backing plate extension 13 (FIG. 9). Moreover, the overlapping portion 13 of backing plates (such as 12e) and the projections such as 10k, result in a smoother, flatter outer surface of a series of stacked panels. Irregularities in the outer faces of the panels can distort the wall coverings that may be attached to the backing plates.
The connecting means 14A of FIG. 10 when mounted on one of the panels 10 (FIG. 12) can be tied to a similar connecting means on the other panel 10 of FIG. 12 by the tieing means of FIG. 11. In FIG. 12, each of the connecting means 14A is connected to a backing plate 12 by a strong structure 19.
The concrete form of FIG. 12 is made as shown in FIG. 6 and as follows. At a factory each panel 10 is molded as follows: The connecting means 14A, the strong structures 15 and the backing plates 12 that are a part of a panel will be placed in a mold M (FIG. 6): If the panel requires the protection of several backing plates all of them will be in the mold along with their strong structures 19 and their connecting means:) The foam is then fed into the mold via pipe P to embed all of the parts in the mold.
The molded panels are then shipped separately, and joined together with said tieing means at the construction site.
The builder at the construction site may select the thickness of the concrete wall by selecting a tieing means to give the desired width of wall.
FIG. 13 shows a modified form of tieing means. With this tieing means there is a strong structure 20, 21, 22 holding four slotted strips 23 that can engage suitable connecting means having a vertical strip.
FIG. 14 shows another form of connecting means 25 in the form of a wide vertical strip. This strip is connected to a backing plate by strong structure 24.
FIG. 15 shows how the connecting means 25 of FIG. 14 on two panels can be held from outward movement, despite the force of fluid concrete. The tieing means has strong structure 20, 22 and sockets 21.
Thus, FIG. 15 shows a complete form embodying two panels 12, each having the structure of FIG. 14 molded into it. A flat strip 25 (FIG. 14) is adjacent the inner surface of each panel 12 of FIG. 15. The apparatus 20, 21, 22 (see FIG. 13) has C-shaped grooves 23 which mate with the strips 25 (FIG. 14). The apparatus of FIG. 13 is added to the two panels 12 at the job site.
FIG. 7 illustrates a wall constructed on a previously poured concrete base 56 using a plurality of panel assemblies 10. The wall is formed by taking numerous panel assemblies 10, as described above, and placing them one on top of the other and edge-to-edge on concrete base 56 until a complete wall is formed. The lower edge of the bottom panel 12 rests on wood cleats 48 which are in turn fastened to concrete base 56 by concrete nails 50. The purpose of using wood cleats 48 is, of course, to stabilize the wall being constructed both in a horizontal and vertical direction and to help keep the wall plumb during the pouring of concrete 28.
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Foam forms for use in making a concrete wall are disclosed together with a method of making the forms. The forms are stackable to form a cavity that receives the concrete. Each form has two identical panels. The panels are molded separately by first placing a structure, consisting of backing plates that will be along one side of the mold, connecting members that will be along the opposite side of the mold and an apparatus that connects the backing plates to the connecting members, in the mold. The mold is then filled with foam which cures and produces a panel with the backing plates, connecting members and apparatus molded into the panel. The molded panels are then shipped to the job site where the forms are assembled. Each form is assembled as follows: The connecting members on one panel are interconnected, by tieing means, to the connecting members on a second panel to provide a form.
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BACKGROUND OF THE INVENTION
The present invention relates to a data alignment correction apparatus for performing alignment correction of a data structure in order that it is properly formatted for a different computer architecture.
In general, when a data structure such as the structure of C language shown in FIG. 1 is processed by a compiler, a head of a word must be aligned to a halfword or fullword boundary. The resultant structure differs depending on the computer and compiler used. This is because computer architectures relating to memory access differ from one model to another. For this reason, when a C language file is planted from one computer to another, the file cannot be directly used if the architectures of the two computers are different. This problem is posed when, for example, a word in the file is written in a specific structure or a header of a communication protocol is output in a specific structure. Therefore, the file cannot be commonly used, and communication cannot be performed even though the same programming language is used, a user cannot use the file.
Therefore data alignment of the data structures must be performed. Conventionally, alignment correction of a structure has been performed by software processing using a special subroutine. However, in order to perform alignment correction by software, a separate subroutine must be formed for each structure, and it takes a very long time to create the software.
SUMMARY OF THE INVENTION
The present invention has been developed in consideration of the above situation and has as its object to provide a data alignment correction apparatus which can perform alignment correction of a data structure at a high speed by a common processing routine. The apparatus comprises: first storage means for storing a source data structure, second storage means for sequentially storing an object data structure, alignment data storage means for storing alignment data corresponding to the source data structure, the alignment data including a plurality of alignment data blocks each corresponding to one of said source data blocks, and central processor means for selectively reading out said source data blocks from said first storage means, said selection being in accordance with the corresponding alignment data blocks from said alignment data storage means, and for outputting the selected source data blocks to said second storage means for storage as object data blocks in said object data structure. The central processor sequentially reads out the alignment data blocks from the alignment data storage section in response to an alignment correction instruction. When the alignment data block is a predetermined value, the source data block is read out from the first storage section and stored to the second storage section. When the alignment data block does not match a predetermined value, the next alignment data blocks is read out from the alignment data storage section without storing the source data element. In this manner, the source data blocks are transferred in accordance with the alignment data blocks, thereby performing alignment correction of the structure.
As described above, according to the present invention, when a program created in one computer is to be run in another (i.e. different) model, alignment correction for a required structure can be performed at a high speed by a common processing subroutine by merely preparing alignment data, regardless of the type of the structure.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 shows a conventional C language data structure;
FIG. 2 is a block diagram of an arrangement of an alignment correction apparatus according to an embodiment of the present invention;
FIGS. 3A and 3B are flow charts for explaining an operation of the first embodiment in FIG. 1;
FIG. 4 is a view of alignment data used to perform alignment correction of a structure having a 4-byte boundary into a structure having a 2-byte boundary;
FIGS. 5A and 5B are views having the structures of 4- and 2-byte boundaries, respectively, to which the alignment data in FIG. 4 is applied;
FIG. 6 is a view of a modification of the alignment data in FIG. 4;
FIG. 7 is a view of alignment data used to perform alignment correction of a structure of 4-byte boundary in a 32-bit machine into a structure of 1-byte boundary in a 16-bit machine;
FIGS. 8A and 8B are views of the structures of 4- and 1-byte boundaries, respectively, to which the alignment data in FIG. 7 is applied;
FIG. 9 is a flow chart for explaining an operation of alignment correction of a structure having a 1-byte boundary in a 16-bit machine into a structure having a 4-byte boundary in a 32-bit machine;
FIG. 10 is a view of the alignment data used in the operation of FIG. 9;
FIGS. 11A and 11B are views of the structures having a 4- and 1-byte boundaries to which the alignment data in FIG. 10 is applied; and
FIG. 12 is a view for explaining a routine of obtaining an object data structure by alignment processing.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
An embodiment of the alignment correction apparatus according to the present invention will now be described below, with reference to the accompanying drawings.
First, referring to FIG. 2, the arrangement of an embodiment of the alignment correction apparatus according to the present invention will be described in detail. In FIG. 2, source data structure storage section 11 stores at least one source data structure 20. Object data structure storage section 12 stores an object data structure 21 which is obtained by correcting the alignment of the source data structure stored in section 11. Alignment data storage section 13 stores alignment data which corresponds to the alignment relationship between the source and object data structures. The number of alignment data stored in section 13 depends on the number of types and the source data structures.
The alignment data includes bit groups. Each bit group (alignment data block) determines whether a data byte (data block) of the source data structure is to be retained or deleted during the alignment correction procedure. A data byte to be deleted is padding data which is inserted for alignment correction. Each data byte of the source data structure is in 1:1 correspondence with each data bit of the alignment data. Therefore, when the size of the source data structure is 16 bytes, as is shown in FIG. 5A, the alignment data includes 16 bits. In this embodiment, each logic "1" bit of the alignment data represents that the corresponding data byte is to remain after correction, and each logic "0" represents that the data is to be deleted thereafter.
Returning to FIG. 2, the data alignment correction apparatus also includes size register section 14 for storing the byte size value of a source data structure, counter 15 for indicating the location of a byte to be accessed in source data structure, and instruction register section 19 for holding an instruction of an alignment correction routine. The alignment correction apparatus further includes counter 16 for indicating the location of a byte to be stored in storage section 12, counter 17 for indicating the location of a bit to be accessed in alignment data storage section 13, and CPU 18 for executing a variety of alignment correction instructions. Note that in this embodiment, source data structure, object data structure, and alignment data storage sections 11, 12, and 13, registers 14 and 19, and counters 15 and 17 are allocated in a main memory.
An alignment correction operation performed by the first embodiment will now be described below, with reference to the flow charts of FIGS. 3A and 3B. Assume that source data structure storage section 11 stores, as a source data structure, the structure shown in FIG. 5A, that size register section 14 stores the byte size value of the structure, i.e., "15", and that alignment data storage section 13 stores the alignment data shown in FIG. 4.
CPU 18 fetches an alignment correction instruction from instruction register section 19 and decodes it. As a result, in step S2, counters 15 to 17 are initialized to, for example, "0". By the alignment correction instruction, a source data structure and alignment data are designated, and a head location of object data structure storage section 12 storing for an object data structure is designated. In this embodiment, the alignment correction instruction is either a delete alignment correction instruction or an insertion alignment correction instruction. If the instruction is a delete alignment correction instruction, step S6 is sequentially executed subsequent to step S4. If the instruction is an insertion alignment correction instruction, step S18 is sequentially executed after step S4.
If the fetched instruction is a delete alignment instruction, bit 0 of the alignment data in storage section 13, designated by the content of counter 17 is read out in step S6. In step S8, CPU 18 checks whether the readout bit 0 data is logic "1". If Y (YES) in step S8, step S10 is executed. If N (NO) in step S8, step S16 is executed. In this case, since the alignment data is given as shown in FIG. 4, the bit 0 data is logic "1". Therefore, steps S8 and S10 are sequentially executed.
In step S10, byte data of the source data structure in storage section 11, designated as by the content of counter 159, is read out. The byte data is written in a location of storage section 12 as designated by the content of counter 16. As a result, the byte data read out from storage section 11 remains after correction. When step S10 is completed, the contents of counters 15, 16, and 17 are all incremented by "1" in step S12 and advance to the location of the next byte to be read out from source data storage section 11, the location of the next byte to be written to object data storage section 12, and the location of the next bit to be read out from alignment data storage section 17, respectively.
On the other hand, if the bit data of the alignment data is logic "0", as is bit 3 data, only counters 15 and 17 are incremented by "1", in step S16. As a result, the byte data, of the source data structure in storage section 11, as designated by the content of counter 15 is deleted after correction.
When step S12 or S16 is executed, the content of counter 15 and that of register section 14, i.e., the size value of the source data structure, are fetched 11 and CPU 18 checks whether the content of counter 15 exceeds the size value set in register section 14, in step S14. If N (NO) in step S14, CPU 18 determines that the alignment correction processing with respect to all the byte data of the source data structure is not completed, and the flow returns to step S6.
By repeatedly performing the alignment correction processing, the structure shown in FIG. 5B is generated from its start byte, in units of bytes, in storage section 12. When the count of counter 15 exceeds the size value set in register section 14, CPU 18 completes the alignment correction processing. In this manner, the delete alignment correction instruction is executed.
In the above description, one data byte of the source data structure corresponds to one data bit of the alignment data. However, when a structure having a 4-byte boundary is to be aligned to a structure having a 2-byte boundary, the alignment data can be reduced by causing 2-byte data of the source data structure to correspond to 1-bit data of the alignment data, as shown in FIG. 6. In this case, two bytes of source data is one source data block, and counters 15 and 16 are incremented by "2" in step S12 or S16.
The case wherein object file B including structure B is obtained from a source file will now be described below.
In this case, as is shown in FIG. 12, object file B can be obtained at S140 by compiling the source file by compiler B at S120 including alignment correction routine B as described above. When object file A compiled by compiler A at S110 including alignment correction routine A as described above is present at S130, object file C can be obtained at S150 by performing alignment correction processing by alignment correction routine C substantially the same as alignment correction routine B S120.
FIGS. 7 and 8A and 8B show alignment correction of a structure having a 4-byte boundary in a 32-bit machine into a structure having a 1-byte boundary in a 16-bit machine. An alignment correction processing routine is similar to that in steps S2 to S16 described above.
Alignment correction of a structure of 2-byte boundary shown in FIG. 5B into a structure of 4-byte boundary shown in FIG. 5A by insertion alignment correction will be described with reference to the flow charts of FIGS. 3A and 3B. In this case, the structure shown in FIG. 5B is stored in storage section 11, and a size value and alignment data corresponding to the structure are stored in register section 14 and storage section 13, respectively.
First, an alignment correction instruction is decoded. Then, if CPU 18 determines in step S4 that the instruction is the insertion alignment correction instruction, step S18 is executed. In this case, the alignment data is given as shown in FIG. 4, i.e., the same as that used in the case of the delete alignment correction instruction but may be different therefrom.
In step S18, bit data of the alignment data in storage section 13 designated by the content of counter 17 is read out. Then, in step S20, CPU 18 checks whether the readout bit data is logic "1". If Y (YES) in step S20, step S22 is executed. If N (NO) in step S20, step S28 is executed. In step S22, byte data of a source data structure in storage section 11 designated by the content of counter 15 is read out. The readout byte data is written in a location in storage section 12 designated by the content of counter 16. As a result, the byte data read out from storage section 11 remains after correction. When step S22 is completed, the contents of counters 15, 16, and 17 are all incremented by "1" in step S24 and advance to a position of the next byte to be read out, a position of the next byte to be written, and a position of the next bit to be read out, respectively.
On the contrary, if the readout bit data is logic "0", CPU 18 generates padding data. The generated padding data is stored in a location designated by the content of counter 16 of storage section 12. Thereafter, the contents of counters 16 and 17 are incremented by "1" in step S30.
When step S24 or S30 is executed, the content of counter 15 and the content of register section 14, i.e., the size value of the source data structure are read out, and CPU 18 checks whether the content of counter 15 exceeds the size value set in register section 14, in step S26. If N in step S26, CPU 18 determines that the alignment correction processing with respect to all the byte data of the source data structure in storage section 11 is not completed, and the flow returns to step S18.
As described above, by repeatedly performing the alignment correction processing, the structure shown in FIG. 5A is generated from its start byte in units of bytes in storage section 12. When the count of counter 15 exceeds the size value set in register section 14, CPU 18 completes the alignment processing. In this manner, the insertion alignment processing is executed.
The present invention can also be used to absorb a difference between the numbers of bits of "int" in 32- and 16-bit computers. Note that in order to extend a negative number from 2 bytes to 4 bytes, padding data of FFFFH and not 0000H must be used, etc. An operation in this case will be described with reference to FIGS. 9, 10, and 11A and 11B. First, a structure, alignment data, and a size value are designated by an insertion alignment correction instruction. A structure to be designated is shown in FIG. 11B and is stored in storage section 11. Alignment data to be designated is shown in FIG. 10 and is stored in storage section 13.
The basic operation is substantially the same as that used in the case of the insertion alignment correction instruction shown in FIGS. 3A and 3B except that steps S32 to S36 are executed instead of step S28.
If CPU 18 determines in step S20 that bit data is logic "0", step S32 is executed. In step S32, CPU 18 checks whether byte data designated by the content of counter 15 is start byte data in an integer area. Since a byte position where the integer area begins is indicated in the insertion alignment correction instruction, CPU 18 checks the content of counter 15 to determine whether the integer area is designated. If N (NO) in step S32, the flow advances to step S34, and the same processing as that in step S28 is executed.
If Y in step S32, byte data designated by the content of counter 15 is read out from storage section 11, and CPU 18 checks whether its MSB is logic "1" or "0". If the MSB is "0", padding byte data of "00"H is generated as described above. If the MSB is logic "1", padding byte data of "FF"H is generated. The generated padding data is stored in a location designated by the content of counter 16 of storage section 12. After step S34 or S36 is executed, processing similar to that in the case of the insertion alignment correction instruction shown in FIG. 3B is executed.
In the above embodiment, counters 15 to 17 are sequentially incremented. However, the content of counter 17 may be set in accordance with subinstructions of the alignment correction instruction. Each subinstruction includes information for designating a location of storage section 12 for byte data of the source structure which is to be stored. In this case, descriptions with respect to counter 17 can be omitted in steps S2, S16, S12, S24, and S30 can be also omitted, and the content of counter 17 may be set in accordance with the subinstructions in steps S6 and S20.
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An alignment correction apparatus includes: a first storage section for storing a source data stucture, a second storage section for sequentially storing input block data elements, an alignment data storage section, and a processor. The source data structure includes a plurality of data elements, and each block data element includes at least one data element. Alignment data includes a plurality of alignment data elements independently associated with the block data element. The processor sequentially reads out the alignment data elements from the alignment data storage section, in response to an alignment correction instruction. When the readout alignment data element is predetermined data, a block data element is read out from the first storage section and stored in the second storage section. When the readout alignment data element is not predetermined data, the next alignment data element is read out from the alignment data storage section.
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[0001] The present application claims the benefit of priority under 35 USC §119(e) to U.S. Provisional Patent Application 61/187,302 entitled “Anti-michotic Wallboard Tape”, filed Jun. 16, 2009, which is hereby incorporated, in its entirety, herein by reference.
FIELD OF THE INVENTION
[0002] This invention relates to paper products and/or substrates suitable for being made into wallboard tape (also may be known as joint tape and/or drywall tape) and having improved reduction or inhibition in the growth of microbes, mold and/or fungus. The paper substrate is characterized by its excellent physical properties including cross direction (CD) tensile, machine (MD) tensile, internal bond, wet tensile, hygroexpansivity, curl, bonding properties, bonding of joint tape to joint compound, etc. The paper product of the invention contains a sizing agent and an antimicrobial compound as well as other optional components including without limitation a binder. The paper product of the invention may be produced by contacting the plurality of cellulose fibers with each of the sizing agent, antimicrobial compound, and optional components at any point in the papermaking process, converting process, and/or post-converting process. Finally, the invention relates to methods of using the paper substrate.
BACKGROUND OF THE INVENTION
[0003] Wallboard (also known as drywall) has become the dominant material in the production of interior building partitions. In particular, interior building partitions generally comprise a studwall of spaced parallel vertical members (studs) which are used as a support for preformed panels (wallboard) which are attached to the studwall by screws, nails, adhesive or any other conventional attachment system. Obviously, joints exist between adjacent preformed panels. In order to provide a continuous flat surface to the wall, it is necessary to “finish” the joint between adjacent panels. Generally, such “finishing” may include the building up of multiple layers of a mastic material (joint compound) and the blending of this joint compound and paper substrate suitable for wallboard tape utility into the panel surface so as to form the desired flat and contiguous wall surface. In addition, wallboard tape may be used to bring together a plurality of panels forming a corner which may include but is not limited to corner bead.
[0004] In order to facilitate this finishing of the joints and/or corners, most manufacturers bevel the longitudinal edges of the wallboard panels so as to allow a build-up of mastic material which will then match the level of the major surface area of the preformed panel. Typically, the buildup of the mastic material in the joint area comprises the application of a first layer of mastic material, the embedding of a wallboard tape (for example a paper tape) in the first layer of mastic material and then the overcoating of the tape with one or more, generally two layers of additional mastic material. This finishing of the joints is a time consuming process, since it is generally necessary to wait 24 hours between each application of a coat of mastic material in order to allow the coat to dry before the application of an overcoat of an additional layer of mastic material. Moreover, it is then necessary generally to sand the joint area so as to produce a finish which will match the major portion of the surface area of the wallboard panels. The “finishing” process thus is both time-consuming and labor-intensive.
[0005] In addition to the above, it is desirable to, create building materials that are antimicrobial so that they resist or inhibit the growth of microbes such as bacteria, fungus, molds, and mildew.
[0006] Wallboard tape paper is a very challenging paper to make as there is a very narrow window of operation in which to achieve the required high tensile strengths while maintaining other good physical properties such as bonding properties, bonding of joint tape to joint compound, hygroexpansivity, curl, etc. The challenge to the next generation of wallboard tape paper substrate production is to program an addition antimicrobial function into what is already a very specific and stringent set of physical properties such as CD tensile, MD tensile, internal bond, wet tensile, hygroexpansivity, curl, bonding properties, bond of joint tape to joint compound, etc (which are demanded by wallboard tape paper substrate converters and users). Such levels of physical properties such as CD tensile, MD tensile, internal bond, wet tensile, hygroexpansivity, curl, bonding properties, bond of joint tape to joint compound, etc, have been achieved by conventional production of paper substrates under acidic conditions and alkaline conditions. However, an alkaline paper substrate suitable for wallboard tape converting (e.g. have acceptable physical properties such as CD tensile, MD tensile, internal bond, wet tensile, hygroexpansivity, curl, bonding properties, bond of joint tape to joint compound, etc) has been difficult to achieve.
[0007] Despite the considerable efforts, there exists a need for a wallboard tape to satisfy the construction industries' requirements wallboard tape having highly sought after physical properties and maintain sustainable antimicrobial properties.
BRIEF DESCRIPTION OF THE DRAWINGS
[0008] FIG. 1 : A first schematic cross section of just one exemplified embodiment of the paper substrate that is included in the paper substrate of the present invention.
[0009] FIG. 2 : A second schematic cross section of just one exemplified embodiment of the paper substrate that is included in the paper substrate of the present invention.
[0010] FIG. 3 : A third schematic cross section of just one exemplified embodiment of the paper substrate that is included in the paper substrate of the present invention.
[0011] FIG. 4 : A first pictorial representation of how wallboard and tape samples were tested for antimicrobial performance according to Example 1.
[0012] FIG. 5 : A second pictorial representation of how wallboard and tape samples were tested for antimicrobial performance according to Example 1.
[0013] FIG. 6 : A photograph showing the antimicrobial performance of Sample A after 62 days as measured by the process of Example 1.
[0014] FIG. 7 : A photograph showing the antimicrobial performance of Sample B after 62 days as measured by the process of Example 1.
[0015] FIG. 8 : A photograph showing the antimicrobial performance of Sample C after 62 days as measured by the process of Example 1.
[0016] FIG. 9 : A photograph showing the antimicrobial performance of Sample D after 62 days as measured by the process of Example 1.
[0017] FIG. 10 : A photograph showing the antimicrobial performance of Sample E after 62 days as measured by the process of Example 1.
[0018] FIG. 11 : A photograph showing the antimicrobial performance of Sample F after 62 days as measured by the process of Example 1.
[0019] FIG. 12 : A photograph showing the antimicrobial performance of Sample G after 62 days as measured by the process of Example 1.
[0020] FIG. 13 : A photograph showing the antimicrobial performance of Sample H after 62 days as measured by the process of Example 1.
DETAILED DESCRIPTION OF THE INVENTION
[0021] The present inventors have now discovered a paper substrate which, until now, was unable to meet the stringent physical properties required by the construction industries for useful wallboard tape application that also has sustainable antimicrobial properties, as well as methods of making and using the same.
[0022] The paper substrate of the present invention may contain recycled fibers and/or virgin fibers. Recycled fibers differ from virgin fibers in that the fibers have gone through the drying process at least once.
[0023] The paper substrate of the present invention may contain from 1 to 99 wt % of cellulose fibers based upon the total weight of the substrate, including 1, 5, 10, 15, 20, 25, 30, 35, 40, 45, 50, 55, 60, 65, 70, 75, 80, 85, 90, 95 and 99 wt %, and including any and all ranges and subranges therein.
[0024] Preferably, the sources of the cellulose fibers are from softwood and/or hardwood. The paper substrate of the present invention may contain from 1 to 99 wt %, preferably from 5 to 95 wt %, cellulose fibers originating from softwood species based upon the total amount of cellulose fibers in the paper substrate. This range includes 5, 10, 15, 20, 25, 30, 35, 40, 45, 50, 55, 60, 65, 70, 75, 80, 85, 90, 95, and 100 wt %, including any and all ranges and subranges therein, based upon the total amount of cellulose fibers in the paper substrate.
[0025] The paper substrate of the present invention may contain from 1 to 99 wt %, preferably from 5 to 95 wt %, cellulose fibers originating from hardwood species based upon the total amount of cellulose fibers in the paper substrate. This range includes 5, 10, 15, 20, 25, 30, 35, 40, 45, 50, 55, 60, 65, 70, 75, 80, 85, 90, 95, and 100 wt %, including any and all ranges and subranges therein, based upon the total amount of cellulose fibers in the paper substrate.
[0026] Further, the softwood and/or hardwood fibers contained by the paper substrate of the present invention may be modified by physical and/or chemical means. Examples of physical means include, but is not limited to, electromagnetic and mechanical means. Means for electrical modification include, but are not limited to, means involving contacting the fibers with an electromagnetic energy source such as light and/or electrical current. Means for mechanical modification include, but are not limited to, means involving contacting an inanimate object with the fibers. Examples of such inanimate objects include those with sharp and/or dull edges. Such means also involve, for example, cutting, kneading, pounding, impaling, etc means.
[0027] Examples of chemical means include, but is not limited to, conventional chemical fiber modification means. Examples of such modification of fibers may be, but is not limited to, those found in the following patents U.S. Pat. Nos. 6,592,717, 6,582,557, 6,579,415, 6,579,414, 6,506,282, 6,471,824, 6,361,651, 6,146,494, H1,704, 5,698,688, 5,698,074, 5,667,637, 5,662,773, 5,531,728, 5,443,899, 5,360,420, 5,266,250, 5,209,953, 5,160,789, 5,049,235, 4,986,882, 4,496,427, 4,431,481, 4,174,417, 4,166,894, 4,075,136, and 4,022,965, which are hereby incorporated in their entirety by reference.
[0028] The paper substrate of the present invention may contain an antimicrobial compound. The paper substrate's antimicrobial tendency may be measured in part by ASTM standard testing methodologies such as D 2020-92, E 2180-01, G 21-966, C1338, and D2020, all of which can be found as published by ASTM and all of which are hereby incorporated, in their entirety, herein by reference.
[0029] Antimycotics, fungicides are examples of antimicrobial compounds. Antimicrobial compounds may retard, inhibit, reduce, and/or prevent the tendency of microbial growth over time on/in a product containing such compounds as compared to that tendency of microbial growth on/in a product not containing the antimicrobial compounds. The antimicrobial compound when incorporated into the paper substrate of the present invention preferably retards, inhibits, reduces, and/or prevents microbial growth for a time that is at least 5, 10, 15, 20, 25, 30, 35, 40, 45, 50, 75, 100, 125, 150, 200, 250, 300, 350, 400, 450, 500, 550, 600, 700, 800, 900, 1000% greater than that of a paper substrate that does not contain an antimicrobial compound, including all ranges and subranges therein.
[0030] Antimycotic compounds are, in part, mold resistant. Fungicide compounds are, in part, fungus resistant. The antimicrobial compound may have other functions and activities than provide either mold resistance and/or fungus resistance to a product containing the same.
[0031] The antimicrobial compound may also be mildew, bacteria and/or virus resistant. A mold specifically targeted, but meant to be non-limiting, is Black mold as applied to the above-mentioned paper substrate of the present invention.
[0032] It is preferable for the antimycotic and/or fungicide to not be highly toxic to humans.
[0033] The antimycotic and/or fungicide may be water insoluble and/or water soluble, most preferably water insoluble. The antimycotic and/or fungicide may be volatile and/or non-volatile, most preferably non-volatile. The antimycotic and/or fungicide may be organic and/or inorganic. The antimycotic and/or fungicide may be polymeric and/or monomeric.
[0034] The antimycotic and/or fungicide may be multivalent which means that the agent may carry one or more active compounds so as to protect against a wider range of mold, mildew and/or fungus species and to protect from evolving defense mechanisms within each species of mold, mildew and/or fungus.
[0035] Any water-soluble salt of pyrithione having antimicrobial properties is useful as the antimicrobial compound. Pyrithione is known by several names, including 2 mercaptopyridine-N-oxide; 2-pyridinethiol-1-oxide (CAS Registry No. 1121-31-9); 1-hydroxypyridine-2-thione and 1 hydroxy-2(1H)-pyridinethione (CAS Registry No. 1121-30-8). The sodium derivative, known as sodium pyrithione (CAS Registry No. 3811-73-2), is one embodiment of this salt that is particularly useful. Pyrithione salts are commercially available from Arch Chemicals, Inc. of Norwalk, Conn., such as Sodium OMADINE or Zinc OMADINE.
[0036] Examples of the antimicrobial compound may include silver-containing compound, zinc-containing compound, an isothiazolone-containing compound, a benzothiazole-containing compound, a triazole-containing compound, an azole-containing compound, a benzimidazol-containing compound, a nitrile containing compound, alcohol-containing compound, a silane-containing compound, a carboxylic acid-containing compound, a glycol-containing compound, a thiol-containing compound or mixtures thereof.
[0037] Additional exemplified commercial antimicrobial compounds may include those from Intace including B-6773 and B-350, those from Progressive Coatings VJ series, those from Buckman Labs including Busan 1218, 1420 and 1200 WB, those from Troy Corp including Polyphase 641, those from Clariant Corporation, including Sanitized TB 83-85 and Sanitized Brand T 96-21, and those from Bentech LLC including Preservor Coater 36. Others include AgION (silver zeolite) from AgION and Mircroban from Microban International (e.g. Microban additive TZ1, S2470, and PZ2). Further examples include dichloro-octyl-isothiazolone, Tri-n-butylin oxide, borax, G-4, chlorothalonil, organic fungicides, and silver-based fungicides. Any one or more of these agents would be considered satisfactory as an additive in the process of making paper material. Further commercial products may be those from AEGIS Environments (e.g. AEM 5772 Antimicrobial), from BASF Corporation (e.g. propionic acid), from Bayer (e.g. Metasol TK-100, TK-25), those from Bendiner Technologies, LLC, those from Ondei-Nalco (e.g. Nalcon 7645 and 7622), and those from Hercules (e.g. RX8700, RX3100, and PR 1912). The MSDS's of each and every commercial product mentioned above is hereby incorporated by reference in its entirety.
[0038] Still further, examples of the antimicrobial compounds may include silver zeolite, dichloro-octyl-isothiazolone, 4,5-dichloro-2-n-octyl-3(2H)-isothiazolone, 5-chloro-2-methyl-4-isothiazolin-3-one, 1,2-benzothiazol-3(2H)-one, poly[oxyethylene(ethylimino)ethylene dichloride], Tri-n-butylin oxide, borax, G-4, chlorothalonil, Alkyl-dimethylbenzyl-ammonium saccharinate, dichloropeyl-propyl-dioxolan-methlyl-triazole, alpha-chlorphenyl, ethyl-dimethylethyl-trazole-ethanol, benzimidazol, 2-(thiocyanomethylthio)benzothiazole, alpha-2(-(4-chlorophenyl)ethyl)-alpha-(1-1-dimethylethyl)-1H-1,2,4-triazole-1-ethanol, (1-[[2-(2,4-dichlorophenyl)-4-propyl-1,3-dioxolan-2-yl]-methyl]-1H-1,2,4-triazole, alkyl dimethylbenzyl ammonium saccharinate, 2-(methoxy-carbamoyl)-benzimidazol, tetracholorisophthalonitrile, P-[(diiodomethyl) sulfonyl]toluol, methyl alcohol, 3-(trimethoxysilyl) propyldimethyl octadecyl ammonium chloride, chloropropyltrimethylsilane, dimethyl octadecyllamine, propionic acid, 2-(4-thiazolyl)benzimidazole, 1,2-benzisothiazolin-3-one, 2-N-octyl-4-isothiazolin-3-one, diethylene glycol monoethyl ether, ethylene glycol, propylene glycol, hexylene glycol, tributoxyethyl phosphate, 2-pyridinethio-1-oxide, potassium sorbate, diiodomethyl-p-tolysulfone, citric acid, lemon grass oil, and thiocyanomethylhio-benzothiazole.
[0039] The antimicrobial compound may be present in the paper substrate at amounts from 1 to 5000 ppm dry weight, more preferably, from 100 to 3000 ppm thy weight, most preferably 50 to 1500 ppm dry weight. The amounts of antimycotic and/or fungicide may be 2, 5, 10, 25, 50, 75, 100, 12, 150, 175, 200, 225, 250, 275, 300, 325, 350, 375, 400, 425, 450, 475, 500, 600, 700, 800, 900, 1000, 1100, 1200, 1300, 1400, 1500, 1600, 1700, 1800, 1900, 2000, 2100, 2200, 2300, 2400, 2500, 2600, 2700, 2800, 2900, 3000, 3200, 3500, 3750, 4000, 4250, 4500, 4750, and 5000 ppm dry weight based upon the total weight of the paper substrate, including all ranges and subranges therein. Higher amounts of such antimycotic and/or fungicide may also prove produce an antibacterial paper material and article therefrom as well. These amounts are based upon the total weight of the paper substrate.
[0040] The paper substrate of the present invention may contain at least one sizing agent. Examples of the sizing agent may be, but is not limited to, alkaline sizing agents and acid-based sizing agents. Examples of alkaline sizing agents include without limitation unsaturated hydrocarbon compounds, such as C6 to C24, preferably C18 to C20, unsaturated hydrocarbon compounds and mixtures thereof. Examples of acid-based sizing agents include without limitation alum and rosin-based sizing agents such as Plasmine N-750-P from Pasmine Technology Inc.
[0041] FIGS. 1-3 demonstrate different embodiments of the paper substrate 1 in the paper substrate of the present invention. FIG. 1 demonstrates a paper substrate 1 that has a web of cellulose fibers 3 and a composition containing an antimicrobial compound 2 where the composition containing an antimicrobial compound 2 has minimal interpenetration of the web of cellulose fibers 3 . Such an embodiment may be made, for example, when an antimicrobial compound is coated onto a web of cellulose fibers during or after papermaking and/or during or after converting the substrate to a useful wallboard tape and/or during or after abrading (such as sanding) the surface of the substrate.
[0042] FIG. 2 demonstrates a paper substrate 1 that has a web of cellulose fibers 3 and a composition containing an antimicrobial compound 2 where the composition containing an antimicrobial compound 2 interpenetrates the web of cellulose fibers 3 . The interpenetration layer 4 of the paper substrate 1 defines a region in which at least the antimicrobial compound penetrates into and is among the cellulose fibers. The interpenetration layer may be from 1 to 99% of the entire cross section of at least a portion of the paper substrate, including 1, 2, 5, 10, 15, 20, 25, 30, 35, 40, 45, 50, 55, 60, 65, 70, 75, 80, 85, 90, 95, and 99% of the paper substrate, including any and all ranges and subranges therein. Such an embodiment may be made, for example, when an antimicrobial compound is added to the cellulose fibers prior to a coating method and may be combined with a subsequent coating method if required. Addition points may be at the size press, for example.
[0043] FIG. 3 demonstrates a paper substrate 1 that has a web of cellulose fibers 3 and an antimicrobial compound 2 where the antimicrobial compound 2 is approximately evenly distributed throughout the web of cellulose fibers 3 . Such an embodiment may be made, for example, when an antimicrobial compound is added to the cellulose fibers prior to a coating method and may be combined with a subsequent coating method if required. Exemplified addition points may be at the wet end of the paper making process, the thin stock, and the thick stock.
[0044] The web of cellulose fibers and the antimicrobial compound may be in a multilayered structure. The thicknesses of such layers may be any thickness commonly utilized in the paper making industry for a paper substrate, a coating layer, or the combination of the two. The layers do not have to be of approximate equal size. One layer may be larger than the other. One preferably embodiment is that the layer of cellulose fibers has a greater thickness than that of any layer containing the antimicrobial compound. The layer containing the cellulose fibers may also contain, in part, the antimicrobial compound.
[0045] Further examples of sizing agents that may be incorporated into the present invention may include, but is not limited to, those found in the following patents: U.S. Pat. Nos. 6,595,632, 6,512,146, 6,316,095, 6,273,997, 6,228,219, 6,165,321, 6,126,783, 6,033,526, 6,007,906, 5,766,417, 5,685,815, 5,527,430, 5,011,741, 4,710,422, and 4,184,914, which are hereby incorporated in their entirety by reference. Preferred alkaline sizing agent may be, but not limited to, alkyl ketene dimer, alkenyl ketene dimer and alkenyl succinic anhydride.
[0046] The paper substrate of the present invention may contain from 0.05 to 1.5 wt % of the alkaline sizing agent based upon the total weight of the substrate. This range includes 0.05, 0.06, 0.07, 0.08, 0.09, 0.1, 0.2, 0.3, 0.4, 0.5, 0.6, 0.7, 0.8, 0.9, 1.0, 1.1, 1.2, 1.3, 1.4, and 1.5 wt %, including any and all ranges and subranges therein.
[0047] The paper substrate of the present invention may have a MD tensile as measured by conventional TAPPI method 494 of from 25 to 100, preferably from 40 to 90 lbf/inch width. This range includes MD tensile of 25, 30, 35, 40, 45, 50, 55, 60, 65, 70, 75, 80, 85, 90, 95, and 100 lbf/inch width, including any and all ranges and subranges therein.
[0048] The paper substrate of the present invention may have a CD tensile as measured by conventional TAPPI method 494 of from 5 to 50, preferably from 20 to 50 lbf/inch width, most preferably 25 to 40 lbf/inch width. This range includes CD tensile of 5, 10, 15, 20, 25, 30, 35, 40, 45, and 50 lbf/inch width, including any and all ranges and subranges therein.
[0049] The paper substrate of the present invention may have a wet strength as measured by conventional TAPPI method 456 of from 5 to 50, preferably from 10 to 25, most preferably from 15 to 25, lb/inch width. This range includes wet strengths of 5, 10, 15, 20, 25, 30, 35, 40, 45, and 50 lb/inch width, including any and all ranges and subranges therein.
[0050] The paper substrate of the present invention may have an internal bond as measured by conventional TAPPI method 541 of from 25 to 350, preferably from 50 to 250, most preferably from 100-200, milli ft-lb/sq. in. This range includes internal bond of 25, 30, 35, 40, 45, 50, 55, 60, 65, 70, 75, 80, 85, 90, 95, 100, 110, 125, 150, 175, 200, 225, 250, 275, 300, 325 and 350 milli ft-lb/sq. in, including any and all ranges and subranges therein.
[0051] The paper substrate of the present invention may have a pH of at least about 1.0 to about 14.0 as measured by any conventional method such as a pH marker/pen and conventional TAPPI methods 252 and 529 (hot extraction test and/or surface pH test). The pH of the paper may be from about 1.0 to 14.0, preferably about 4.0 to 9.0, most preferably from about 6.5 to 8.5. This range includes pHs of 1.0, 2.0, 3.0, 4.0, 5.0, 6.0 6.5, 6.6., 6.7, 6.8, 6.9, 7.0, 7.1, 7.2, 7.3, 7.4, 7.5, 7.6, 7.7, 7.8, 7.9, 8.0, 8.1, 8.2, 8.3, 8.4, 8.5, 8.6, 8.7, 8.8, 8.9, 9.0, 9.2, 9.4, 9.5, 9.6, 9.8, 10.0, 10.5, 11.0, 11.5, 12.0, 12.5, 13.0, 13.5, and 14.0, including any and all ranges and subranges therein.
[0052] The density, basis weight and caliper of the web of this invention may vary widely and conventional basis weights, densities and calipers may be employed depending on the paper-based product formed from the web.
[0053] The paper substrate according to the present invention may be made off of the paper machine having a basis weight of from 50 lb/3000 sq. ft. to 120 lb/3000 sq. ft, preferably from 70 to 120, and most preferably from 80-100 lb/3000 sq. ft. The basis weight of the substrate may be 50, 52, 54, 55, 56, 58, 60, 62, 64, 65, 66, 68, 70, 72, 74, 75, 76, 78, 80, 82, 84, 85, 86, 88, 90, 92, 94, 95, 96, 98, 100, 105, 110, 115 and 120 lb/3000 sq. ft, including any and all ranges and subranges therein.
[0054] The paper substrate according to the present invention may be made off of the paper machine having an apparent density of from 5.0 to 20.0, preferably 9.0 to 13.0, most preferably from 9.5 to 11.5, lb/3000 sq. ft. per 0.001 inch thickness. The apparent density of the substrate may be 5.0, 5.2, 5.4, 5.5, 5.6, 5.8, 6.0, 6.2, 6.4, 6.5, 6.6, 6.8, 7.0, 7.2, 7.4, 7.5, 8.0, 8.5, 9.0, 9.5, 10.0, 10.5, 11.0, 11.5, 12.0, 12.5, 13.0, 13.5, 14.0, 14.5, 15.0, 15.5, 16.0, 16.5, 17.0, 17.5, 18.0, 18.5, 19.0, 19.5 and 20.0 lb/3000 sq. ft. per 0.001 inch thickness, including any and all ranges and subranges therein.
[0055] The paper substrate according to the present invention may have a width off the winder of a paper machine of from 5 to 100 inches and can vary in length. The width of the paper substrate may be 5, 10, 15, 20, 25, 30, 35, 40, 45, 50, 55, 60, 65, 70, 75, 80, 85, 90, 95, 100 inches, including any and all ranges and subranges therein.
[0056] Additionally, the paper substrate according to the present invention may be cut into streamers that have a width of from 1.5 to 3.25 inches wide and may vary in length. The width of the paper substrate streamer may have a width of 1.50, 1.60, 1.70, 1.75, 1.80, 1.85, 1.9, 1.95, 2.00, 2.10, 2.20, 2.30, 2.40, 2.50, 2.60, 2.70, 2.80, 2.90, 3.00, 3.05, 3.10, 3.15, 3.20, and 3.25 inches, including any and all ranges and subranges therein.
[0057] The paper substrate of the present invention may contain optional components as well including but not limited to binders, wet strength additives, and anionic promoters.
[0058] One optional component that is included as one embodiment of the paper substrate of the present invention includes without limitation a binder. Examples of binders include, but are not limited to, polyvinyl alcohol, Amres (a Kymene type), Bayer Parez, polychloride emulsion, modified starch such as hydroxyethyl starch, starch, polyacrylamide, modified polyacrylamide, polyol, polyol carbonyl adduct, ethanedial/polyol condensate, polyimide, epichlorohydrin, glyoxal, glyoxal urea, ethanedial, aliphatic polyisocyanate, isocyanate, 1,6 hexamethylene diisocyanate, diisocyanate, polyisocyanate, polyester, polyester resin, polyacrylate, polyacrylate resin, acrylate, and methacrylate. When the substrate of the present invention contains a binder, preferable binders include without limitation starch and polyvinyl alcohol.
[0059] When the substrate of the present invention contains a binder, the substrate may include any amount of binder including less than 5% of binder, This range includes less than 0.001, 0.002, 0.005, 0.006, 0.008, 0.01, 0.02, 0.03, 0.04, 0.05, 0.1, 0.2, 0.4, 0.5, 0.6, 0.7, 0.8, 0.9, 1, 2, 4, and 5 wt % based on the total weight of the substrate, including any and all ranges and subranges therein.
[0060] One optional component that is included as one embodiment of the paper substrate of the present invention includes without limitation a wet strength additive. The paper substrate of the present invention may contain at least one wet strength additive. The wet strength additive may be cationic, anionic, neutral, and amphoteric. A preferred wet strength additive is cationic and/or contains a basic functional group. Examples of the wet strength additive may be, but is not limited to, polymeric amine epichlorohydrin (PAE), urea formaldehyde, melamine formaldehyde and glyoxylated polyacrylamide resins. Further examples of wet strength additives that may be incorporated in to the present invention may include, but is not limited to, those found in the following patents: U.S. Pat. Nos. 6,355,137 and 6,171,440, which are hereby incorporated in their entirety by reference. Preferred wet strength additives include, but are not limited to, polymeric amine epichlorohydrin (PAE).
[0061] The paper substrate of the present invention may contain from 0.25 to 2.5 wt % of the wet strength additive based upon the total weight of the substrate. This range includes 0.25, 0.30, 0.35, 0.40, 0.45, 0.50, 0.6, 0.7, 0.8, 0.9, 1.0, 1.1, 1.2, 1.3, 1.4, 1.5, 1.6, 1.7, 1.8, 1.9, 2.0, 2.1, 2.2, 2.3, 2.4 and 2.5 wt %, including any and all ranges and subranges therein.
[0062] One optional component that is included as one embodiment of the paper substrate of the present invention includes without limitation an anionic promoter. The paper substrate of the present invention may contain at least one anionic promoter. Examples of the anionic promoter may be, but is not limited to, polyacrylates, sulfonates, carboxymethyl celluloses, galactomannan hemicelluloses and polyacrylamides. Preferred anionic promoters include, but are not limited to polyacrylates such as Nalco 64873.
[0063] The paper substrate of the present invention may contain from 0.05 to 1.5 wt % of the anionic promoter based upon the total weight of the substrate. This range includes 0.05, 0.06, 0.07, 0.08, 0.09, 0.1, 0.2, 0.3, 0.4, 0.5, 0.6, 0.7, 0.8, 0.9, 1.0, 1.1, 1.2, 1.3, 1.4, and 1.5 wt %, including any and all ranges and subranges therein.
[0064] The paper substrate of the present invention may also optionally include inert substances including without limitation fillers, thickeners, and preservatives. Other inert substances include, but are not limited to silicas such as colloids and/or sols. Examples of silicas include, but are not limited to, sodium silicate and/or borosilicates. Another example of inert substances is solvents including but not limited to water. Examples of fillers include, but are not limited to; calcium carbonate, calcium sulfate hemihydrate, and calcium sulfate dehydrate. A preferable filler is calcium carbonate.
[0065] The paper substrate of the present invention may contain from 0.001 to 20 wt % of the inert substances based on the total weight of the substrate, preferably from 0.01 to 10 wt %, most preferably 0.1 to 5.0 wt %, of each of at least one of the inert substances. This range includes 0.001, 0.002, 0.005, 0.006, 0.008, 0.01, 0.02, 0.03, 0.04, 0.05, 0.1, 0.2, 0.4, 0.5, 0.6, 0.7, 0.8, 0.9, 1, 2, 4, 5, 6, 8, 10, 12, 14, 15, 16, 18, and 20 wt % based on the total weight of the substrate, including any and all ranges and subranges therein.
[0066] The paper substrate may be made by contacting a plurality of cellulose fibers with a antimicrobial compound and/or a sizing agent consecutively in any order and/or simultaneously. Further, the contacting may occur in an aqueous environment having a pH of from about 1.0 to about 14.0, preferably from about 6.8 to about 8.5. The pH may be 1.0, 2.0, 3.0, 4.0, 5.0, 6.0 6.5, 6.6., 6.7, 6.8, 6.9, 7.0, 7.1, 7.2, 7.3, 7.4, 7.5, 7.6, 7.7, 7.8, 7.9, 8.0, 8.1, 8.2, 8.3, 8.4, 8.5, 8.6, 8.7, 8.8, 8.9, 9.0, 9.2, 9.4, 9.5, 9.6, 9.8, 10.0, 10.5, 11.0, 11.5, 12.0, 12.5, 13.0, 13.5, and 14.0, including any and all ranges and subranges therein. Accordingly the paper substrate may be made using acidic, near neutral, neutral, or alkaline conditions.
[0067] Still further, the contacting may occur at acceptable concentration levels that provide the paper substrate of the present invention to contain any of the above-mentioned amounts of cellulose fibers, antimicrobial compound, sizing agent, optional components, and/or inert substances isolated or in any combination thereof. The contacting may occur anytime in the papermaking process including, but not limited to the thick stock, thin stock, head box, size press, water box, and coater. The cellulose fibers, antimicrobial compound, sizing agent, optional components, and/or inert substances may be contacted serially, consecutively, and/or simultaneously in any combination with each other. The cellulose fibers, antimicrobial compound, sizing agent, optional components, and/or inert substances may be pre-mixed in any combination before addition to the paper-making process.
[0068] These methods of making the paper substrate of the present invention may be added to any conventional papermaking processes, as well as converting processes, including abrading or sanding to create a fine nap for greater adhesion qualities, slitting, scoring, perforating, sparking, calendaring, sheet finishing, converting, coating, laminating, printing, etc. Preferred conventional processes include those tailored to produce paper substrates capable to be utilized as wallboard tape. Textbooks such as those described in the “Handbook for pulp and paper technologists” by G. A. Smook (1992), Angus Wilde Publications, describe such processes and is hereby incorporated, in its entirety, by reference.
[0069] In one embodiment, the cellulosic fibers and sizing agent may be contacted at anytime during papermaking with or without optional substances or inert substances. In such an embodiment, the cellulosic fibers and sizing agent are contacted at least at the wet end of the paper machine, then the web is dried to make a paper substrate suitable for use as wallboard tape. Optional substances and/or inert substances may optionally be added at anytime during papermaking including without limitation optionally adding the binder to the web using a size press. The substrate may be sanded creating a nap, preferably a fine nap, for greater adhesion qualities. The surface of the substrate carrying the nap may then be contacted with the antimicrobial compound. The contacting may occur using a size press or any coater apparatus including without limitation a spray coater apparatus. Within this embodiment, the optional components and/or inert substances may optionally be contacted with the surface of the substrate at the same time as the antimicrobial compound.
[0070] The present invention is explained in more detail with the aid of the following embodiment example which is not intended to limit the scope of the present invention in any manner.
EXAMPLES
Example 1
Materials
[0000]
Handsheet Furnish: 100% refined southern softwood collected on Jul. 20, 2007
Sizing Agent: Plasmine N-750-P (40% solids)
Aluminum Sulfate (Alum): (40% consistency)
Wet Strength Agent: Poly(amido-amine)-epichlorohydrin (25% solids)
Antimicrobial Agent (A/M): Intace B350
Starch: Tate & Lyle Pearl
Antimicrobial Gypsum Board: ½″ Dense Armor Plus Mold & Humidity Resistant gypsum panel from Georgia Pacific
Joint Compound: Ready Mixed Sheetrock All Purpose Joint Compound from US Gypsum
Method:
[0079] Two Dynamic Sheet Former (DSF) handsheets were made according to the following experimental design:
[0000]
TABLE 1
DSF Study for paper substrates for use
as antimicrobial wallboard tape
Design:
Liquid
Wet
Surface
DSF
Sizing
Alum
Strength
Sizing
A/M*
BDBW
I.D.
lb/T
lb/T
lb/T
(Starch)
Agent
Target gsm
A
0
20
12
N
N
131.5
B
0
20
12
N
Y
131.5
C
10
20
12
N
N
131.5
D
10
20
12
N
Y
131.5
E
0
20
12
Y
N
125.0
F
0
20
12
Y
Y
125.0
G
10
20
12
Y
N
125.0
H
10
20
12
Y
Y
125.0
[0080] Due to the size of the wet-press felt, all sheets were divided into thirds and then wet-pressed at a pressure of 40 psi before drying on a rotary drum-dryer.
[0081] All sheets were tested for the following physical properties prior to any surface sizing with starch: Basis Weight (TAPPI T-410), Caliper (TAPPI T-411), Gurley Porosity (TAPPI T-460), and HST with 10% formic acid and dye solution (TAPPI T-530).
[0082] Samples E-H were then run through a bench-top puddle size press using the Pearl Starch and dried on a drum-dryer. The pearl starch was cooked in two batches having solids measuring 16.7% and 16.3% yielding an approximate pick up of 110 #/Ton.
[0083] Sheets for samples E-H were tested again for the same physical properties as before. All sheets for samples A-H were manually sanded using a belt sander and 80 grit sand paper.
[0084] Samples B, D, F, and H were manually dipped in a bath of Intace B350 anti-michotic agent to yield an approximate pick up of 2 #/Ton. Then each sheet for those samples was dried on a drum-dryer.
[0085] Samples from each condition A-H were cut into 1″ wide tape strips. Then they were adhered to 3″×3″ squares of anti-microbial gypsum board using joint compound and allowed to air dry.
[0086] Prior to inoculation, 3 samples from each condition (A-H) were soaked in ½″ of sterile water for 1 hour. Each gypsum board square was placed upright on its edge so that the water comes ½ ″ up the side of the square that has the tape touching the edge as indicated in FIG. 4 .
[0087] Sample squares were placed on 150×25 mm agar plates and inoculated with 0.38 mL of inoculum containing Chaetomium globosum, Aspergillus terreus , and Aspergillus niger . The inoculum was spread along the bottom half of the sample square (as seen in FIG. 5 ), allowing a portion of the tape to remain uninoculated.
[0088] There was also a set of additional tape samples (A-H) that were not bonded to gypsum panels that corresponded to each gypsum board specimen that was tested. The tape was exposed to water in the same manner as the gypsum board samples, but for 2 minutes instead of 1 hour. They were then inoculated over their entire surface with 0.25 mL of the inoculum.
[0089] Growth observations for all samples were recorded at 7, 21, 33, and 62 days after the samples were inoculated. Photographs of a representative sample for each condition were taken on or near each observation date.
[0090] An amended*form of ASTM Method D2020-92 Standard Test Methods for Mildew (Fungus) Resistance of Paper and Paperboard was followed. The amendments included
1) The test substances were wallboard pieces (i.e. gypsum board square) measuring 3 inches by 3 inches (see above and in FIG. 4 ). 2) Prior to inoculation, each wallboard piece was exposed to a ½ inch of sterile water for 1 hour. The test substance pieces were placed on their edge upright so that the water comes ½ inch up the side of the piece that has the tape touching the edge (see FIG. 5 ). 3) After exposure to the water, the test substances pieces were placed on the 150×25 mm agar plates. 4) Each replicate was inoculated with 0.38 mL of the inoculums. The inoculums were spread along the bottom half of the wallboard piece, the bottom being the edge that was immersed. This will allowed a portion of the tape to remain uninoculated. 5) For each wallboard piece, there was a corresponding separate piece of tape. The tape was exposed to the water in the same manner as the wallboard for 2 minutes. The tape pieces were inoculated over their entire surface with 0.25 mL of the inoculums.
Results;
[0096] Summary (Observations until day 33)
[0097] A/M Treatment—Application hinders mold growth from day 7 to 33 in all but one sample (Sample F).
[0098] Starch Content—Mold growth differences in samples with and without starch in them were not noted until day 33. There is a visual difference on day 20: Samples with starch had noticeably more and larger spore clusters than samples without.
[0099] Sizing Content—Mold growth was noticeably smaller in spore size and cluster amounts on samples where sizing was present.
[0100] Growth with Increasing Time—For samples with mold growth, regardless of starch or sizing content, sporulation mostly began on the edges of the tape by the first observation day (7 days after inoculation). By the second observation day (21 days after inoculation), mold growth had spread across the surface of the tape.
Time-Specific Observations
[0101] Day 7 Observations
[0102] All samples that contain the a/m application show no growth—a/m agent has an effect in prohibiting growth of mold.
[0103] Most growth initiated at the tape edge for samples where slight growth was noted.
[0104] At this stage of growth sizing and starch content do not appear to have an effect on mold growth due to the fact that replicates where “heavy” growth was noted in the “soaked” portion of the sample had sizing in one and no sizing in the other.
[0105] Most samples did not have growth past the inoculation site.
[0106] Day 21 Observations
[0107] Growth began to occur in the non-inoculated region where water “wicked” up the drywall portion of the sample during the soaking portion of sample prep.
[0108] Sizing still does not seem to hinder mold growth at this stage since occurrences of “heavy” growth appeared on samples with and without sizing. The effects of the content of starch are still not seen at this point either because the “heavy” mold growth appeared on samples with and without starch in them.
[0109] All samples that contain the a/m application still show no growth with the exception of sample F (no starch, no sizing, with a/m). This particular sample is believed to be an outlier. Two replicates for this sample had mold growth on the dry portion of the non-inoculated drywall.
[0110] Growth is now seen on the surface of all samples that show growth, not just the edge of the tape.
[0111] Day 33 Observations
[0112] Still no growth on the samples with the a/m treatment.
[0113] Most reps have the same mold coverage as day 21 results.
[0114] Additional mold growth is noted along the edge of the inoculated portion of the tape on samples containing starch but no a/m treatment.—effect of added nutrients (aka starch) now visible.
[0115] Day 62 Observations—
[0116] A/M Treatment—all samples show no growth on the tape itself. Sample F (with starch, no sizing, with a/m) has very slight growth on the drywall above the inoculation point only for two of three reps. No other a/m treated samples have growth anywhere on them.
[0117] Starch Content—For those samples without starch, sporadic mold growth is noted above the inoculation point. Samples that contain starch have evenly spread growth above the inoculation point with slightly larger spores below the inoculation point.
[0118] Sizing Content—Samples without sizing show consistent growth above and below the inoculation point. Samples with sizing show growth mostly confined to the inoculation area.
[0119] As used throughout, ranges are used as a short hand for describing each and every value that is within the range, including all subranges therein.
[0120] Numerous modifications and variations on the present invention are possible in light of the above teachings. It is, therefore, to be understood that within the scope of the accompanying claims, the invention may be practiced otherwise than as specifically described herein.
[0121] All of the references, as well as their cited references, cited herein are hereby incorporated by reference with respect to relative portions related to the subject matter of the present invention and all of its embodiment
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This invention relates to paper products and/or substrates suitable for being made into wallboard tape (also may be known as joint tape and/or drywall tape) and having improved reduction or inhibition in the growth of microbes, mold and/or fungus. The paper substrate is characterized by its excellent physical properties including cross direction (CD) tensile, machine (MD) tensile, internal bond, wet tensile, hygroexpansivity, curl, bonding properties, bonding of joint tape to joint compound, etc. The paper product of the invention contains a sizing agent and an antimicrobial compound as well as other optional components including without limitation a binder. The paper product of the invention may be produced by contacting the plurality of cellulose fibers with each of the sizing agent, antimicrobial compound, and optional components at any point in the papermaking process, converting process, and/or post-converting process. Finally, the invention relates to methods of using the paper substrate.
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CROSS REFERENCE TO RELATED APPLICATIONS
[0001] This application claims priority of German application No. 10 2010 062 340.7 filed Dec. 2, 2010, which is incorporated by reference herein in its entirety.
FIELD OF THE INVENTION
[0002] The invention relates to a method for image support in the navigation of a medical instrument, in particular a catheter, in at least one hollow organ in a surgical site of a body, wherein a presentation of the current position of the instrument in the hollow organ is generated from a three-dimensional dataset of the surgical site and presentation data describing the current position of the instrument, as well as a medical examination device for implementation of the method.
BACKGROUND OF THE INVENTION
[0003] In minimally invasive surgery a medical instrument, for example a catheter or an endoscope, is used for navigation in a hollow organ of a patient, in particular the blood vessels or the heart. An example of a procedure of this type is the insertion of ablation catheters into heart ventricles, for example to treat atrial fibrillation in the left atrium.
[0004] To be able to actually guide the instrument to the right destination in order to carry out the treatment there, methods for image support in the navigation of the instrument have been proposed in which the position of the instrument, mostly specifically the tip of the instrument, is to be visualized in a three-dimensional presentation of the hollow organ. To this end a three-dimensional dataset of the surgical site is used which clearly shows the at least one hollow organ through which the instrument is to be navigated. The three-dimensional dataset can here be obtained from at least one image dataset or an image dataset can be used directly, for example an MR dataset, a CT dataset or the like. For the most part contrast-medium-enhanced 3D recordings are produced for this, in which the relevant hollow organ is segmented using known methods. The result of the segmentation is a three-dimensional mapping of the inner surface of the organ, for example of the endocardium of the atrium.
[0005] The realtime control of the navigation of the instrument is normally achieved by recording radioscopy images (fluoroscopy images), in other words two-dimensional X-ray images, whereby by means of a 2D/3D registration the instrument can be visualized geometrically precisely in three-dimensional space together with the three-dimensional dataset. Although it is also known for the position of the instrument to be determined using a position determination system, which for example works on the basis of sensors, nevertheless it is for the most part preferred to record two-dimensional fluoroscopic images, since the three-dimensional data of the dataset is static and the assignment of the position may be imprecise, in particular when work is to be performed in rapidly moving surgical sites, for example on the heart. In two-dimensional fluoroscopic images the movement itself can be seen. Ultrasound images are sometimes used as an alternative to fluoroscopic recordings.
[0006] As already mentioned, it is known for a presentation of the current position and orientation of the instrument in the hollow organ to be generated, in that ultimately the three-dimensional dataset of the surgical site and the presentation data that describes the position and orientation of the instrument, in particular of the tip of the instrument, wherein the three-dimensional dataset and the presentation data are registered with one another, are merged. The presentation can then be displayed on a display device, for example a monitor, to the person performing the surgery.
[0007] However, the problem with this is that it can happen that in the three-dimensional datasets known structures can overlap the mapping of the instrument in the presentation. For example, the tip of a catheter can be located on the rear wall of the atrium, but is overlaid by the front wall of the atrium such that the catheter superimposed onto the presentation is no longer visible. To solve this problem it has been proposed to increase the transparency of the anatomical structures shown in the presentation, which however taken as a whole results in poorer recognizability of the overall presentation.
[0008] Hence it is generally preferred to set “clip planes” which define regions of the three-dimensional dataset not to be taken over into the presentation. In this way it is possible to look into the hollow organ without any obstruction and to track the instrument in the hollow organ. The problem with this is that the position and orientation of the clip plane must be set manually by the person performing the surgery or by an assistant. With every significant movement of the instrument this setting has to be performed or optimized afresh. This interaction of users is particularly cumbersome in the sterile environment of a catheter laboratory or other areas for minimally invasive surgery.
[0009] EP 2 147 636 A1 describes an apparatus and a method for guiding surgical tools using ultrasound imaging. This aims to create a pure realtime method which does not require any previously recorded images. Consequently it is there proposed to record a time sequence of three-dimensional ultrasound images in real time, with the position and orientation of a surgical instrument being likewise tracked in real time, so that a characteristic axis of the tool can be defined, this mainly being geared to application in the field of needles, canulas, etc. inserted through the skin.
[0010] Since the relative position in space between the three-dimensional ultrasound image and the characteristic axis of the tool has now been determined, a realtime 2D image can now be generated which is defined by an image plane through the corresponding three-dimensional image, and consequently represents a sectional image. This sectional image should now be recorded so that all pixels at a defined distance from the tip of the tool are displayed to someone sitting on said tip of the tool, if this person is looking down from said tip. The clip plane can also be selected in parallel to the characteristic axis of the tool, but in this case too does not show the tool, but merely parallel lines that show the extension of the tool along the characteristic axis.
SUMMARY OF THE INVENTION
[0011] The object of the invention is hence to improve image monitoring of a medical instrument, in line with the situation, in respect of manageability, legibility and the information contained therein.
[0012] To achieve this object it is inventively provided in a method that at least one geometry parameter influencing the generation and/or display be automatically adjusted, taking into account position data of the instrument describing the current three-dimensional position and the current three-dimensional orientation of a tip of the instrument and that the presentation corresponding to the geometry parameters be displayed.
[0013] The presentation is inventively thus adjusted completely automatically as a function of current position data of the instrument, whereby in the context of this description “position” is also to be understood in the following as the six-dimensional position, in other words the position and orientation. Preferably it can be provided here that the viewing direction of the presentation and/or at least one clip plane defining regions of the three-dimensional dataset not to be taken over into the presentation are used as geometry parameters. As regards the viewing direction, this can ultimately always be selected so that a good view is obtained of the feed motion of the instrument, in particular of the catheter. For example, a basic viewing direction relative to the instrument can be defined for this, for example a view from obliquely behind in the direction of feed. The viewing direction, shown in the presentation, to the hollow organ in which the instrument is located is then always adjusted as a function of the position data, and is consequently advantageously updated in real time. The person performing the surgery or an assistant then no longer needs to carry out any other operator functions. This is extremely advantageous in the sterile region in particular.
[0014] Furthermore a clip plane can always be maintained as a function of the position data so that a view of the instrument is possible. Preferably an unobstructed view is additionally in principle available in the direction of a target position or the target position itself. In a particularly advantageous embodiment the viewing direction and the clip plane are jointly adjusted in real time and thus are kept updated in line with the movement of the instrument, so that not only is there an optimum viewing direction for the further feed motion of the instrument, but in addition it is always ensured that an unobstructed view of the instrument exists, in particular, without thereby masking out the target position.
[0015] In a concrete embodiment it can here be provided that a clip plane to be adjusted on the basis of the position data is defined at a fixed distance and a fixed angle of inclination to the tip of the instrument, in particular automatically or semi-automatically. Analogously, as already described, it can be provided that the viewing direction is adjusted on the basis of the position data, in particular relative to the orientation of the tip of the instrument, wherein this too is preferably possible automatically and/or at least at the start of the surgery. As regards the clip plane, it can here particularly advantageously be provided that the definition is effected as a function of at least one target position marked in particular in the three-dimensional dataset and/or a set viewing direction. This means it is on the one hand possible, for a target position, for example a location to be treated, to be marked beforehand, for example by a user, which target position can likewise be taken into account when setting the clip plane (and also, as addressed in greater detail in the following, the viewing direction). For example, the target position can be used when adjusting the geometry parameters such that the clip plane is selected so that the target position still remains visible. But the definition of the clip plane can also be effected as a function of the viewing direction, since ultimately this specifies in what regions of the three-dimensional dataset structures overlaying the instrument may potentially exist which should be cropped. It is also particularly advantageous here if both the at least one target position and the set viewing direction are taken into account.
[0016] It is also conceivable for the definition to be effected as a function of a user input. However, at least during surgery this should only be necessary in exceptional cases, for example if the person performing the surgery has “misnavigated”, in particular, in that a target position now lies behind the instrument or similar. The geometry parameters of the presentation may then need to be completely reset manually, which advantageously can be effected on a graphical user interface. In this connection it can be provided in an advantageous embodiment that to assist with the user input a schematic presentation of the instrument can in particular be presented. For example, the clip plane can be presented at the same time as the instrument, so that a user can grip, move and/or tilt it using a suitable tool. Preferably the viewing direction to the schematic presentation of the instrument and the clip plane is selected such that it corresponds to the viewing direction currently set for the up-to-date presentation.
[0017] As regards the viewing direction, it can be expediently provided that it is selected by taking account of a straight line connecting the tip of the instrument to a target position marked in particular in the three-dimensional dataset, in particular along the straight line. In this way the person performing the surgery can be made intuitively aware of the direction in which the current target position is located, so that he or she can navigate particularly purposefully to the target position. Alternatively it is obviously also conceivable for the viewing direction to be selected as a function of the orientation of the tip of the instrument, in particular in the direction of slide of the instrument or in a fixed angular position thereto. Thus the regions of the hollow organ lying in front of the instrument are always in the view of the person performing the surgery. It is also conceivable for a user interface to be used to toggle between the way in which the geometry parameters, in particular the viewing direction, are determined.
[0018] It is generally advantageous in this connection if both the viewing direction and the clip plane are automatically continuously updated as geometry parameters, in particular in real time, if the new viewing direction is always determined first and if the clip plane then is correspondingly updated taking account of this new viewing direction set. In this way the best possible presentation for the person performing the surgery is always achieved.
[0019] Preferably the position data is determined using at least one position sensor arranged on the instrument, in particular an electromagnetic position sensor. Thus an instrument is used which for example comprises at least one position sensor provided in or on the tip of the instrument. A position sensor of this type, in particular an electromagnetic position sensor, can then determine the spatial coordinates of the tip of the instrument and its direction angle in space as position data. Such position determination systems and their registration with image recording modalities or similar are widely known in the prior art and need not be explained further here.
[0020] Alternatively it is in principle also conceivable for fluoroscopic images recorded for example at an angle, in particular 90°, to one another to be used to determine the position data. However, this is less preferred, since fluoroscopic images from different angles can only with difficulty be recorded on an up-to-date basis. If a biplane X-ray device is used, space problems can occur.
[0021] It can further be provided that at least some of the position data corresponds to the presentation data. For reasons mentioned in the introduction it is however preferably the case that a current fluoroscopic image of the surgical site is used as at least a part of the presentation data. The tip of the instrument is for the most part readily recognizable in this.
[0022] As already mentioned in the introduction, fluoroscopy monitoring is in principle expedient in respect of the traceability of movements in the surgical site, so that a position determination system is preferably provided in parallel with fluoroscopy monitoring. In this case the data can obviously be used in common, providing mutual plausibility if necessary, wherein data of the position determination system can in addition supply information on the missing spatial direction in the fluoroscopic images, which are in fact two-dimensional. Even where in the following only the data of the position determination system is used as position data, some of the position data is nonetheless also included as presentation data.
[0023] The three-dimensional dataset can be an image dataset recorded beforehand of the surgery area and/or a dataset derived from such an image dataset. For example, the three-dimensional dataset may be based on a magnetic resonance image dataset, a computed tomography image dataset and/or a three-dimensional image dataset recorded using another modality, which then for example is further processed using segmentation methods known in the prior art, in order to extract the inner surface of the hollow organ in which navigation is effected and to create a model of the hollow organ for example as a three-dimensional dataset, in which the instrument is then navigated. For example, in this way a model of the heart and of the surrounding blood vessels can be generated if this corresponds to the surgical site.
[0024] Besides the method the present invention also relates to a medical examination device, comprising a display device and a control device designed for implementing the inventive method. All explanations relating to the inventive method can be transferred analogously to the inventive examination device, so that the advantages of the invention can also be achieved herewith. An inventive examination device can for example comprise an X-ray device with a C-arm, on which an X-ray tube and an X-ray receiver are arranged opposite one another. This can be used to record fluoroscopic images as presentation data or as a basis for the presentation data. At the same time a medical instrument can be provided which contains position sensors built into its tip, which are part of an in particular electromagnetic position determination system. A three-dimensional dataset can be obtained via a corresponding communication link, and forms the basis for the presentation to be generated, wherein it is advantageously also conceivable for a three-dimensional image dataset to be generated with the X-ray device also used for recording fluoroscopic images, for example, in that during the rotation of the C-arm projection images are recorded at different projection angles and from these a three-dimensional image dataset is generated in known fashion. If necessary a contrast medium can be administered here beforehand. A three-dimensional image dataset of this type, recorded using a C-arm-X-ray device, has the advantage that even three-dimensional datasets derived therefrom, which for example are obtained by corresponding segmentation, can already be registered with the fluoroscopic images, in particular, if the patient remains motionless. If the position determination system is moreover permanently integrated into the medical examination device, then a fixed registration can also exist in respect of the position determination system and the X-ray device. Thus an environment is created which is excellently suited for implementation of the inventive method.
BRIEF DESCRIPTION OF THE DRAWINGS
[0025] Further advantages and details of the present invention emerge from the exemplary embodiments described in the following as well as on the basis of the drawing, in which:
[0026] FIG. 1 shows an inventive examination device,
[0027] FIG. 2 shows a sketch in explanation of the inventive method and
[0028] FIG. 3 shows a possible user interface for setting a relative position of a clip plane.
DETAILED DESCRIPTION OF THE INVENTION
[0029] FIG. 1 shows an inventive medical examination device 1 . It comprises an X-ray device 2 with a C-arm 3 , on which an X-ray tube 4 and an X-ray receiver 5 are arranged opposite one another. The C-arm 3 can here be moved in respect of at least one degree of freedom of movement, in particular one degree of freedom of rotation, relative to a patient couch 6 .
[0030] Furthermore, a catheter 8 , here an ablation catheter, is provided as a medical instrument 7 to be inserted into a hollow organ for treatment, and is connected to a catheter control device 9 . Electromagnetic position sensors 11 are provided in the tip 10 of the catheter 8 as in principle known, and are assigned to a position determination system 12 which for example can generate an external magnetic field, in order to measure signals induced in the position sensors 11 and from them to determine the six-dimensional orientation of the tip of the instrument 10 , in other words the three-dimensional position and the three-dimensional orientation of the tip of the instrument 10 .
[0031] The X-ray device 2 , the position determination system 12 and the catheter control device 9 are connected to a control device 13 which controls the operation of the medical examination device 1 and is designed for implementing the inventive method, which is explained in greater detail in the following.
[0032] The control device 13 further has access to a display device 14 , here a monitor, and an operator device 15 .
[0033] The control device 13 is now able, by taking account of position data, to automatically adjust geometry parameters of a three-dimensional presentation showing the hollow organ in the surgical site with the current position of the catheter 8 , in particular the tip of the instrument 10 , said presentation being obtained from a three-dimensional dataset and presentation data describing the position of the catheter 8 , if the catheter 8 is moved, in other words changes its position. The viewing direction and the position of a clip plane, which defines regions of the three-dimensional dataset not to be taken over into the presentation, are automatically adjusted here.
[0034] This will now be explained in greater detail with the aid of FIG. 2 . The method is based, as described, on a three-dimensional dataset 16 of the surgical site 17 , which shows particularly clearly or even exclusively the inner walls of the hollow organs to be traversed, in the exemplary embodiment according to FIG. 2 for example the heart 18 with the surrounding blood vessels 19 , in particular the pulmonary vein 20 , which in this instance contains the destination 21 of the surgery.
[0035] In this example the three-dimensional dataset 16 is obtained from a three-dimensional image dataset 22 which was recorded using the X-ray device 2 . To this end a plurality of projection images was recorded from different angles during a rotation of the C-arm, and was transferred to the three-dimensional image dataset 22 using a reconstruction method. Since a contrast medium was administered prior to recording this three-dimensional image dataset 22 , the heart 18 and the blood vessels 19 can be recognized particularly clearly. Hence the heart 18 and the blood vessels 19 can be segmented using a standard segmentation method, so that finally the inner boundaries of the heart 18 and of the blood vessels 19 can be used as a basis for the three-dimensional dataset 16 , which ultimately represents a model which contains the hollow organs in their position.
[0036] The three-dimensional dataset 16 can be used prior to the planned minimally invasive surgery with the catheter 8 , in order to plan the surgery, which means the destination 21 can be marked in the three-dimensional dataset 16 .
[0037] The aim is now to use the three-dimensional dataset 16 jointly with presentation data 23 in order to generate a three-dimensional presentation 24 that shows both the anatomy of the surgical site 17 and the current position of the catheter 8 . Two-dimensional fluoroscopic images 25 from the X-ray device 2 , recorded at regular intervals, and from which the tip of the instrument 10 is readily apparent, are here used as presentation data. This position information is supported by position data 26 obtained from the position determination system 12 , cf. arrow 27 .
[0038] However, on looking at the three-dimensional dataset 16 it is clear that a catheter 8 moving inside the hollow organs 18 , 19 is not visible at all, since the front walls may cover the catheter 8 . Consequently two essential geometry parameters 28 exist which also influence the optimum legibility and utility of the three-dimensional presentation 24 , namely on the one hand the viewing direction from which the scene is viewed, but on the other hand also at least one clip plane which determines which regions of the three-dimensional dataset 16 should not be visible in the presentation 24 , in order that the catheter 8 (and if necessary the destination 21 ) are visible.
[0039] In the inventive method the position data 26 from the position determination system 12 is hence now used in order to update the geometry parameters 28 automatically in the case of updated position data 26 , arrow 29 . In this instance, if new position data 26 exists, the viewing direction is first adjusted as geometry parameters 28 to the new position of the catheter 8 , in particular the tip of the instrument 10 . This happens in this instance in that a connection line is drawn from the tip of the instrument 10 to the destination 21 and on the basis of this connection line the viewing direction is defined, for example so that a user, when the presentation 24 is displayed on the display device 14 , has a good view of both the catheter 8 and the destination 21 , in other words ultimately also the path to the destination 21 , for example in the form of an oblique top view. To this end a fixed angle of inclination of the viewing direction to the connection line can for example be used. Alternatively it is also possible that the current orientation of the tip of the catheter, in other words the direction of feed motion of the catheter 8 , acts as a reference for the definition of the viewing direction. It may be noted that more complex possibilities for determining a viewing direction from the position data 26 are obviously also possible, which for example seek to achieve a good view of the hollow organ 18 , 19 lying in front of the catheter 8 and the destination 21 . It is possible to toggle between different possibilities for automatically setting the viewing direction, for example using the operator device 15 .
[0040] If the viewing direction is first known, the clip plane can also be updated. It is here possible that the position of the clip plane likewise orients itself to the viewing direction, but it is also conceivable for the clip plane to be defined essentially at a fixed distance and at a fixed angle to the position and orientation of the tip of the instrument 10 . Thus the clip plane too is kept updated—be it directly or indirectly—as a function of the position data 26 .
[0041] The result is a presentation 24 , as shown for example in FIG. 2 . It can be seen that because of the clip plane a part of the heart 18 and of the blood vessels 19 is now shown unobstructed, in particular also the pulmonary artery 20 . The tip of the instrument 10 and the destination 21 are readily recognizable, as is the path on which the destination 21 can be achieved.
[0042] Since the steps of the inventive method are executed completely automatically, no operator interaction is necessary in order to maintain a constant presentation of an up-to-date and optimally legible image.
[0043] If nonetheless a change in the basic parameters set for the automatic updating of viewing direction and clip plane should be necessary, for example, if the destination 21 has mistakenly already been passed by the catheter tip 10 or similar, the user interface 30 shown in FIG. 3 can for example be used to redefine the parameters for determining the clip plane. The catheter 8 with the tip of the instrument 10 is shown schematically there. The clip plane 31 is also shown in the schematic three-dimensional presentation relative to the catheter, and can be gripped and correspondingly manipulated, in particular moved or rotated, using a corresponding tool, in this case a gripper hand 32 . The whole presentation can also be changed. A similar possibility for setting is also conceivable in respect of the viewing direction.
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A method for image support in a navigation of a medical instrument, in particular a catheter, in at least one hollow organ in a surgical site of a body is proposed. A presentation of a current position of the instrument in the hollow organ is generated from a three-dimensional dataset of the surgical site and the presentation data describes the current position of the instrument. At least one geometry parameter influencing the generation and/or display of the presentation is automatically adjusted taking into account position data of the instrument describing the current three-dimensional position and the current three-dimensional orientation of a tip of the instrument. The presentation corresponding to the geometry parameters is displayed.
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[0001] This application is a continuation and claims the benefit of U.S. application Ser. No. 12/543,055 filed Aug. 18, 2009, now U.S. Pat. No. 8,360,590, which claims the benefit of U.S. provisional Application No. 61/091,260, filed Aug. 22, 2008.
BACKGROUND OF THE INVENTION
[0002] 1. Field of the Invention
[0003] The present invention relates generally to the field of illuminated plumbing fixtures. More specifically, the present invention is a plumbing fixture including a molded in place integrated light pipe feature for components used both above and below the waterline in spas, pools and all related recreational water products
[0004] 2. Background
[0005] Plumbing fixtures combining illumination have likely been known since illumination has been known. Roman baths combined effective uses of daylight and torch light and reflection to illuminate otherwise unlit rooms and bathing hardware. With the advent of pressurized fountain works, public and private pools, etc, many lighting elements have been incorporated into bathing and water related displays.
[0006] The primary shortcoming of prior combinations of plumbing and light has been cost and durability. A light is somewhat more subject to failure when exposed to the rugged environment of a pool or spa or fountain and protecting the water tight integrity of the light creates cost and complication. If the integrity of the light and/or electrical source is compromised serious complications can result, including inadvertent electrocution.
SUMMARY OF THE INVENTION
[0007] The present invention overcomes the drawbacks of the prior art by combining simplicity and ruggedness into a single feature adaptable to a variety of plumbing fixtures. In its most basic form, this device includes the following components: 1) a part geometry (or shape) otherwise known as the Substrate (or 1 st -shot) which may include all exposed plumbing fixture parts used in the spa/pool industry, (i.e. Jet Body/Face, Bezels, etc.); 2) the Decoration Layer (optional) layered onto the underlying substrate; and, 3) the Integrated Light Pipe (or 2 nd -shot) is a clear/clear tinted/clear colored/semi-clear plastic which is molded over (or encapsulates) a partial or complete surface area of the substrate.
[0008] The light pipe, or translucent molded, layer functions as an integrated light pipe and thusly allows an applied light to be dispersed from a photo-connected light source across the part either partially or completely. The light pipe or translucent molded layer is applied over the substrate and/or the decorative layer using various forms of injection molding but preferably multi-shot molding or pre-mold/over-mold molding. The lighting element would use a light source, either colored or non-colored, such as but not limited to L.E.D., Laser, Fiber Optic, Incandescent or similar but preferably L.E.D. and Fiber Optic. Lastly, a power supply is necessary to provide electricity to the wired lighting element. The power supply could be a low voltage power supply (or battery, in the case where portability is necessary or desirable) that could provide electrical power to one (1) or any number of lighting elements and, thus, part(s).
[0009] The present invention now will be described more fully hereinafter with reference to the accompanying drawings, which are intended to be read in conjunction with both this summary, the detailed description and any preferred and/or particular embodiments specifically discussed or otherwise disclosed. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein; rather, these embodiments are provided by way of illustration only and so that this disclosure will be thorough, complete and will fully convey the full scope of the invention to those skilled in the art.
BRIEF DESCRIPTION OF THE DRAWINGS
[0010] FIG. 1 illustrates a schematic sectional view of a spa part trim element incorporating the integrated light pipe feature of the present invention.
[0011] FIG. 2 illustrates a schematic sectional view of a spa fixture body part showing the integrated light pipe feature.
[0012] FIG. 3 illustrates a schematic sectional view of a spa part showing the integrated light pipe feature and a molded lighting element.
[0013] FIGS. 4A and B illustrate two schematic sectional views of a uni-directional lighting element, with and without a power cord.
[0014] FIG. 5 illustrates a schematic sectional view of the multi-directional lighting element, with a power cord.
[0015] FIG. 6 illustrates a simplistic, non-detailed, schematic sectional view of a large Jet Face, including a uni-directional lighting element which is not integrally molded.
[0016] FIG. 7 shows a sectional view of the light pipe feature according to the present invention incorporated into an actual plumbing fixture.
DETAILED DESCRIPTION OF THE INVENTION
[0017] With reference to the drawing Figures: FIG. 1 illustrates a sectional view of a spa part 10 , in this case a Jet Face, showing the substrate (1 st -shot) 1 , decoration layer 2 , integrated molded light pipe translucent layer feature (2 nd -shot) 3 and barrier wall 4 (of the associated spa, pool, tub, etc.) that the part 10 would be mounted against. Although 10 is shown as a Jet Face, other exposed plumbing fixtures could be similarly equipped.
[0018] FIG. 2 illustrates a sectional view of another spa part 10 , in this case also a Jet Body, but with a lighting element not integrally molded. FIG. 2 shows the plumbing component substrate (1 st -shot) 1 , decoration layer 2 , integrated light pipe feature (2 nd -shot) 3 and the barrier wall 4 (i.e., tub wall, etc.) that the part 10 would be mounted against. FIG. 3 illustrates a similar sectional view, as compared to FIG. 2 , of a spa part 10 , in this case also a Jet Body, but with the lighting element 6 array molded integrally to the jet body. FIG. 3 shows the substrate (1 st -shot) 1 , decoration layer 2 , integrated light pipe feature (2 nd -shot) 3 and barrier wall 4 that the part 10 would be mounted against.
[0019] FIGS. 4A and B illustrate two (2) sectional views of a uni-directional lighting element array 15 having lighting elements 6 included therein. FIG. 4B shows a partial section of an annular multiple light source array 15 with a power cord 7 , and FIG. 4A shows the array 15 without the power cord attached, both arrays 15 showing 3 light sources 6 . The light provided by each array 15 is generally directed as indicated by arrows 8 upwardly from the lighting array 15 and into a light piping feature 3 associated with a given light pipe equipped fixture. The device in FIG. 4B further includes a PC Board 9 , as may be required for certain types of light array control (i.e., LED, or sequencing, dimming, etc.). Each array 15 also shows the substrate (1 st -shot) 1 and integrated light pipe feature (2 nd -shot) 3 .
[0020] FIG. 5 illustrates a sectional view of the annular multi-directional lighting element array 15 , with a power cord 7 , using 3 light sources 6 , and showing the substrate (1 st -shot) 1 and integrated light pipe feature (2 nd -shot) 2 . The FIG. 5 array 15 would be used when light needs to be provided in each direction into a multi ported fixture with several light pipe equipped exposed portions. The array 15 is a 2 nd shot of light piping material with lights 6 embedded therein or attached thereto. The array 15 is shown as an annular shape, but can be any shape complementary to an associated light piping element associated with a fixture. Thusly, the array 15 could be arced, straight, segmented, etc. in accord with an associated light pipe light receiving interface.
[0021] FIG. 6 illustrates a simplistic, non-detailed sectional view of a large Jet Face 10 , including a uni-directional lighting element which is not molded into the Jet face body itself but is, instead, separately associated and attached. The lighting array 15 showing 3 light sources 6 . This array 15 combines the FIGS. 1 and 4 features to create a complete installable part 10 assembly.
[0022] FIG. 7 shows a partial sectional view of an actual plumbing fixture jet 20 . The jet 20 is equipped with a molded substrate 1 , overlying decorative layer 2 , and a light pipe layer 3 layered onto the decorative layer. The light pipe is illuminated by lights 6 (LED type shown) in annular array 15 , each light 6 wired to a control system for providing suitable electric power/control to provide illumination.
[0023] The light pipe 3 is illuminated using a wired lighting element array 15 that can be attached in a number of known or conventional ways. Such methods of attachment would include, but would not limited to: being threaded onto its mating part; molded directly into the geometry of a particular part; glued into place; press fit into place; heat staked into place and/or sonically welded into place which would make a complete assembly (i.e. Substrate, Decoration Layer, Integrated Light Pipe and wired Lighting Element) as shown in FIG. 7 .
[0024] The decorative layer 2 can be applied (but does not have to be present if the underlying substrate is suitable to purpose) by various means such as but not limited to: paint; water immersion; sublimation; and, films applied to the surface of the substrate to enhance the overall look of the finished part(s) when lit or unlit The layer 2 may include but is not limited to: various solid colors; intricate artwork; theme related graphics; unique or varied patterns; metallic's; texture or fabric looks; photographic images; and, any type of graphical decoration that can be added to a part prior to molding the integrated light pipe feature into place.
[0025] The foregoing components are connected as follows: the power supply 7 is electrically connected to every lighting element 6 that will be lit (illuminated) via a direct and/or serial wiring system which runs throughout the entire appliance/structure and will in turn provide constant and regulated electrical power to each lighting element and the attached part(s). Light 8 is transmitted up and through the molded in place integrated light pipe translucent molded layer 3 , past the barrier wall 4 of the appliance/structure and is dispersed across a partial or complete exposed surface area of the targeted part(s) 10 and 20 . The part(s) 10 and 20 can be illuminated with various forms of lighting such as, but not limited to: bright light; low light; soft glowing light and/or colored light, both above and below the water line for a complete or partial illumination effect. This effect is currently not available in the spa, pool and related recreational water industries at this time or via this integrated light pipe technology using molding technologies known primarily as multi-shot molding and/or pre-mold/over-mold molding.
[0026] It should further be noted that: A) this technology could also include but is not limited to different designs, shapes, sizes, diameters, surface and subsurface textures and colors, on either the substrate, which could also be translucent, or the integrated light pipe or all other targeted parts; B) the construction of the lighting elements can be varied such as but not limited to the lighting element being either molded directly into a part(s) at various locations and/or angles on the part(s) thus allowing the light pipe feature to channel light to specific part(s) when assembled, or as an individually molded lighting element which can be either a uni-directional or multi-directional lighting element and can then be assembled to the finished molded part(s) and any associated mating part(s) in any number of aforementioned ways (to form the complete assembly) and could utilize multiple lighting technologies such as but not limited to: L.E.D.; Laser; Incandescent; Fiber Optics; Colored Lighting; Strobe Lighting; LCD; Halogen; Fluorescent and other commonly used lighting sources found within the general lighting industry. The included lighting element(s) preferably being controlled with various types of switches/controls including, for example, rheostat controls. The quantity, angle, location, layout, direction or installation location of lights may be changed to create unique and/or different lighting effects; C) whereas chemical environments in the spa and pool industry are often caustic and/or corrosive, various types of clear/clear tinted/clear colored/semi-clear and opaque thermoplastic materials should be used for the substrate such as but not limited to commodity and/or engineered plastic resins commonly known as ABS, ASA, PVC, PMMA but preferably the plastic resins would be ABS, ASA and PMMA; D) whereas chemical environments in the spa and pool industry are often caustic and/or corrosive various types of clear/clear tinted/clear colored/semi-clear thermoplastics can be used for the integrated light pipe such as but not limited to commodity and/or engineered plastic resins commonly known as ABS, ASA, PMMA, SAN, TPU but preferably the plastic resins would be PMMA, ABS, ASA and would be applied using a multi-shot molding or pre-mold/over-mold molding technology; E) it should be further noted that the use of common materials and/or additives such as but not limited to: nitrogen; air; foaming agents; colorants; glitters; and, specialty additives can create unique and different looks, colors and/or light emission effects; F) additionally, unique processing techniques such as but not limited to fluctuating injection pressures, injection speeds and injection holding pressures will also create unique and different looks such as but not limited to: entrained bubbles; streaks; bursts; striations; and check marks within the integrated light pipe to add unique and different light emission effects; G) or the use of design features molded directly into the integrated light pipe such as but not limited to: bumps; ribs; dimples; undulations; nicks; scallops; textures; etc. can be added for unique light emissions or looks when the parts are lit and not lit and which is not currently available in the spa and pool industry at this time; H) the Decoration Layer can utilize various methods of decoration such as but not limited to: painted graphics; water immersion graphics; sublimation graphics; vacuum metalizing; metal plating and graphical films all of which would consist of specific or random graphics, which said graphics are applied to the substrate prior to the light pipe (transparent plastic) being molded into place and which said decoration techniques and methods are currently not in use in the spa and pool industry but the preferred methods would be painted graphics, water immersion graphics, sublimation graphics and graphical films; and, I) furthermore, it should be noted that depending on the specific design of a particular part and the desired effects to be accomplished the integrated light pipe can be molded to both the inside and outside geometry of a part that would be viewable during use. The substrate of the part having the integrated light pipe molded thereover, as mentioned above, may also be translucent.
[0027] Though primarily intended for the spa and pool industry, this technology could also be adapted to all forms of recreational and/or non-recreational water applications. For example, lighting the jet inlets/outlets of recreational water craft, water jets associated with underwater propulsion systems for divers, etc. Such a light feature might become a safety issue so as alert those nearby that a jet/suction device was active or about to become active.
[0028] While it has been described in terms of specific embodiments, it is to be understood that the invention is not limited to those embodiments. This invention may be embodied in many different forms and should not be construed as limited to the embodiments set forth herein; rather, these embodiments are provided by way of illustration only and so that this disclosure will be thorough, complete and will fully convey the full scope of the invention to those skilled in the art. Indeed, many modifications and other embodiments of the invention will come to mind of those skilled in the art to which this invention pertains, and which are intended to be and are covered by both this disclosure, the drawings and the claims.
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A plumbing fixture using an integrated light pipe wherein a multi-shot method of injection molding is used to apply transparent, light channeling plastic completely or partially over surface areas of parts used above and below the waterline in the spa, pool or recreational water industry. Light is provided to the transparent over-molded portion of parts via a lighting element that can be molded onto the specific parts to be lit or assembled as a separate component to a part. All parts to be lit are directly or serially wired to a power supply mounted within the major appliance housing and are operated by an appropriate control device. This unique multi-shot manufacturing method and approach to illuminating targeted components and/or features provides lighting effects in a way that is simple and rugged and well suited to the rigorous environment of recreational uses of plumbing fixtures and illumination.
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This is a continuation of application Ser. No. 07/311,071, filed Feb. 14, 1989, now abandoned.
BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention relates to a rectifier regulator system adapted to receive power from a source of AC power such as a permanent magnet or rotating field alternator and supplying direct current to a load such as a battery and vehicle electrical system. This regulator contains components for supplying the usual functions for rectifying the AC power and controlling the output voltage to the battery or the load. In addition components are included to prevent the application of dangerous and destructively high voltages to the output lead in the case where the battery or other load is intermittently or permanently opened with the system operating. In addition circuitry is included to turn off an auxiliary output in the event that the load voltage drops below a selected level thus preventing failures of load items which may be damaged by operation with abnormally low voltage applied.
2. Description of Prior Art
Many systems for rectifying the output of an alternator and controlling the charging of the battery are known in the art. An example would be applicant's U.S. Pat. No. 4,791,349. Some prior art circuits have included protection to prevent high voltages from appearing at the battery terminals if the battery is open circuited. Typically in the prior art this has included electronic means to short circuit the source of AC power for the entire time that the battery is, open thus requiring high current components and large heat sinks. In some other prior art circuitry if the battery is completely open and the voltage goes to zero, no power is available to turn on the components that normally allow and control the flow of power to the load. Thus after the first alternator cycle no power is dissipated in the shunt device. This type of circuitry in the prior art while eliminating the need for the large heat sink, however, will fail very quickly if the battery is at an intermediate state between normal characteristics and open circuit.
Also known in the art are systems such as described in applicant's U.S. Pat. No. 4,664,080 for limiting the speed of an internal combustion engine by removing the ignition in response to certain operating or signal conditions. Such systems may receive a portion of their power or a signal from the vehicle battery system such as is charged by the electric power system of the present invention. Under certain conditions of abnormally low battery voltage such as could be created by internal short circuits in the battery, speed limiting apparatus of the type or functional equivalent of that described in the above mentioned U.S. Pat. No. 4,664,080 may produce erratic turning on and off of the ignition, thus creating back firing in the engine which in some engine types could cause severe engine damage. An auxiliary output on the circuit of this present invention is intended to be connected to the input of such speed limiting apparatus, completely turning off such apparatus under abnormally low battery voltage conditions.
The objects and purposes of this invention are as follows:
(1) To produce a simple, light, inexpensive and highly efficient system to rectify and regulate the output of an alternator and produce direct current suitable for recharging a battery or operating the electrical system of a vehicle, and to include in that system means for sensing an intermittent or complete open circuit or partial open circuit of the battery and in response to that condition to turn off the output of the regulator and prevent the creation of abnormal voltages at the battery terminals.
(2) To perform the functions in 1 above without the necessity of large heat sinks or continually conducting the maximum output of the AC source through components within the regulator when the battery circuit is open or intermittently open.
(3) To provide an auxiliary output of the regulator with the voltage at the auxiliary output being abruptly reduced to zero when the voltage of the battery goes, even momentarily, below a predetermined, abnormally low limit.
SUMMARY OF THE INVENTION
This invention relates to an electrical rectification and regulation system. A alternator or other source of alternating current electrical energy provides the input power. A first controllable rectification unit such as a silicon control rectifier selectively allows energy to pass from that source of AC to a direct current load such as a battery. A means of sensing the voltage on the battery and selectively energizing the gate or control electrode of the rectification unit is included. Also included is a second electronic switch means connected effectively across the source of AC power and responsive to a first abnormally high, instantaneous voltage across the battery terminals. Also a portion of the invention is a long time constant peak detecting circuit, sensitive to voltages above the normal battery voltage, but below the first abnormally high voltage. The output of that long time constant circuit is used to lock off the first controllable rectification unit. Also as part of the invention is optionally included an output circuit for driving a tachometer or similar speed measuring device requiring a rectangular waveform. Also included in the invention is an auxiliary output circuit which provides output voltage only provided the load voltage remains above a preselected level, reducing that voltage to zero if the load voltage drops below the preselected level and maintaining that voltage at zero until that circuit is reset from an external signal source.
BRIEF DESCRIPTION OF THE DRAWINGS AND THE APPENDIX
FIG. 1 is a block diagram of a preferred embodiment of this invention. This block diagram includes descriptions of the functional blocks and numbers 1-5 assigned to those functional blocks.
FIG. 2 is an electronic circuit diagram of a preferred embodiment of the present invention. Components corresponding to the functional blocks in FIG. 1 are numbered with the same numbers used in FIG. 1.
The accompanying appendix is a parts list with component values or known industry standard types shown corresponding to the labeling of parts in FIG. 2. The value shown will be typical for a system connected, for instance on an outboard motor to a permanent magnet alternator capable of supplying 15 amps charging current to a 12 volt DC battery. These values are given only to aid in the understanding of the operation of this circuit and are not to be considered to be limiting to the adaptations of the circuit which can be made by someone skilled in the state of the art. For example, in the circuit diagrams and the detailed descriptions that follow, where for instance a bipolar transistor is shown, one skilled in the art may substitute many electrical amplifying devices such as junction or insulated gate field effect in lieu there of transistors. The same will be true when a silicon control rectifier is shown. Where one skilled in the art may substitute other controllable rectifying and switching devices.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
Section number 2 in both FIGS. 1 and 2 correspond generally to the functions in the components in FIG. 4 of applicant's U.S. Pat. No. 4,791,349. The understandings of the teachings of that patent is assumed by reader. The components in blocks 1, 3, 4 and 5 could therefore be omitted and the circuitry in block 2 together with the alternator and load would function as a regulator rectifier but without the high and low voltage protection described as an object of this invention. SCR1 is connected in series with the source of alternating current power shown as A1 and a direct current load shown as a battery. Other external loads of course could be connected across the battery and the battery could be replaced by a large capacitor. The flow of current from the alternator to the load is enabled by gate current to the SCR, flow of gate current is controlled by transistor Q2 in series with resistor R10 and diode D2. Diode D2 prevents reverse voltages from being supplied to transistor Q2 during the half of the AC cycle when SCR1 is reversed biased. Resistor R10 prevents excessively high currents and therefore dissipations through Q2 when the output voltage is below the set regulation level even when SCR1 is turned on and therefore conducting. Resistor R1 is connected from the emitter to the base of Q2 to minimize the effect of leakage current, particularly at high temperature. Zener diode Z1 is the voltage reference for this regulator. Under normal operation, the major portion of the current through this reference is supplied through resistor R4. Under initial start up conditions if the battery voltage is zero, sufficient current can come from the alternator AC through resistor R2 to start the system. Thus, this regulator system is capable of being started with the battery or load at zero voltage. Transistor Q3 shown as a junction field effect transistor controls the base drive to transistor Q2 with respect to the reference voltage across Zener diode Z1. As is known, this device is normally in the conducting mode and rendered nonconductive by negative voltage on the gate with respect to the source which is connected to the anode of Z1. A diode D5 is forward biased by a relatively low current supplied by resistor R7. The voltage across D5 also serves as a portion of the reference voltage, compared to the junction of resistors R5 and R6 which are series connected directly across the battery or load. Diode D5 serves the additional functions of compensation for the down temperature coefficients of Z1, and Q3 and preventing the discharge of C1, through the voltage divider R5, and R6. Thus the relatively fixed voltages established by Zener diode Z1, the gate source voltage of Q3 and the forward bias voltage of D5 are compared by the circuit with a portion of the battery voltage selected by the ratio of R5 to R6. One skilled in the art will see that the phasing is such that an increase in battery voltage above the desired level will apply a negative voltage to the gate of Q3, thus turning Q3 off, which will in turn, turn Q2 off, which will in turn, remove the gate drive from SCR1, preventing the flow of further current from A1 to the battery or load. The values shown in FIG. 3 were chosen to give a approximately zero temperature coefficient with addition of the known characteristics of Z1, Q3 and D5. This produces a stable output voltage with temperature. Alternatively in situations where a predictable change in output voltage with temperatures is desired, such as in some lead acid battery charging applications where it is desireable to reduce the terminal voltage as temperature increases the values of the semiconductors previously mentioned could be changed or alternatively a known temperature coefficient resistor could be substituted for R5 or R6. This circuit is particularly desirable for that adaptation because of the high impedance of the gate of Q3, thus allowing relatively high value resistors to be used for R5 and R6, minimizing the internal heating and therefore drift of value if non zero temperature coefficient parts are used. The value shown in the appendix will give a output regulation voltage of approximately 14 volts typical of a 12 volt lead acid battery under charge.
Block 1 and FIG. 1 is a peak sensitive over voltage protection circuit. Circuitry of this general type is sometimes called a crow bar circuit. These components short circuits the alternator in response to excessive voltage across the battery terminals. It should be stressed that this differs from the conventional crow bar circuit and that the conventional circuit senses the voltage across the same points that the short circuit is applied, the circuit in block 1 senses the voltage across a different circuit, that is the battery, from the circuit that is shorted, circular clamp that is the alternator. When the voltage across the battery exceeds a preset limit, establish primarily by Z2. With minor contributions from the base emitter saturation of Q1 and the drop across R11, current is conducted through Z2, Q1 and D1 into the gate of SCR2 thus turning on SCR2 and reducing the voltage across alternator A1 to essentially 0 for the remainder of that half cycle. The response of these components is extremely fast (in the micro second range). However if no other components were present and the battery was open circuited the SCR2 would have to have a steady state current capability equalling the short circuit current output of the alternator A1. This would typically be between 1 and 2 times the output battery charging capability of A1, thus requiring an extensive heat sink on SCR2. If however only a single cycle out of every several hundred cycles must be short circuited by SCR2 then will normal and practical components the peck current capability of SCR2 becomes the limiting factor and no heat sinking other than that associated with the case itself or SCR2 is required. Diode D1 prevents reverse gate current in SCR2 or reverse voltage application to transistor Q1 during the portion of the alternator waveform when SCR1 annode is negative compared to its cathode. Resistor R11 prevents destructive currents from flowing in transistor Q1 if the battery polarity is in reversed from incorrect connection of jumper cables or other similar happenings. Resistor 11 can also prevent excessive dissipation and transistor Q1 and zener Z2 resulting from a partial short circuit of the winding of alternator A1 to ground. A typical voltage for zener Z2 might be 200% of the nominal battery charging voltage or approximately 28 volts in a nominal 12 volt system.
In FIGS. 1 and 2 reference numeral 3 can be described as sample and hold circuitry with a time constant long compared to the period of the alternator A1. Diode D4 charges capacitor C1 to nearly that peak voltage appearing across the battery terminals. The time constant of capacitor C1 and resistor R8 is chosen to be many times (normally many hundreds of times) the period of the alternator. Resistor R8 together with R7 produce a voltage divider. The ratios in the resistor divider consisting of R5 and R6 compared to the ratio of the resistor divider consisting of R7 and R8 is such that under normal operation the junction of R7 and R8 is positive with respect to the junction of R5 and R6. The resistance of R7 and R8 are normally much higher than the resistors R5 and R6 thus under normal operation a small current flows through resistor R7 and diode D5 and has very little effect on the voltage at the center of the divider compressing R5 and R6. This is the normal condition with the output at its designed approximately 14 volts. If however because of a internal battery failure or a loose battery cable the battery cannot absorb the peak current out of the alternator A1 when SCR1 is turned on, C1 will charge to a level that will turn off Q3 for not only the remaining portion of the alternator cycle when the peck occurs, but for many hundreds of cycles thereafter. The methods of analyzing these time constants and divider ratios is well known in the art will not be described here further. The voltage where this turn off of Q3, caused by the peak voltage detected and stored on C1, occurs would normally be chosen in this invention to lie between the maximum normal charge voltage to the battery and the set voltage of circuit 1, that is primarily the voltage of Z2. Thus a voltage somewhere between 15 and 27 would be appropriate for the example values given herein for illustration purposes. Thus if the load or battery terminal is opened with the system operating, when SCR1 next turns on the voltage to the load would start to raise rapidly. This would charge capacitor C1 as the voltage. When the voltage reaches the voltage that can turn on SCR2, as previously described, the remainder of that half cycle would be shorted. The peak voltage retained on capacitor C1 would turn off transistor Q3. As previously described no gate signal will be supplied to SCR1 for subsequent cycles, typically for several seconds. During that several seconds no current will flow through SCR2. When C1 has discharged through R8 and the associated components to a level where Q3 could again turn on SCR1 may again turn on. If the battery or load circuit still remand open the sequence just described would repeat. If the battery is not still open normal operation will automatically resume. Thus SCR2 is required to short only one cycle every several seconds. One skilled in the state of the art can adapt the various divider ratios and time constants, or in more general terms the entire unique operating sequence disclosed here into a wide range of specific voltage or other requirements.
FIG. 1 and FIG. 2 reference 4 is a tachometer output circuit. Resistor R3 connects the base of transistor Q4 directly to the alternator A1. During one half of the alternator cycle, transistor Q4 is biased on allowing the flow of currant from the battery plus lead through Q4 and the currant limiting resistor R9 to the tachometer output labeled as C. Resistor R9 can be chosen to prevent the burn out of transistor Q4 even if lead C is inadvertently grounded. Diode D3 prevents the application of destructive reverse voltages to the base emitter junction of transistor Q4 during the half of the cycle when transistor Q4 would be non conducting. The slight reverse bias created be the forward voltage drop of D3 reduces the leakage currant on the collector of Q4 to extremely low levels, thus eliminating the need for a resistor from point c to ground. Thus the output of this tachometer circuit at point c is a rectangle waveform going from 0 to the battery plus voltage. This voltage does not vary with the alternator voltage, and therefore speed, and may therefore be connected to tachometers which would be damaged if connected directly to the alternator lead at point B. Diode D3 in conjunction with current limiting resistor R9 can also be seen by one skilled in the art to protect the components in block 4 from the effects of a reversed battery voltage. In a similar manner diode D2 and resistors R4 and R6 will protect components in Block 2 from reverse battery conditions.
In FIG. 1 and FIG. 2 reference numeral 5 refer to a low voltage protection circuit. This circuit receives its main power input from the battery plus lead through diode D6 thus protecting the remainder of the circuitry from possible reverse battery installation. A control signal input is received on the terminal marked E. This might typically be connected to the starter motor armature or starter solenoid or other source that is energized upon starting the engine to which this electrical system may be attached. The output of this circuit is at reference letter D. This could typically be connected to circuitry, such as a speed sensitive ignition interruption circuit, that might cause failure of the circuit or the engine to which it is attached if operated from a voltage below a arbitrarily selected level. The functioning of the circuit is as follows: An input positive signal at point E allows current to flow through resistor R16 and diode D7 and resistor R14 and the base emitter junction of transistor Q6 thus turning on transistor Q6. This input pulse must be of sufficient duration to turn on transistor Q6 in the presence of the time constance associated with R14, R16 and C2. Thus C2 maybe selected by one skilled in the art to prevent turn on of the transistor Q6 and therefore this circuit block from short duration noise that may be associated with the unshielded wire frequently used in engine installations. If point E is connected directly to the starter armature, or other inductive source, a large negative tangent will be produced when the starter motor is deenergized. Diode D8 will allow a path for the flow of this reverse current thus preventing a high reverse voltage and possible breakdown of diode D7. When transistor Q6 is turned on as just described current will flow from the battery plus through diode D6 and the base emitter junction of transistor Q5 and resistor R12 thus turning on transistor Q5. The current will primarily be controlled by resistor R12 which maybe selected to prevent the destruction of transistor Q5 if the output, reference point D, is shorted to ground. When transistor Q5 is turned on, as previously described, it will remain on as long as its collector voltage is higher than the breakdown voltage are zener diode Z3, plus the drops that may be computed for the selected values of resistors R13, R14, and R15. R13 prevents high transient charging currents through zener diode Z3 charging capacitor C2. Alternatively the output D of the low voltage protection circuit could be connected back to a point such as supplying the emitter current for transistor Q2. That would shut down the entire regulator below the voltage selected by the combination of zener diode D3 and resistors R13, R14, and R15.
APPENDIX______________________________________ R1 30K R2 330K R3 150K R4 3.9K R5 15K R6 2.4K R7 10 MEG R8 5 MEG R9 221 R10 270 R11 1K R12 24K R13 150 R14 1.2K R15 1.2K R16 680 D1 IN4004 D2 IN4004 D3 IN4148 D4 IN4148 D5 IN4148 D6 IN4004 D7 IN4148 D8 IN4148 Z1 IN962 Z2 IN971 Z3 IN957 C1 .1 MF C2 .1 MF Q1 MPSA92 Q2 MPSA92 Q3 J230 Q4 MPSA92 Q5 MPSA92 Q6 SCR1 2N6508 SCR2 2N6508______________________________________
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Disclosed is an electrical power system adapted to receiving power from a source of alternating current, typically a small alternator and supplying a direct potentially to a load. This power system contains protective circuits which control or shut off a portion or all of the electrical power system in response to abnormally high or low voltage conditions. The high voltage protection circuit short circuits the alternator in response to abnormally high load voltage. A second high voltage sensing circuit, locks out the main regulation and rectification circuit for a selected period of time after the over voltage sensing point is exceeded. The low voltage protection circuit abruptly reduce output to zero once the output voltage decreases to a minimum level. This voltage then remains at zero until the circuit is reset by an external signal.
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BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to a treatment apparatus for chemical modification of animal fibers of a continuous web form, and particularly relates to the treatment apparatus for improving the property to prevent felting shrinkage of the animal fibers and for improving the resistance to pilling.
2. Description of the Related Arts
Animal fibers have a characteristic hand-feeling as textile fibers employed for clothes, and they are excellent in absorption/desorption of moisture, in water retaining property, and in heat retaining property. They also have a particular nature of water repellency, have moderate tensile strength, moderate elastic property and moderate resistance against abrasion or against wear. In addition, they have biodegradability. However, the animal fibers have, in general, week property in the resistance to pilling thereof, and the pilling nature is not preferable as that of fibers employed for clothes. Therefore, surface modification, and improvement of such fibers, have been long studied and researched, mainly from the aspect of shrink-resistant treatment. As part of the studies and researches, the pilling-resistant treatment (or treatment for preventing the formation of the pilling) has also been sought. However, employing such a conventional treatment or process, the water repellency as an inherent nature of the animal fibers are spoiled more or less.
The conventional method for the surface modification of the animal fibers includes the step of softening or removing the scales which are epidermal structures of the animal fibers, using chlorinating agents or oxidizing agents, for the purpose of performing the shrink-resistant treatment. However, the use of the chlorinating agent may possibly cause a social environmental problem in the future from the view point of the effluent regulation of the Absorbable Organic Halides (AOX). In addition, the treatment, or process, employing the chlorinating agents or the oxidizing agents, leads to such disadvantages as spoil of the hand-feeling to the animal fibers and/or impairment of the water repellency thereof. Moreover, the treatment leads to the reduction of the tensile strength of the animal fibers and the reduction of resistance against abrasion thereof.
Japanese Laid-Open Patent Publication No. 50-126997 discloses a method for improving the dye-affinity and shrink-resistance of wool and for improving the pilling resistance of wool-synthetic blend products, without deteriorating the hand-feeling and tensile strength of the wool. In the disclosed method, the wool impregnated with an aqueous solution of an acid or an acid salt, is brought into contact with an ozone-containing gas. This method, however, has the following problems. That is, the system for performing the method must be a closed system (or a sealed system), because the method involves treatment in an ozone gas atmosphere. According to the method, the water-impregnated wool fibers react with the gaseous ozone. Therefore, the unevenness at which location the wool fibers are impregnated with water, and/or the unevenness at which location the wool fibers are exposed to the gaseous ozone, directly cause(s) the unevenness treatment, thus deteriorating uniformity of the treatment. Moreover, since the treatment or process is carried out in the closed system, the productivity is low. Also, because the environmental loads, such as leakage of ozone from a treating machine (or processing machine) and deterioration in work environment, are great, industrialization employing this method is difficult.
On the other hand, Japanese Laid-Open Patent Publication No. 3-19961 discloses a shrink-resistant treatment method for processing animal fibers, employing ozone as an oxidizing agent. The publication describes that animal fibers in water is brought into contact with fine bubbles of ozone. However, the ozone gas bubbles formed or generated by the glass filter, are too large to be allowed to go into minute portions of a group of the fibers of the animal. Actually, the bubbles can process or treat only the surface portion of the group of the fibers thereof. This results in forming the unevenness treatment thereon, and it fails to provide sufficient shrink resistance to the fibers. As the amount of treatment of the animal fibers increases, more unevenness treatment are formed. In order to enable ozone gas bubbles to go into minute portions of a group of the animal fibers, the size of the gas bubbles must be smaller than the fineness (i.e. the diameter) of the animal fibers to be treated. In addition, the disclosed agitation at 30° C. for 30 minutes is insufficient.
To solve the above problem, Japanese Laid-Open Patent Publication No. 2001-164430 discloses an ozone treatment method. According to the method, in order to enable ozone gas bubbles to go into minute portions of a group of fibers, an aqueous treatment liquid containing gaseous ozone as superfine bubbles having a size of 10 microns or less is blown to the fibers. FIG. 1 shown in the same publication illustrates an apparatus in continuous system for modification of the animal fibers, employing the method. However, the apparatus illustrated on the aforementioned No. 2001-164430 is constructed in a batch system for ozone treatment of a fabric which is fixed to a fixing frame, and it is not constructed for ozone treatment of a continuous fiber structure. Moreover, this apparatus finds difficulty in treating fabric uniformly, or evenly, with the ozone gas in the direction of thickness of the fabric.
SUMMARY OF THE INVENTION
It is an object of the present invention to provide a treatment apparatus for modifying animal fibers of a continuous web form, in which the nature or property to prevent shrink (or shrinkage) of the animal fibers and the nature or property to prevent the animal fibers from pilling are improved or enhanced, in which the hand-feeling unique to the animal hair fibers and the water repellency thereof are not spoiled, and in which the load to the environment is significantly reduced.
In accomplishing this and other objects of the present invention, there is provided a treatment apparatus for chemical modification of animal fibers of a continuous web form, comprising: a tank filled with an aqueous treatment liquid; a net coveyor which has a pair of mesh belts composed of an upper mesh belt and a lower mesh belt and which conveys the continuous web form (or continuous web-like form) through the aqueous treatment liquid in the tank, with the pair of mesh belts overlapping each other in a state in which the pair of mesh belts sandwich the continuous web form therebetween for holding the continuous web form; a treatment liquid circulation system having: a gas-liquid mixing pump which includes an inlet connected to a suction port provided in the tank and which includes an outlet for supplying the aqueous treatment liquid into the tank; a static mixer which is connected downstream of the outlet of the gas-liquid mixing pump; and a discharge nozzle which is provided opposite the suction port in the tank with respect to the pair of mesh belts, in which the discharge nozzle is connected downstream of the static mixer; and an ozonizer for supplying ozone gas to the treatment liquid circulation system, wherein the continuous web form of the animal fibers (or the animal fibers of the continuous web form) is(are) continuously treated with the ozone gas, by mixing the aqueous treatment liquid supplied from the gas-liquid mixing pump with the ozone gas supplied from the ozonizer by the static mixer into dispersing the ozone gas as fine gas bubbles thereof in the aqueous treatment liquid uniformly, by discharging the aqueous treatment liquid containing the fine gas bubbles thereof toward the pair of mesh belts from the discharge nozzle, and by sucking the aqueous treatment liquid containing the fine gas bubbles thereof from the suction port.
As the animal fibers, for example, there are wool, mohair, alpaca, cashmere, llama, vicuna, camel hair and Angora, and the continuous form of such animal fibers includes fabrics and slivers which are produced from animal fibers or produced from a blend of animal fibers and other fibers such as synthetic fibers, by a weaving method, a sewing method or a non-woven fabric manufacturing method. The pair of mesh belts of the net conveyor are overlapped one upon the other, at least inside the tank. As an embodiment, the pair of mesh belts can sandwich the continuous web form of animal fibers therebetween at an entrance to the treatment apparatus at the time of supplying the continuous web form thereof thereinto, and the pair of mesh belts can be separated from each other at an exit therefrom in order to release the continuous web form thereof therefrom at the time of getting the continuous web form thereof out of the treatment apparatus.
According to the construction, the treatment liquid circulation system has both of the discharge nozzle and the suction port in the tank, thereby circulating part of the aqueous treatment liquid in the tank. With the construction, the aqueous treatment liquid including the fine ozone gas bubbles dispersed uniformly or evenly therein, is discharged from the discharge nozzle; and at the same time, the aqueous treatment liquid including the fine ozone gas bubbles thereof are sucked from (or by) the suction port.
The static mixer of the treatment liquid circulation system operates to disperse the ozone gas supplied from the ozonizer in the aqueous treatment liquid which is pumped out from the gas-liquid mixing pump as fine gas bubbles. The position or location at which the ozone gas is supplied into the treatment liquid circulation system, is, preferably, somewhere between the suction port and the gas-liquid mixing pump.
As the ozone gas, any ozone-containing gas can be employed as it is, which is produced from oxygen as a material by changing part of the oxygen, with a silently electric discharging method (or silent discharge method), with a method of photochemistry (or photochemical method), with a plasma discharging method, or the like. Incidentally, when a terminology of “ozone” is referred to hereinafter, the terminology also means a gas containing the ozone.
The aqueous treatment liquid containing the fine ozone gas bubbles dispersed uniformly therein by the static mixer, can be discharged toward one side of the pair of mesh belts from the discharge nozzle; and the continuous web form of animal hair fibers sandwiched between the pair of mesh belts reacts with the ozone gas chemically. Then, due to the power to suck the aqueous treatment liquid by the suction port which can be arranged opposite the discharge nozzle with respect to the mesh belts, the fine ozone gas bubbles dispersed in the aqueous treatment liquid pass through the animal fibers of the continuous web form. Then the aqueous treatment liquid containing the fine ozone gas bubbles are sucked through the suction port.
According to the construction, the continuous web form of animal fibers, supplied continuously, is transported, or fed, continuously through the tank by the net coveyor; and at the same time, the aqueous treatment liquid is circulated in the tank by the treatment liquid circulation system, thereby treating the continuous web form thereof with the ozone gas.
Also, according to the construction, the ozone gas, dispersed in the aqueous treatment liquid in the form of fine gas bubbles, can stay long in the treatment liquid, and the ozone gas easily passes through the animal fibers of the continuous web form, thereby realizing the effective contact between the ozone gas and the continuous web form.
Also, according to the above construction, the aqueous treatment liquid containing the ozone gas bubbles dispersed therein is discharged from a side of one surface of the mesh belts and the aqueous treatment liquid is sucked from a side of the other surface of the mesh belts. Therefore, the ozone gas is allowed to reach a back surface (or a rear surface) of the continuous web form of animal fibers rapidly. This enables a uniform treatment of the continuous web form thereof with the ozone gas.
More specifically, the treatment apparatus can be embodied as follows.
Preferably, there are provided a pair of treatment liquid circulation systems each of which is the treatment liquid circulation system, and the discharge nozzle of one of the pair of treatment liquid circulation systems is provided on one of sides of the mesh belts, and the discharge nozzle of the other of the pair of treatment liquid circulation systems is provided on the other of sides of the mesh belts in which the discharge nozzle of the one thereof and the discharge nozzle of the other thereof are arranged at different locations with respect to a direction in which the continuous web form of animal fibers is conveyed by the mesh belts.
According to the construction, in one of the pair of treatment liquid circulation systems, the aqueous treatment liquid is discharged toward one surface of the continuous web form of animal fibers from the one of sides of the mesh belts; and at the same time, the aqueous treatment liquid is sucked from the other surface of the continuous web form thereof (i.e. sucked from the other of sides of the mesh belts). On the other hand, in the other of the pair of treatment liquid circulation systems, the aqueous treatment liquid is discharged toward the other surface of the continuous web form of animal fibers from the other of sides of the mesh belts; and at the same time, the aqueous treatment liquid is sucked from the one surface of the continuous web form thereof (i.e. sucked from the one of sides of mesh belts). In the construction, the pair of discharge nozzles are positioned at locations where the pair thereof do not oppose each other, with respect to the mesh belts, or with respect to the continuous web form of animal fibers. With the construction, both sides, or both surfaces, of the continuous web form thereof are uniformly, or evenly, treated with the ozone gas, thereby preventing uneven treatment of the continuous web form thereof with the ozone gas in a direction of thickness of the continuous web form thereof.
Preferably, the tank comprises a generally V-shaped tubular body, having an inner space, that is generally rectangular in cross section, in which the inner space has a dimension allowing the pair of mesh belts to pass through therein, wherein the generally V-shaped tubular body comprises: a descending part inside which the pair of mesh belts move down; an ascending part inside which the pair of mesh belts move up; and a central lower part inside which the pair of mesh belts turn from the descending part to the ascending part, in which the descending part and the ascending part are connected by the central lower part.
According to the construction, the tank comprises a tube-like body (or tubular body) that is generally rectangular in cross section, and the inner space has a dimension which allows the mesh belts to pass through therein. Therefore, with the construction, the amount of the aqueous treatment liquid which is filled in the tank can be small. In other words, with the construction, it is possible to increase the number of ozone gas bubbles per unit volume of the aqueous treatment liquid, by increasing the amount of ozone gas per unit volume thereof, or by reducing the bath ratio.
Also, according to the construction, the tank is formed generally V-shaped, in which the mesh belts move down obliquely, or slantingly, inside the descending part thereof, turn inside the central lower part thereof, and then move up obliquely, or slantingly, inside the ascending part thereof. This construction can shorten the overall length of the tank in a direction in which the continuous web form of animal fibers is conveyed, or carried, or transported, thus reducing the size of the treatment apparatus.
Also, according to the construction, the mesh belts are held in the tilted state; therefore, the ozone gas bubbles are allowed to escape upward along the mesh belts. This results in prevention of accumulation of the ozone gas bubbles at one particular location.
Also, according to the construction, the ozone gas bubbles moving upward along the mesh belts are sucked from the suction port in the tank. Therefore, the reaction of the continuous web-like form of animal fibers with the ozone gas is further effectively promoted.
Preferably, there is further provided a treatment liquid circulation system having a circulation pump which includes an inlet connected to the suction port in the tank and which includes an outlet for returning the aqueous treatment liquid into the tank.
In the construction, the outlet of the circulation pump can be connected to the tank at any arbitrary position.
According to the construction, the circulation pump functions so as to strengthen the force to suck the aqueous treatment liquid by (or from) the suction port in the tank. As a result of the increase in power to suck the aqueous treatment liquid thereby, the suction rate becomes greater than the discharge rate in the treatment liquid circulation system, and the fine ozone gas bubbles can be sucked more rapidly though the suction port.
Incidentally, in order to increase the suction rate of the aqueous treatment liquid in the treatment liquid circulation system, a large-size gas-liquid mixing pump may be used. However, the use of such a large-size pump also leads to the increase in the discharge rate of the aqueous treatment liquid from the discharge nozzle. Namely, even if such a large-size gas-liquid mixing pump is employed in the treatment liquid circulation system, it is difficult to sufficiently suck the discharged ozone gas in the treatment liquid, only with the sucking power of the large-size gas-liquid mixing pump. In contrast, according to the above construction, it is possible to increase the suction rate by an amount which is equivalent to the suction by the circulation pump. Therefore, the ozone gas can be sucked more rapidly by the suction port in the tank.
In the construction, the temperature of the aqueous treatment liquid in the tank can be adjusted easily by adjusting the temperature of the aqueous treatment liquid pumped out from the outlet of the gas-liquid mixing pump.
Preferably, the ozone gas supplied from the ozonizer and a fresh liquid of the aqueous treatment liquid are supplied between the suction port of the tank and the inlet of the gas-liquid mixing pump.
In the construction, the aqueous treatment liquid circulating in the treatment liquid circulation system is employed for treating the continuous web form of animal fibers conveyed, or transported, through the tank, with the ozone gas. Therefore, the treatment liquid may contain substances, or materials, which come off from the continuous web form thereof, such as protein forming the animal fibers. Consequently, if the ozone gas is supplied into the treatment liquid circulation system, the ozone gas may possibly react with such substances or materials, and the ozone gas may be consumed inside the tank, as a result. That is, by supplying the ozone gas and the fresh aqueous treatment liquid between the suction port of the tank and the inlet of the gas-liquid mixing pump, the concentration of such substances or materials contained in the aqueous treatment liquid can be made low, and the reaction of the substances or materials with the newly-supplied ozone gas can be effectively suppressed.
According to the construction, both of the ozone gas and the aqueous treatment liquid, are supplied to a position upstream of the inlet of the gas-liquid mixing pump, and both thereof are sent together to the gas-liquid mixing pump. Therefore, both of the ozone gas and the aqueous treatment liquid are mixed together preliminarily inside the gas-liquid mixing pump. Accordingly, with this construction, the efficiency of mixing the ozone gas with the aqueous treatment liquid by the static mixer is increased.
Preferably, there are provided a plurality of discharge nozzles each of which is the discharge nozzle, wherein the discharge nozzle has a predetermined length in a direction of width of the mesh belts, and wherein the plurality of discharge nozzles are provided in the direction of width thereof so that the plurality of discharge nozzles extend from both sides, in the direction of width, of the mesh belts toward a center of the mesh belts in the direction of width.
That is, when the continuous web-like form of animal fibers has a predetermined width, it is preferable to make the continuous web-like form thereof react with the fine gas bubbles of the ozone gas uniformly, or evenly, also in the direction of width of the web-like form (i.e. in the direction of width of the mesh belts), by making the ozone gas contact with the continuous web form thereof. In order to realize this, a discharge nozzle having a predetermine length in the direction of width of the mesh belts, can be employed effectively. However, when the aqueous treatment liquid containing the ozone gas bubbles dispersed uniformly therein is supplied to the discharge nozzle, the amount of the fine ozone gas bubbles discharged through the discharge nozzle under the discharge pressure varies in the direction of width of the continuous web form thereof, or in the direction of width of the mesh belts. As a result, it becomes difficult to evenly treat the continuous web-like form thereof with the ozone gas. In this connection, according to the above construction of the present invention, there are provided a plurality of discharge nozzles in the treatment liquid circulation system, and the plurality of discharge nozzles are provided in the direction of width of the mesh belts so that the plurality of discharge nozzles extend from both sides, in the direction of width thereof, of the mesh belts towards the center of the mesh belts in the direction of width thereof. Consequently, the difference in discharge rate of the ozone gas in the direction of width thereof is reduced or diminished. Namely, with the construction, it is possible to reduce the unevenness, or non-uniformity, of treatment of the continuous web form of animal fibers with the ozone gas in the direction of width of the continuous web form thereof, or in the direction of width of the mesh belts.
Preferably, each of the fine gas bubbles has a size of 50 microns or less.
With the fine gas bubbles of the ozone gas, the ozone gas bubbles can stay longer in the aqueous treatment liquid in a state in which the ozone gas bubbles are dispersed therein. Thereby, it is possible to prolong the time, or duration, to treat the continuous web-like form of animal fibers with the ozone gas.
Also, with the fine gas bubbles of the ozone gas, the fine ozone gas bubbles can easily pass through gaps, or spaces, amongst the animal fibers of the continuous web form. Thereby, it is possible to make the ozone gas bubbles contact the continuous web form thereof up to the inside of the continuous web form, and it is possible to make the ozone gas bubbles react with the continuous web-like form thereof up to the inside thereof.
BRIEF DESCRIPTION OF THE DRAWINGS
This and other objects and features of the present invention will become clear from the following description taken in conjunction with the preferred embodiment thereof with reference to the accompanying drawings.
FIG. 1 is an arrangement plan view of a wool fiber treatment system including a treatment apparatus, for chemical modification of animal fibers of the continuous web-like form, according to the present invention.
FIG. 2 is a schematic perspective view of the treatment apparatus of FIG. 1 .
FIG. 3 is a schematic front view to explanatorily illustrate a construction of the treatment apparatus of FIG. 2 .
FIG. 4 is a schematic left-hand view of the treatment apparatus of FIG. 3 .
FIG. 5 is a schematic right-hand view of the treatment apparatus of FIG. 3 .
FIG. 6 is a schematic view to explanatorily illustrate a construction of a circulation system provided in the treatment apparatus of FIG. 2 .
FIG. 7 is a cross-sectional view taken along a line of VII in FIG. 2 .
FIG. 8 is a cross-sectional view taken along a line of VIII in FIG. 2 .
FIG. 9 is a view showing a structure of a discharge nozzle which is employed in the treatment apparatus of FIG. 2 .
FIG. 10 is a cross-sectional view taken along a line of X—X in FIG. 9 .
FIG. 11 is an explanatory view showing the movement of the ozone gas bubbles.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
Before the description of a preferred embodiment of the present invention proceeds, it is to be noted that like or corresponding parts are designated by like reference numerals throughout the accompanying drawings.
With reference to FIGS. 1 through 11 , a description is made below upon a treatment apparatus for reforming a continuous web form (or continuous web-like form) of animal fibers, according to the preferred embodiment of the present invention.
FIG. 1 is an arrangement view of a wool fiber treatment system including the treatment apparatus of the preferred embodiment. To this system, wool in the form of a top which is not treated by ozone, is used as a supply material. The wool is treated by ozone with the treatment apparatus of the preferred embodiment which is arranged in the wool fiber treatment system, and the ozone-treated wool is again wound up in the form of a top as a finished product (or an end product).
That is, first, with the use of a creel 1 , the top as the supply material is unwound, and a plurality of slivers are bound together to form a bundle with predetermined width. The slivers are then combed, or gilled, by a gill 2 for making the width thereof greater, in order to form or obtain a continuous web form of wool fibers having a width of about 135 mm. The continuous web-like form of the wool fibers thus gilled therewith, is then impregnated with an aqueous pretreatment solution by a padder 3 , in order to improve, or increase, the efficiency in the subsequent ozone treatment. Then, the continuous web-like form of the wool fibers thus impregnated with the aqueous pretreatment solution, is kept at a predetermined temperature by a steamer 4 , in order to promote the reaction of the continuous form thereof with the aqueous pretreatment solution. This pretreatment is desirable, because the impregnation of the wool fibers therewith before the wool fibers are subjected to blowing of the ozone gas in water, enhances the reforming effect. After the aqueous pretreatment solution is washed away from the wool fibers by a washer 5 , the continuous web-like form of the wool fibers is supplied to the treatment apparatus 6 of the preferred embodiment.
The treatment apparatus 6 of the embodiment performs the ozone treatment so that an aqueous treatment liquid containing the ozone gas as superfine bubbles is blown to the continuous structure of the wool fibers while the continuous form thereof is being conveyed in succession through the aqueous treatment liquid. As a result, the surface of each wool fiber is reformed, and thus the property of resistance against shrink and the property of resistance against pilling are improved, without spoiling the wool-intrinsic excellent hand-feeling and water repellency. Specifically, this treatment apparatus is an apparatus for continuously executing the method for reforming animal fibers which is disclosed in Japanese Laid-Open Patent Publication No. 2001-164460.
Then, the aqueous treatment liquid is washed away from the wool fibers of the continuous form which has been moved from the treatment apparatus 6 by a back washer 7 , and the continuous form thereof is dried by a dryer 8 .
Finally, the continuous web form of the wool fibers is wound by a coiler 9 to be provided as a top.
FIG. 2 is a schematic perspective view of the treatment apparatus of the embodiment. In the treatment apparatus 6 , the wool fibers of the continuous web form 10 , sandwiched or held between a pair of two mesh belts 12 a and 12 b , is allowed to pass through an inner space of a tank 11 , generally V-shaped in cross section, filled with the aqueous treatment liquid. The aqueous treatment liquid containing superfine ozone bubbles, is discharged (or blown or jetted) toward the wool fibers of the continuous web form 10 that is being conveyed, from one surface of the continuous form thereof. Simultaneously, the aqueous treatment liquid containing the ozone gas bubbles is sucked by suction ports 15 (i.e. 15 a , 15 b , 15 c ); 16 (i.e. 16 a , 16 b , 16 c ) which are arranged on the other surface (or on the opposite surface) of the wool fibers of the continuous form.
The tank 11 is dimensioned as follows. Namely, the tank 11 has a tube-like body having a generally rectangular cross section of which the inner space has a dimension large enough to allow the two mesh belts 12 (i.e. 12 a , 12 b ) to pass therethrough. The body is bent into a generally V-shape with its center portion locating at a low position so that the mesh belts 12 passing through the inner space descend once and then ascend therein. That is, the tank 11 has a descending portion 11 a allowing the two mesh belts 12 to descend, an ascending portion 11 b allowing the mesh belts 12 to ascend, and a turning portion 11 c locating therebetween. Each of the descending and ascending portions 11 a and 11 b is, respectively, tilted with respect to the normal, as shown in FIG. 2 .
The tank 11 is filled with the aqueous treatment liquid. The tank 11 is replenished with a fresh liquid by gas-liquid mixing pumps 13 (i.e. 13 a , 13 b , 13 c , 13 d ) as will be described later, and an amount of the liquid exceeding a predetermined level is drained from the tank 11 via a drain outlet 18 .
Each of the two mesh belts 12 a and 12 b which are allowed to pass through the inside of the tank 11 , is made of a metal meshed endless belt, and the two mesh belts 12 a and 12 b are arranged to move along a predetermined route over a plurality of rollers at generally the same speed. A part of the lower mesh belt 12 a thereof moves along a route corresponding to a lower part inside the tank 11 , as shown by an arrow 90 in the figure. On the other hand, a part of the upper mesh belt 12 b moves along a route corresponding to an upper part inside the tank 11 , as shown by an arrow 91 therein. The two mesh belts 12 a and 12 b which are put together one on the other so as to sandwich, or pinch, the wool fibers of the continuous web form 10 therebetween at a location near an entrance of the tank 11 , descend in the descending portion 11 a of the tank 11 in a tilted state, are turned in the turning portion 11 c thereof, and then ascend in the ascending portion 11 b thereof in a tilted state. After passing through an exit of the tank 11 , the two mesh belts 12 a and 12 b separate from each other.
Incidentally, the wool fibers of the continuous web form which has been released from the mesh belts 12 a and 12 b , is compressed vertically with a pair of squeezing rollers 31 a and 31 b for squeezing out the aqueous treatment liquid, and then the squeezed structure of the wool fibers is sent to the back washer 7 .
Each of the descending portion 11 a and the ascending portion 11 b , of the tank 11 , is provided with discharge nozzles for discharging the aqueous treatment liquid including superfine ozone gas bubbles dispersed therein, and is provided with the suction ports 15 (i.e. 15 a , 15 b , 15 c ) and 16 (i.e. 16 a , 16 b , 16 c ), respectively, for sucking the aqueous treatment liquid. The discharge nozzles and the suction ports 15 and 16 , will be described later in detail.
Inside the turning portion 11 c of the tank 11 , there is arranged a turn roller 32 for turning, or changing, a direction in which the two mesh belts 12 a and 12 b are carried or transported, in a state in which the two mesh belts 12 a and 12 b are overlapped on each other. The turn roller 32 is a drive roller which is driven by a drive motor 34 a , as will be explained later (refer to FIG. 3 ).
The treatment apparatus 6 has two types of pumps, which are: four gas-liquid mixing pumps 13 a , 13 b , 13 c , 13 d and two circulation pumps 17 , 17 . More specifically, two gas-liquid mixing pumps 13 a , 13 b and one circulation pump 17 are mounted on the side of the descending portion 11 a ; on the other hand, two gas-liquid mixing pumps 13 c , 13 d and one circulation pump 17 are mounted on the side of the ascending portion 11 b . By the way, FIG. 2 shows only the two gas-liquid mixing pumps 13 a , 13 b and the one circulation pump 17 which locate on the side of the descending portion 11 a.
As explained above, the two gas-liquid mixing pumps 13 ( 13 a and 13 b ), and the two gas-liquid mixing pumps 13 ( 13 c and 13 d ) are provided for the descending portion 11 a and the ascending portion 11 b , of the tank 11 , respectively. Each of the gas-liquid mixing pumps 13 a , 13 b , 13 c , 13 d has an inlet which is connected to each of the suction ports 15 b , 15 a , 16 a , 16 b which are mounted on the tank 11 ; and each of the gas-liquid mixing pumps 13 a , 13 b , 13 c , 13 d has an outlet for discharging, or blowing out, both of the aqueous treatment liquid and the ozone gas dispersed therein, into the tank 11 , simultaneously. Each of the gas-liquid mixing pumps 13 a , 13 b , 13 c , 13 d constitutes a circulation system of the treatment liquid, together with a static mixer 14 which is connected downstream of the outlet of the gas-liquid mixing pump and together with a discharge nozzle connected downstream of the static mixer 14 , in which the discharge nozzle is placed at a position facing the corresponding suction port 15 (i.e. 15 b , 15 a ), 16 (i.e. 16 b , 16 a ) of the tank 11 with respect to the mesh belt 12 (i.e. 12 a , 12 b ).
In the arrangement, as the gas-liquid mixing pump 13 (i.e. 13 a , 13 b , 13 c , 13 d ), the pump which is capable of preventing drop in flow and pressure of the aqueous treatment liquid to be pumped out, is employed, even when the pump sucks ozone gas equal to an amount as much as one-tenth of the flow of the aqueous treatment liquid. Specifically, it is preferable to employ a gas-liquid mixing pump of OMC32-6 (model name or type name), manufactured by Oshima Machinery & Co., Ltd.
Hereinafter, it will be explained typically about an aqueous treatment liquid circulation system including the gas-liquid mixing pump 13 a of all the four aqueous treatment liquid circulation systems arranged in the treatment apparatus, two of which are arranged for the descending portion 11 a , and two of which are arranged for the ascending portion 11 b.
The descending portion 11 a of the tank 11 has the three suction ports 15 a , 15 b and 15 c . The suction port 15 a located at the lowest position is connected to the inlet of the gas-liquid mixing pump 13 b . In the arrangement, by driving the gas-liquid mixing pump 13 b , the aqueous treatment liquid in the tank 11 is sucked through the suction port 15 a and a pipe 21 a into the inlet of the gas-liquid mixing pump 13 b , as shown by an arrow 71 . The pipe 21 a has a supply port 29 for passing the aqueous treatment liquid and has a supply port 30 for passing the ozone gas at certain positions of the pipe 21 a , respectively, as will be explained later.
The supplied aqueous treatment liquid and the supplied ozone gas, are dispersed preliminarily in the gas-liquid mixing pump 13 b , and they are pumped out from the outlet to the static mixer 14 via a pipe 20 a . As the static mixer 14 , it is preferable to employ such a mixer which can generate, or form, fine gas bubbles and which can mix a large amount of aqueous treatment liquid with the gas. Specifically, an OHR Line Mixer (product name) manufactured by Seika Industry & Co., Ltd. is preferably employed. With the static mixer 14 , the ozone gas in the aqueous treatment liquid is changed into superfine gas bubbles having a size of 30 microns or less, which are dispersed in the aqueous treatment liquid, uniformly or evenly.
The pipe 20 a extends through a side-wall of the descending portion 11 a of the tank 11 , and it enters the inside of the tank 11 . At the tip of the pipe 20 a , is mounted the discharge nozzle, from which the aqueous treatment liquid including the fine ozone gas bubbles dispersed therein is blown out, or jetted out. Most of the aqueous treatment liquid and the ozone gas, discharged from the discharge nozzle, are sucked by the suction port 15 a , and the liquid including the gas thus sucked circulate in the circulation system as aforementioned.
The aqueous treatment liquid circulation system including the gas-liquid mixing pump 13 a also has an arrangement (or construction) which is substantially equal to the arrangement (or construction) as aforementioned, except that a pipe 20 b extends through the side-wall which is opposite to the side-wall through which the pipe 20 a extends.
Similarly, a pair of aqueous treatment liquid circulation systems are provided for the ascending portion 11 b of the tank 11 . However, in contrast with the arrangement of the descending portion 11 a , there exists a difference in that the position of the discharge nozzles and the position of the suction ports in the ascending portion 11 b with respect to the mesh belts 12 (i.e. 12 a , 12 b ) are reverse to those in the aqueous treatment liquid circulation system for the descending portion 11 a . This will be described later.
Next, it is explained about the circulation pump 17 . One circulation pump 17 is mounted for each of the descending portion 11 a and the ascending portion 11 b of the tank 11 . The circulation pump 17 is provided mainly for the purpose of enhancing the suction force in the circulation systems. The inlet of the circulation pumps 17 , 17 are connected to the suction ports 15 (i.e. 15 a , 15 b , 15 c ) and 16 (i.e. 16 a , 16 b , 16 c ) of the tank 11 through pipes 23 a , 23 b and 23 c , for mainly sucking the aqueous treatment liquid.
The aqueous treatment liquid which has been sucked through the suction port 15 ( 15 a , 15 b and 15 c ) provided for the descending portion 11 a and through the suction port 16 ( 16 a , 16 b and 16 c ) provided for the ascending portion 11 b , of the tank 11 , is sent, or transported, to the circulation pumps 17 , 17 via a pipe 24 as shown by an arrow 73 . The aqueous treatment liquid in each of the circulation pumps 17 , 17 is then pumped back into the tank 11 at an upper position and a position in the turning portion 11 c , as shown by an arrow 72 . During the liquid circulation, the temperature of the aqueous treatment liquid is adjusted, so that the temperature of the aqueous treatment liquid in the tank 11 is easily adjusted.
With the provision of the circulation pumps 17 in the treatment apparatus, the suction rate of the ozone gas through the suction ports 15 (i.e. 15 a , 15 b , 15 c ) and 16 (i.e. 16 a , 16 b , 16 c ) becomes greater than the discharge rate of the ozone gas which is blown, or jetted, toward the wool fibers of the continuous web form, thus increasing the rate, or speed, of suction of the ozone gas. Namely, this enables the ozone gas bubbles dispersed in the aqueous treatment liquid to react with the wool fibers of the continuous web form before the bubbles of the ozone gas rise and separate in the liquid, thus improving, or enhancing, the efficiency in the chemical modification of the wool fibers.
FIG. 3 is a schematic front view to explanatorily illustrate the construction of the treatment apparatus 6 of FIG. 2 . Namely, on a frame 33 of the treatment apparatus 6 , there are arranged the aforementioned tank 11 which has the generally V-shaped cross-section, the gas-liquid mixing pumps 13 (i.e. 13 a , 13 b ; 13 c , 13 d ), the circulation pumps 17 and 17 , the drive motors 34 (i.e. 34 a , 34 b ) for driving the mesh belts 12 a and 12 b , and so on.
The lower mesh belt 12 a and the upper mesh belt 12 b , are driven by driving rollers 32 , 35 and 36 which are driven to rotate by force transmitted, or exerted, from the drive motors 34 a and 34 b.
The mesh belts 12 (i.e. 12 a , 12 b ) moved, or carried, inside the tank 11 , are turned by the drive roller 32 which is placed at the turning portion 11 c of the tank 11 . As shown in FIG. 3 , the turning portion 11 c is configured so that the side of the ascending portion 11 b is higher than the side of the descending portion 11 a , and so that the driving roller 32 is placed at a deviated position closer to the ascending portion 11 b . With this arrangement, the mesh belts 12 can be moved through the descending portion 11 a and the ascending portion 11 b of the tank 11 along a route, or a course, closer to the suction ports 15 (i.e. 15 a , 15 b , 15 c ) mounted on the upper wall of the descending portion 11 a and closer to the suction ports 16 (i.e. 16 a , 16 b , 16 c ) mounted on the lower wall of the ascending portion 11 b , respectively. That is, with the arrangement, it is possible to strongly suck, or absorb, the aqueous treatment liquid including the ozone gas bubbles blown from the discharge nozzles with the suction ports 15 and 16 .
FIG. 4 is a schematic left-hand view of the treatment apparatus of FIG. 3 , and FIG. 5 is a schematic right-hand view of the treatment apparatus of FIG. 3 . As described above, a total of four aqueous treatment liquid circulation systems including the gas-liquid mixing pumps 13 a , 13 b ; 13 d , 13 d , are provided in the treatment apparatus 6 . Namely, two aqueous treatment liquid circulation systems are provided for the descending portion 11 a of the tank 11 , and two aqueous treatment liquid circulation systems are provided for the ascending portion 11 b thereof. In the arrangement, each of the four circulation systems includes the discharge nozzle 19 for discharging the aqueous treatment liquid including fine ozone gas bubbles dispersed therein uniformly. The discharge nozzle 19 has a length which extends in a direction of width of the continuous web form 10 of the wool fibers so that the ozone gas bubbles can be delivered to the entire surface of the continuous web form 10 thereof uniformly and evenly.
However, in a case that the discharge nozzle having a too long hole or slit (refer to FIGS. 9 and 10 ) is employed, and in a case that the aqueous treatment liquid having the ozone gas bubbles dispersed therein uniformly is supplied to the discharge nozzle 19 , the discharge amount and/or discharge speed (or discharge rate) of the liquid from the hole or slit decreases as the position where the liquid is discharged is farther away from the proximal end of the discharge nozzle. In other words, in a case that a discharge nozzle having a length exceeding a predetermined one is employed, the amount of discharge of the fine ozone gas bubbles therefrom varies along the length of the discharge nozzle, or the amount thereof has a distribution in the direction of the length of the discharge nozzle, thus making it difficult to uniformly treat the wool fibers of the continuous web form with the ozone gas bubbles.
In the treatment apparatus 6 of the preferred embodiment, as shown in FIGS. 4 , 7 and 8 , each of the discharge nozzles 19 employed in each of the circulation systems is made short, and the each thereof is arranged, or aligned, in the direction of the width of the tank 11 (i.e. the width of the descending portion 11 a , and the width of the ascending portion 11 b ), in order to uniformize the discharge rate of the ozone gas bubbles therefrom.
In addition, as shown in FIG. 4 , the discharge nozzles are positioned so that the aqueous treatment liquid is supplied toward the center of the tank 11 with respect to the direction of the width of the tank 11 , through the discharge nozzles 19 and 19 , from both side-walls of the tank 11 . By this arrangement, the difference (or non-uniformity) in discharge rate, or discharge amount, of the aqueous treatment liquid in the direction of width thereof is reduced, thus diminishing, or preventing, non-uniformity in the treatment of the wool fibers with the ozone gas.
As shown in FIG. 3 , the suction ports 15 (i.e. 15 a , 15 b ) are mounted on the descending portion 11 a of the tank 11 in opposition to the discharge nozzles 19 and 19 with respect to the mesh belts 12 a and 12 b which are located between the suction ports 15 (i.e. 15 a , 15 b ) and the discharge nozzles 19 and 19 . Also, as shown in FIGS. 3 and 5 , the suction ports 16 (i.e. 16 a , 16 b ) are mounted on the ascending portion 11 b of the tank 11 in opposition to the discharge nozzles 19 , 19 with respect to the mesh belts 12 a and 12 b which are located between the suction ports 16 (i.e. 16 a , 16 b ) and the discharge nozzles 19 , 19 .
FIG. 6 is a schematic view to explanatorily illustrate the construction of circulation systems in the treatment apparatus of FIG. 2 . As described above, the treatment apparatus 6 has the circulation systems including the four gas-liquid mixing pumps 13 (i.e. 13 a , 13 b , 13 c , 13 d ) and has the circulation systems including the two circulation pumps 17 , 17 . Each of the gas-liquid mixing pumps 13 has a discharge pressure of 4 to 8 kg/cm 2 and a discharge rate of 80 L/min. On the other hand, each of the circulation pumps 17 , 17 has a discharge pressure of 0.5 kg/cm 2 and a discharge rate of 200 L/min.
As aforementioned, in the circulation systems including the gas-liquid mixing pumps 13 (i.e. 13 a , 13 b , 13 c , 13 d ), the inlets of the gas-liquid mixing pumps 13 are connected to the suction ports 15 (i.e. 15 a and 15 b ) and 16 (i.e. 16 a and 16 b ), so that the ozone gas and the aqueous treatment liquid sucked thereby are sent to the gas-liquid mixing pumps 13 through the pipes 21 a and 21 b . As shown in FIGS. 2 and 6 , at predetermined locations of each of the pipes 21 a and 21 b , there are provided the supply port 29 for adding a fresh aqueous treatment liquid from a fresh liquid replenishment tank 28 as shown by an arrow 75 and the supply port 30 for adding the ozone gas from an ozonizer 27 as shown by an arrow 76 . In this way, by arranging the supply ports 29 and 30 at predetermined locations of the supply-side pipes 21 (i.e. 21 a and 21 b ) connected to the inlets of the gas-liquid mixing pumps 13 (i.e. 13 a , 13 b , 13 c , 13 d ), the ozone gas and the fresh aqueous treatment liquid can be supplied to the gas-liquid mixing pumps 13 at a low pressure. In addition, with the arrangement, the possibility that the used aqueous treatment liquid containing any outflow substance coming off from the animal fibers may react with the ozone gas, is effectively lowered or suppressed.
The aqueous treatment liquid and the ozone gas are pumped out by the gas-liquid mixing pumps 13 (i.e. 13 a , 13 b , 13 c , 13 d ) to the static mixers 14 through the pipes 20 a and 20 b , and the ozone gas is mixed with the aqueous treatment liquid so that superfine ozone gas bubbles are formed in the aqueous treatment liquid and they are dispersed therein, in the static mixers 14 . The aqueous treatment liquid including the fine ozone gas bubbles is then discharged, or jetted, from the discharge nozzles 19 toward one surface of the mesh belt 12 (i.e. 12 a , 12 b ). In order to make the ozone gas bubbles efficiently come into contact with the mesh belt 12 , there is provided a nozzle cover 26 along a partial circumference of each of the discharge nozzles 19 , as shown in FIG. 6 .
FIG. 7 is a cross-sectional view taken along a line of VII in FIG. 2 ; and FIG. 8 is a cross-sectional view taken along a line of VIII in FIG. 2 . These figures show the arrangements of the discharge nozzles 19 , 19 and the suction ports 15 a , 15 b of the two lower circulation systems which are mounted on the descending portion 11 a of the tank 11 . In the respective circulation systems, the suction ports 15 a and 15 b are placed as close to the mesh belts 12 as possible. The suction port 15 a is coupled with the pipe 21 a which is connected to the inlet of the gas-liquid mixing pump 13 b , and the suction port 15 a is also coupled with the pipe 23 a which is connected to the circulation pump 17 . Similarly, the suction port 15 b is coupled with the pipe 21 b which is connected to the inlet of the gas-liquid mixing pump 13 a , and the suction port 15 b is also coupled with the pipe 23 b which is connected to the circulation pump 17 .
As shown in FIGS. 7 and 8 , in order to guide the mesh belts 12 (i.e. 12 a , 12 b ), there are provided a plurality of L-shaped guides 41 fixed to the inside of the tank 11 and a plurality of guide rollers 40 which are rotatably supported by and between the corresponding two guides 41 . With the arrangement, the guide rollers 40 prevent the mesh belts 12 a and 12 b from sagging under their own weights.
As aforementioned, each of the discharge nozzles 19 is placed at a position facing each of the corresponding suction ports 15 (i.e. 15 a , 15 b ), 16 (i.e. 16 a , 16 b ) with the mesh belts 12 locating therebetween. The two discharge nozzles 19 , 19 extend through the opposite side-walls of each of the descending portion 11 a and ascending portion 11 b of the tank 11 , and they are fixed to the guides 41 , respectively, as shown in FIGS. 7 and 8 . In the arrangement, the aqueous treatment liquid including the fine gaseous ozone bubbles sent from the static mixers 14 is discharged from the discharge nozzles 19 , in which non-uniformity, or unevenness, of treatment of the wool fibers of the continuous web form with the ozone gas in the direction of width thereof is suppressed or prevented.
FIGS. 9 and 10 are views showing the structure of the discharge nozzle 19 . The discharge nozzle 19 has a cylindrical body 42 having an elongate hole 43 for discharging, or jetting, the aqueous treatment liquid including the fine ozone gas bubbles. The cylindrical body 42 has a scatter prevention wall 44 , mounted so as to surround the elongate hole 43 , for the purpose of directing, or guiding, the ozone gas bubbles toward the mesh belts 12 .
In the arrangement, the aqueous treatment liquid including the ozone gas bubbles discharged from the discharge nozzles 19 , is guided toward the mesh belts 12 a and 12 b by the scatter prevention walls 44 , with the aqueous treatment liquid being prevented from spreading out or scattering by the scatter prevention walls 44 . The treatment liquid including the ozone gas bubbles thus jetted from the discharge nozzles 19 , passes through meshes, or openings, of the mesh belts 12 a and 12 b , and the treatment liquid including the ozone gas bubbles comes into contact with the continuous web form of the wool fibers. As shown by an arrow 77 in FIG. 11 which is an explanatory view showing a movement of the ozone gas bubbles 39 in the aqueous treatment liquid, the aqueous treatment liquid including the ozone gas bubbles 39 passes through the continuous web form 10 thereof by being sucked toward the suction ports 15 (i.e. 15 a and 15 b ) and 16 (i.e. 16 a and 16 b ).
That is, referring to FIG. 11 , the ozone gas bubbles 39 which have been discharged, or released, from the elongate hole 43 of the discharge nozzle 19 , pass through a plurality of openings of the mesh belt 12 a to reach the continuous web-like form 10 of the wool fibers. The continuous web form 10 of the wool fibers has gaps, or spaces, among the respective fibers 10 a thereof. The size of the gaps, or spaces, is very small. Therefore, preferably, the size of the ozone gas bubbles 39 is 50 microns or less, and more preferably, the size thereof is 30 microns or less. In other words, if the size of the ozone gas bubbles discharged is larger, the ozone gas finds difficulty in entering the inside of the continuous web-like form thereof.
As shown by arrows 77 in the figure, the suction ports 15 (i.e. 15 a and 15 b ) and 16 (i.e. 16 a and 16 b ) suck in the aqueous treatment liquid which has been discharged from the discharge nozzles 19 , so that the aqueous treatment liquid including the ozone gas bubbles 39 moves, or passes, through the gaps or spaces among the respective wool fibers 10 a . During this movement, the ozone gas comes into contact with the surfaces of the individual wool fibers 10 a ; the surfaces of the wool fibers 10 a are allowed to react with the ozone gas; and the surfaces thereof are chemically modified. The ozone gas bubbles 39 and the aqueous treatment liquid which have reached the opposite surface of the wool fibers of the continuous web form 10 , are sucked by the suction ports 15 and 16 , and these bubbles 39 and liquid are guided to the gas-liquid mixing pumps 13 (i.e. 13 a , 13 b , 13 c and 13 d ) for circulation.
As shown in FIG. 6 , and as aforementioned, there are provided a pair of the circulation pumps 17 , 17 in the treatment apparatus. Namely, one of the circulation pumps 17 , 17 is connected to the suction ports 15 a , 15 b and 15 c mounted on the side of the descending portion 11 a ; and the other of the circulation pumps 17 , 17 is connected to the suction ports 16 a , 16 b and 16 c mounted on the side of the ascending portion 11 b , respectively. With the arrangement, the force to suction the aqueous treatment liquid including the ozone gas bubbles in the circulation system, is enhanced. The aqueous treatment liquid which has been supplied to the circulation pump 17 through the pipe 24 , as shown by an arrow 73 in FIG. 6 , is sent back into the tank 11 through the pipe 22 (refer to FIG. 2 ), as described above. As shown in the same figure, the pipe 22 is provided with a heat exchanger 25 for regulating, or adjusting, the temperature of the aqueous treatment liquid contained in the tank 11 , thereby realizing a suitable temperature thereof for the ozone treatment (about 20° C. to 60° C.) of the wool fibers 10 .
As described above, according to the arrangement of the treatment apparatus installed in the wool fiber treatment system, fine bubbles of the ozone gas are continuously blown, or jetted, to the wool fibers of the continuous web form from one side of the continuous web form thereof, and at the same time, the aqueous treatment liquid including the ozone gas is continuously sucked from the other side of the continuous web form thereof, thereby making the ozone gas reach up to the inside of the wool fibers of the continuous web form thereof.
Also, according to the arrangement thereof, the suction ports 15 a , 15 b and 15 c which are mounted on the descending portion 11 a of the tank 11 , are positioned on one side of the wool fibers of the continuous web form 10 ; on the other hand, the suction ports 16 a , 16 b and 16 c which are mounted on the ascending portion 11 b of the tank 11 , are positioned on the other side of the wool fibers of the continuous web form 10 , thereby preventing, or suppressing, the unevenness of treatment of the wool fibers of the continuous web form 10 in the direction of thickness of the continuous web form 10 thereof.
Also, according to the arrangement thereof, the circulation pumps 17 , 17 are connected to the suction ports 15 (i.e. 15 a , 15 b , 15 c ) and 16 (i.e. 16 a , 16 b , 16 c ), thereby enhancing the force to suck the ozone gas bubbles. This improves the efficiency of suction of the ozone gas.
A fresh liquid and ozone gas are always supplied into the circulation systems, and they are circulated therein. This prevents the ozone gas from being consumed due to reaction with the treatment liquid containing contamination coming off from the wool fibers, thus enabling supply of the ozone gas at a high concentration for reaction with the wool fibers of continuous web form.
Also, according to the arrangement thereof, the aqueous treatment liquid in the circulation systems can be maintained at a temperature at which dispersion of the ozone gas is facilitated, and at the same time, the conditions for the reaction in the tank can be easily adjusted by adjusting the conditions of the treatment liquid pumped out from the circulation pumps 17 , 17 .
Although the present invention has been fully described in connection with the preferred embodiment thereof with reference to the accompanying drawings, it is to be noted that various other changes and modifications are also apparent to those skilled in the art. Such changes and modifications are to be understood as included within the scope of the present invention as defined by the appended claims unless they depart therefrom.
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A mechanism, giving less environmental load, for treating animal fibers of a continuous web form so as not to spoil inherent properties of the animal fibers such as hand-feeling and water repellency, so as to improve resistance to felting (shrinkage) and pilling. The mechanism includes: a tank filled with a treatment liquid; a net-conveyor having upper and lower mesh belts put one upon the other to sandwich the continuous web form therebetween for conveying the web form through the liquid of the tank; a treating-liquid circulation system including a gas-liquid mixing pump connected to a suction-port in the tank and pumping out the liquid, a static mixer connected downstream of the pump, and a discharge nozzle placed at a position in the tank facing the suction-port with the mesh belts therebetween, the discharge nozzle being connected downstream of the mixer; and an ozonizer for supplying ozone gas into the system.
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BACKGROUND OF THE INVENTION
The present invention relates to an interlock system for determining whether a door or cover is closed and latched. When a door on a cab on an industrial vehicle, such as a skid steer loader, is unlatched, a lock out signal to disable components of the vehicle is provided until such time as the cab door is again closed and latched.
Skid steer loaders are operated with rollover protection cabs, and in inclement weather, either hot or cold, the cab can be enclosed, and a door provided on the operator entrance opening. It has been found that because of the compact nature of skid steer loader, in particular, if the door is fully opened and the lift arms of the loader are operated, the door can become damaged by the lift arms.
SUMMARY OF THE INVENTION
The present invention relates to a sensor for determining when a latch on a door or other hinged cover is closed and latched to provide a signal indicating the door or cover is properly latched closed. The signal is used, as disclosed, as a signal to an interlock system, and when the latch is not properly secured with the door closed, that is, when the door is ajar or open, controls for operation of some secondary system, such as the lift arm and bucket tilt cylinder of a loader, are disabled.
A switch used for determining when the door is closed and latched can be a magnetic reed switch or a Hall effect sensor, with a magnet mounted on a latch striker or bolt secured to the frame of the cab. The sensor is positioned on the door so that unless the door latch is adjacent to and in alignment with the magnet on the striker bolt, that is, fully seated or secured, there will be no enabling signal to permit operation of the selected system, for example, the lift and tilt cylinders of the loader, that are used for operation of the lift arms.
The skid steer loaders that are made by Bobcat Company, a business unit of Ingersoll-Rand Company presently include a interlock control system that prevents operation of the vehicle in response to selected sensor inputs indicating a selected condition. The sensor of the present invention is designed to provide an input to such a system so that when the door is in place on the cab, an additional signal from the latch sensor is needed to enable the operation of the lift arms and bucket cylinders of the skid steer loader. The same arrangement can be used for locking our functions on other vehicles or systems that have a door or cover that should be closed and latched before the selected functions are enabled.
The present door shown will provide an input to similar interlock systems where a controller is disabled when the sensor signal indicates that a door or cover is not closed and latched.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a schematic perspective view of a skid steer loader having an interlock system made according to the present invention;
FIG. 2 is a fragmentary perspective view of a typical door and latch arrangement;
FIG. 3 is an enlarged, exploded rear perspective view of a door frame and latch assembly as viewed from the interior of the cab;
FIG. 4 is an enlarged exploded perspective view showing a typical latch assembly from an exterior of a cab door having a sensor system of the present invention installed;
FIG. 5 is a rear view of the latch from the interior of the cab showing the striker and the door latch in a latched position with parts broken away;
FIG. 6 is a schematic rear view of a latch having a modified sensor, showing the latch and a sensor from an interior of the cab;
FIG. 7 is a side sectional view of FIG. 6 ; and
FIG. 8 is a fragmentary detailed view of a latch striker of FIG. 6 , with parts broken away.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
A skid steer loader 10 is shown in FIG. 1 , and it has a frame 12 , supported on wheels 14 , and further it has a pair of pivoting lift arms 16 that are operated with hydraulic actuators 18 . The lift arms support a tilting bucket 15 that is raised with the lift arms and tilted using a tilt hydraulic cylinder or actuator 17 . The skid steer loader has a cab 20 , as shown, and in this instance, a door assembly 22 (see FIG. 2 ) is provided on the cab. The door can hinge between an open and closed position. An engine 24 is used for providing power to a hydraulic system including a hydraulic pump 26 connected to a lockout valve 36 , and providing power to a set of actuator hydraulic valves 28 and then to the various hydraulic components such as the lift arm actuator 18 and bucket tilt actuator 17 . Drive hydraulic motors 30 are used for driving the wheels 14 in a conventional manner.
A drive interlock system 32 , is provided as is disclosed in U.S. Pat. No. 5,425,431 in greater detail. The specification of U.S. Pat. No. 5,425,431 is incorporated by reference. The interlock system 32 has logic controls that, among other functions, enables or disables the operation of actuator hydraulic valves 28 , through a lockout valve 36 and it also can control operation of drive motors 30 (or other drive), through a drive lockout 31 . Operation of the lift arm cylinders or actuators 18 , and the tilt cylinders or actuators 17 is enabled only when lockout valve 36 is open.
In the present invention, whenever a door is installed on a cab, a circuit is closed by a normally closed switch or sensor 56 on the door latch, that will be more fully explained, unless the door is closed and a door latch is secured or latched. The closing and latching of the door assembly 22 relative to the cab frame around the door opening on the cab 20 provides a signal to the interlock system 32 by opening the switch or sensor 56 so the lockout valve 36 is enabled or open and the actuator valves 28 receive hydraulic fluid under pressure. The valves 28 can then be operated to provide hydraulic fluid to the cylinders 18 , and 17 .
If desired, the door latch switch or sensor can be used to control other functions of a vehicle, such as operating the drive lockout 31 to prevent the vehicle or loader from moving until the door is closed and latched. Interlock valve 36 must be open in order for hydraulic fluid under pressure to be provided to the hydraulic valves 28 . When interlock valve is closed or disabled it completely shuts off the operation of the selected components or functions of the machine including hydraulic cylinders. The lift actuators 18 and tilt actuator 17 are disabled until the door is closed and latched. Other inputs 33 , as disclosed in U.S. Pat. No. 5,425,431, also may be needed to enable valve 36 and drive lockout 31 .
The door 32 is hinged as at 40 , along one side relative to the cab, and is positioned in a door opening frame shown at 42 . The door assembly 22 is generally made with an exterior peripheral frame in which a transparent panel is supported a shown in U.S. Design Pat. No. D437,275. The door has a handle panel portion 44 that includes a latch assembly plate 46 .
The latch assembly plate 46 supports a conventional door latch assembly 48 , that is operated from a push button handle 50 , also of conventional design. The push button on the handle engages a lever 50 A on the interior of the door that operates cams to open the door. An operator handle 53 in the cab 20 permits the operator to open the door. The handle 50 is securely clamped onto the latch plate 46 .
Movement of the push button on handle 50 operates against lever 50 A so cams move in a conventional manner and open or separate a pair of spring loaded latch dogs 52 , that are pivotally mounted between a plate 49 as supported in a latch housing 58 , and an outer wall 59 of the latch housing 58 . The details of the latch operator are not shown, but the push buttons and lever operate to open or separate the latch dogs 52 , which are spring loaded to a closed position.
The latch housing 58 is used to also support a normally closed latch sensor or switch 56 that is mounted on a bracket 57 which is attached to an inner side of plate 49 . The closed switch 56 closes a circuit and provides a signal to the interlock system controller 32 to close lockout valve 36 whenever a door is installed. The latch housing wall 59 and plate 49 have U-shaped openings or notches 60 that are open on the interior side of the latch and that will receive a latch striker bar 62 that is mounted onto the door opening frame wall 65 on the cab. An end 63 of the latch striker bar 62 , extends through an opening in wall 65 , forming part of the door opening frame on the cab and is held fixed on the wall 65 with a nut in a normal manner.
The latch striker bar 62 is a cylindrical shaft. The latch dogs 52 will cam on the latch striker bar and the spring load on the latch dogs permits them to separate to fit over the striker bar 62 and latch in place when the door is fully closed.
The latch striker carries a permanent, preferably high strength, magnet 66 on a head end 67 of the striker bar. The magnet 66 is suitably positioned to be aligned with an adjacent sensor or switch 56 only when the door is in closed and latched position. The notches 60 in wall 49 are open so the magnetic field from magnet 66 affects notch or sensor 56 when the door is closed and latched. The magnet 66 is held in a recess in the head end 67 of the striker bar 62 , which can be seen in FIG. 5 where the head end 67 of the striker bar 62 has been broken away. When the door is closed and latched, the normally closed sensor or switch 56 will be shifted in state or position to open due to the presence of the magnetic field from the magnet 66 .
The sensor 56 can be a magnetic reed switch, or can be a Hall effect sensor with the actuating magnet 66 carried in the striker bolt or bar 62 .
The sensor leads are extended along the door frame 40 that is used for supporting the glass in the door, and the leads are connected with a coupler 70 on the door that connects to a connector 71 on the frame 12 of the loader that leads to the controller 32 .
In many instances, an industrial vehicle will be operated without a door, and thus, the present arrangement is designed to permit operation of the loader lift and tilt cylinders when a door is not used. The wiring on the loader body can remain in place and the lift and tilt cylinders will be operable.
When a door is not originally present or is taken off, the coupler 70 is separated from connector 71 and the circuit to the interlock controller is open. The normally closed switch or sensor 56 is removed with the door. With the circuit open, there is no signal from the door circuit that causes the controller 32 to close the interlock valve 36 .
The switch or sensor 56 is normally closed as stated, and when the door is installed, the coupler 70 is connected to connector 71 on the frame 12 . The switch 56 is closed and the controller 32 causes the valve 36 to move to position to block operation of the loader lift and tilt actuators. When the door is removed and the coupler 70 and connector 71 separate, the sensor or switch 56 is no longer in the circuit so the circuit is open and the interlock valve 36 is not closed by the door latch circuit.
When the door 23 is in place, the door 22 preferably has to be closed and latched so that the sensor component 56 on the door is operated (opened) by the component on the striker or on a fixed portion on the cab, such as a door frame to “enable” the interlock valve 36 .
It also should be noted that the latch can be on the cab, and a fixed striker positioned on the door. When desired, the sensor arrangement can be selected to sense a door closed, but not fully latched position. The door position could be one where it was known that the door was not going to interfere with, or be in the way of, the lift arm movement.
FIGS. 9 and 10 show a modified form of the invention schematically. A latch plate 76 that mounts onto a door 78 is shown in latched position, with latch dogs 80 . A striker cylinder or bar 82 is held in the latch dogs. The striker bar is mounted onto a fixed cab frame wall 84 .
In this form of the invention, the striker bar 82 has a flange 88 that carries locating pins 90 that are not symmetrical about the axis of the striker bar, and which will fit in provided receptacles 92 in the cab frame wall to make sure that the positioning of the magnet 94 is correct for alignment with a Hall effect sensor 96 that is supported on the latch housing 98 .
The magnet 94 , as shown in FIG. 9 , is inserted into a cross hole or bore 100 in the striker bar. Hole 100 is of size to receive the magnet 94 . A smaller diameter cross bore 102 is provided in alignment with the bore 100 , so that the magnet can be either pushed out or pounded out of hole 100 for replacement.
The Hall effect sensor 96 is connected to the interlock system 32 so that when the door is on the loader but is not closed sufficiently the lift and tilt actuators and other selected power components are disabled, as previously explained. Variations in sensors thus can be made, and variations in magnet mounting also can be provided.
The strength of the magnet field, and the sensitivity of the sensor can be selected so that mounting one or both of the sensor components adjacent the latch and/or striker will provide a door position signal that will enable the lift arms when the door will not be in the path of the lift arms.
In automotive applications, a door striker for a door latch is used and the same sensor system can be utilized. Some door latches operate so that if tripped but not fully latched, the door latches have to be reset by operating the door latch before the door can be fully closed and latched. The sensor system of the present invention is preferably sensitive to the fully closed and latched position of the door and will not permit operation of the controlled function until both door closing and latching occurs. However, as pointed out, in some applications a signal indicating the door is in a closed or newly closed position is satisfactory.
Although the present invention has been described with reference to preferred embodiments, workers skilled in the art will recognize that changes may be made in form and detail without departing from the spirit and scope of the invention.
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A skid steer loader has an interlock system that is responsive to sensor input to lock out such as operation of lift and tilt cylinders of the skid steer loader when the input indicates a condition has not been met. The loader is provided with a cab that has an operator entrance and egress door, and a door latch and a latch striker on the cab are provided with a sensor that senses when the cab door is closed and latched. The lockout prevents carrying out the functions when the door is not closed and latched.
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BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention relates generally to the field of vehicular traffic safety, and more particularly to a removable and portable speed bump which can be easily carried and/or stored on-site where the speed bump is intended to be deployed.
2. State of the Art
Speed bumps have been used for some time to slow down traffic in certain areas where the traffic speeds must be reduced, such as construction areas, school zones, parking lots, pedestrian zones and similar areas. Some speed bumps are permanent in nature and are made from asphalt or concrete. Permanent bumps or ramps are also used to guide traffic or indicate some change in traffic flow. These permanent speed bumps are useful but they have the disadvantage that they can not be moved or taken away when they are not needed. Other speed bumps exist which can be moved but are not easily stored at the desired site of the speed bump such as U.S. Pat. No. 3,880,537 to Jensen and U.S. Pat. No. 5,775,834 to Jackson. Such speed bumps typically are not as durable as one might desire and are unnecessarily complex to install.
Road hazard warning devices are also a common type of traffic control. These road hazard devices usually consist of visual markers like flags, signs, cones, or reflective barrels to warn oncoming vehicle traffic of road work or other road dangers. In some hazard situations, a flagman holds a flag to signal traffic hazards or the need for speed reduction. This is a dangerous job because the flagman is standing in traffic and it is usually temporary in nature. The flagman moves to sites where the flag is needed, and the positions where a flagman is needed change on a daily basis. Traffic passing a flagman will normally reduce its speed, but it would be helpful for the flagman to use a temporary speed bump or similar device which requires the traffic to slow down. A temporary speed bump would force traffic to reduce speed and in turn create a safer area for the flagman. In some situations, a temporary speed bump could even replace a flagman where the speed of the traffic is only being controlled and there is no need to control the traffic flow. A temporary speed bump is needed which can be deployed for a short periods, for example, for just a day or a few hours at a time in a school zone. It would also be an advantage if the speed bump could be set up and removed in minutes.
Highway warning devices exist, such as U.S. Pat. No. 5,775,834 to Jackson and U.S. Pat. No. 5,769,653 to Flynn, which create an audible warnings as cars drive across. These prior art devices warn drivers of impeding hazards with rib or wave like structures but they do not require vehicles to slow down to cross their warning structures. The ribs or waves are large enough to create an audible warning and slight vertical motion when vehicles cross them but these structures do not vehicles to reduce their speed.
Existing temporary traffic hazard systems may be portable and deployed when needed but these systems have disadvantages. Typical temporary road hazard markers are not fastened in place but remain in place by their own weight as taught by U.S. Pat. No. 3,880,537 to Harris and U.S. Pat. No. 5,639,179 to Jensen. Many traffic hazard markers such as those disclosed by Jensen also rely on the weight of the units to hold them in place by attaching the modules together. Such traffic speed bumps or markers are not particularly attached to the road surface which may allow them to move or be knocked down when crossed by a vehicle or affected by wind and weather conditions.
The current invention overcomes the disadvantages of the prior art by providing a stable traffic speed bump system which can be used temporarily and then stored after it has been used.
OBJECTS AND SUMMARY OF THE INVENTION
It is an object of the invention to provide a movable and portable speed bump system which is easy to setup on or remove from a roadway.
It is a further object of the invention to provide a movable speed bump which can be readily removed and stored, for example, during snow removal or road and parking lot cleaning, etc.
It is still a further object of the invention to provide a speed bump system which allows the flow of water therepast.
The present invention is a removable and portable speed bump system using a flexible connector such as a chain or cable lying transversely across the roadway, and a number of generally triangular, or arch-shaped, spaced-apart bump modules disposed on the connector for which cars must slow down to cross. The speed bump modules are either fastened to the flexible connector or molded directly onto the flexible connector. The flexible connector is attached to a connecting anchor fixed into the road curb or road shoulder of a roadway. The opposite end of the flexible connector is fastened to a clasp or spring-loaded link set at a second point transversely across the roadway from the connecting anchor.
The speed bump modules are configured to enable stacking in a compact fashion, for example, in a special container located on the side of the roadway.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a perspective view of a movable speed bump system made in accordance with the present invention;
FIG. 2 is a front view of the speed bump system showing the wheel base and tires of a vehicle passing over the movable speed bumps;
FIG. 3 is a side perspective view of one speed bump module showing the preferred generally triangular shape of the speed bump modules;
FIG. 4 is a cross cut side view of a single speed bump module in the speed bump system;
FIG. 5A is an end view of a speed bump module showing a triangular embodiment;
FIG. 5B is an end view of a speed bump module with an arched embodiment used in the speed bump system;
FIG. 5C is an end view of a speed bump module with a dome shape used in the speed bump system;
FIG. 6A is a side view of the speed bump system showing the speed bump modules stacked in a storage container;
FIG. 6B is a view of the speed bump system showing the speed bumps stacked in a storage container with the container door closed;
FIG. 7 is a top view of the speed bump system showing a speed bump with flourescent or reflective lines painted next to the speed bump system.
DETAILED DESCRIPTION
FIG. 1 illustrates the preferred embodiment of the invention and shows the removable and portable speed bump across a roadway. The invention forces vehicles which pass over the speed bump to reduce their speed to avoid the uncomfortable jarring motion that is created if the speed bump is crossed quickly. The speed bump is attached to the roadway 12 with a connecting anchor 10 . The anchor in the preferred embodiment is an eyebolt which can be secured into the roadway curb or into the shoulder of the road. It should be noted that one who is skilled in the art could devise other methods which would attach the speed bump to the roadway, curb or road shoulder such as metal loops, bolts, screws or the like.
The speed bump itself consists of a number speed bump modules which are elongated rigid bodies arranged in a series. In the preferred embodiment, these speed bump modules can be made of any number of materials including but not limited to rubber, plastic, recycled plastic, rubber covered metal or any other similar material which is partially deformable. It should be noted at this point that the modules in the preferred embodiment of the invention are generally solid and only slightly deformable as a result. If the bumps are very deformable they will not be effective and the result is a speed bump where vehicles do not reduce their speed. Although speed bumps have been devised which are hollow and hollow speed bumps can be substituted for the solid bumps of this invention, solid speed bumps generally wear better. Solid speed bumps also sit better on the road surface because of their weight. The speed bump modules can be made of materials which are not deformable such as concrete or metal but these are not preferred because they are not as easily transportable, light, or movable.
The speed bump modules are connected by flexible connectors 16 to form an alternating series of speed bump modules and connectors. The flexible connectors in the preferred embodiment are metal chains but the connectors could also be plastic chains, plastic connectors, rubber connectors, metal cables, rubber coated cables or chains or any similar type of flexible connector. It should be noted that these connectors must be strong enough to withstand vehicle tires passing over them and the forces created by vehicle traffic. Enough slack is left in the connectors or chains between each set of speed bump modules to allow the chain to touch the road surface when a vehicle passes over it.
At the opposite side of the road is a fastener 18 to which the series of speed bump modules can be attached. This fastener in the preferred embodiment is a strong loop 18 made of metal or similarly strong material or plastic, which is recessed into the road surface. An attachment link 20 connects the fastening loop 18 to the last flexible connector 22 in the speed bump series. The link is a quick link, a snap spring link or a normal lock. The preferred attachment link is a connector that can be attached or detached in a matter of seconds. Another embodiment of the fastener would be a pop-up eyelet mounted flush to the ground in a mounting bracket. It is also conceivable that a hook, looping method or any other type of well known method for connecting a chain or cable to the strong loop 18 could be used.
Another important part of this invention, which is shown in FIG. 1, is the storage container 24 which is attached to the road side or curbside next to the speed bump anchor. The storage container 24 has a door 26 which opens and then the speed bump modules 14 are stacked inside the storage container 24 and the door 26 is shut and locked. This is a very convenient method for using the speed bump modules because they are stored next to the location where they are used. A warning signal with a fold over sign 28 can also be attached to the storage box to indicate that a speed bump has been deployed. The sign is folded over when the speed bump is stored in the container and displayed when the speed bump is in use. In another embodiment of this invention (not shown), the speed bump modules can be anchored to the storage container so they can be stacked in the storage container which is be fastened to the road side. If the speed bump modules are attached to the storage container and the container is not fastened to the roadway then the container and the speed bump modules can be moved as desired. This configuration is especially useful for a speed bump in a temporary construction zone.
In an alternative embodiment, the speed bump can be deployed on an unfinished road surface such as a dirt road or gravel at a construction site. With this configuration, a stationary point is required to attach the connecting anchor 10 into the road side and another stationary point is needed to attach the removable fastener 18 into the transverse road side. The anchor and fastener can be connected to a piece of concrete in the road shoulder, a heavy cement block, a metal anchoring block, or similar anchoring structures. This is an advantage over the prior art which would be difficult to install on an unfinished road surface because they need to be fixed into a finished road surface.
Now referring to FIG. 2, which is a front view of the speed bump system, the invention has the advantage that a vehicle driver who carefully drives across the speed bump may guide the vehicle's tire 34 to cross only one speed bump module 36 while the other tire 30 will cross a connecting member or chain 38 . A vehicle driver who avoids driving one tire 30 over the speed bump modules 14 reduces the jarring motion felt by the passengers of the vehicle but the vehicle must still reduce its speed. In addition, allowing the driver to avoid one speed bump is easier on the vehicle's suspension 32 .
FIG. 3 is a perspective view of a triangular shaped type of elongate member or speed bump module. It can be seen in this invention that the speed bump is triangular in shape, but there is no apex of the triangle. Even though a triangular shape with an apex can be used in this invention, the flattened top surface 42 of the speed bump allows vehicles to more easily pass over the speed bump. The speed bump modules also have a cylindrical aperture or hole 40 in the end of the bump. This hole 40 allows a screw or screw type bolt to be fastened into the speed bump. The preferred embodiment of this invention uses an eyebolt which has a threaded end to screw into the speed bump. The eyebolts are then coupled to the flexible connectors to connect the speed bump modules together. In one embodiment of the invention, metal chains used as connectors would be manufactured with the eyebolts already connected to the metal chain.
In an alternative embodiment, the cylindrical hole runs completely through the speed bump module to allow a flexible connector to pass through the speed bump. This allows the speed bump modules to be connected with one flexible line which runs through the center of all the modules instead of using multiple connectors. In this embodiment, pins would be used at the module ends or inside the modules to couple the speed bump modules to the flexible line so that the speed bump does not rotate or move lengthwise on the line. Alternatively, the speed bump modules could be crimped or formed such that the speed bump can not move lengthwise on the flexible line or chain.
FIG. 4 is a cross cut view of the speed bump in FIG. 3 on the line 3 — 3 . The cylindrical hole 40 for fastening eyebolts is shown, along with the cylindrical shafts 44 and 46 into which the eyebolts are threaded. The cylindrical shafts 44 and 46 could also be one continuous cylindrical shaft which passes through the speed bump.
FIG. 5A is an end view of a speed bump module where the shape of the bump is somewhat triangular in shape. The cylindrical hole 40 for fastening bolts is shown along with a top surface 42 which replaces the apex of the triangular shape, two triangularly angled sides 48 and 50 , and a flat bottom 52 which is designed to sit on the road surface.
FIG. 5B is the end view of another embodiment of a speed bump module with an arched shape. This figure shows the arched shaped top surface 54 which forms the bump, the cylindrical hole 40 for fastening bolts, and the flat bottom 52 as described above. The cylindrical hole in FIG. 5B is shown closer to the bottom of the speed bump to illustrate that the point where the flexible connector is secured to the speed bump may be varied depending on the connector used or the amount of slack desired between the speed bump modules.
FIG. 5C is another end view of an embodiment which is a dome shape. This figure shows the dome shaped top surface 56 , the cylindrical hole 40 for fastening bolts and the flat bottom surface 52 which is designed to sit on the roadway.
The speed bump modules in the preferred embodiment are approximately 1-6 inches high with 4 inches being the preferred height. The speed bump modules have a width which increases depending on the height, and they are approximately 24 inches in length. Further, the preferred length of the flexible connectors between each speed bump is approximately 18 inches. The preferred length arrangement between the speed bump modules and the flexible connectors is such that if a vehicle (car or truck) with an axle length of between 56-70 inches avoids a speed bump with one wheel, the vehicle will drive over a speed bump with the other wheel. It should be recognized that the speed bump modules could be of various heights, widths and lengths, as long as the dimensions are sufficient to require a car to slow down to comfortably drive over the bump and not so tall that a car could not drive over it.
In FIG. 6A the speed bump modules 14 linked by the flexible connectors 16 , are shown stacked on a shelf 58 in a storage container 24 with a door 26 . The first flexible connector 16 is shown attached to the connecting anchor 10 which is secured into the roadway 12 or road curb.
In FIG. 6B the speed bump modules are stacked in the storage container 24 with the door 26 closed. The door handle 60 and door hinges 62 are also shown. The first flexible connector 16 is shown attached to the anchor 10 which is secured into the road 12 or road curb. The first flexible connector 16 is seen passing through an aperture or hole 64 in the container door 26 so that the speed bump modules stay connected to the anchor 10 in the roadside.
FIG. 7 shows a top view of the speed bump modules when they are deployed for use. This figure shows flourescent lines 66 painted on either side of the speed bump modules and it also shows the lane divider lines 68 on the roadway.
It will be appreciated that other embodiments of the present invention may be employed in many applications to accomplish a removable and portable speed bump. While certain preferred embodiments have been explained above, the appropriate scope hereof is deemed to be in accordance with the claims as set forth below.
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A removable and portable speed bump system using a flexible connector such as a chain or cable lying transversely across the roadway, and a number of generally triangular, or arch-shaped, spaced-apart bump modules disposed on the speed bump for which cars must slow down to cross. The speed bump modules are either fastened to the flexible connector or molded directly onto the flexible connector. The flexible connector is attached to a connecting anchor fixed into the road curb or road shoulder of a roadway. The opposite end of the flexible connector is fastened to a clasp or spring-loaded link set at a second point transversely across the roadway from the connecting anchor. The speed bump modules are configured to enable stacking in a compact fashion, for example, in a special container located on the side of the roadway.
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BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to a method for optimizing the scanning process of a mobile terminal, the scanning process being performed by the mobile terminal in order to discover an available network to which a connection is possible, wherein at least a part of existing networks is registered to a server, wherein said server provides its information regarding the registered networks to the mobile terminal.
2. Description of the Related Art
In recent years several types of wireless communication systems have been developed. For example, wireless local area networks (WLAN) are widely spread nowadays, cellular networks, such as Universal Mobile Telecommunication Systems (UMTS), have gained paramount importance, and, most recently, WiMAX (defined as Worldwide Interoperability for Microwave Access) has been developed as a standard-based technology enabling the delivery of last mile wireless broadband access. Each of these systems provides different types of services and specific applications.
According to the existing different types of wireless communication systems, mobile terminals nowadays support multiple network interfaces, with WiFi, UMTS, GSM and Bluetooth already available in the market. While connection to the GSM/UMTS network is neatly arranged by network operators, other networks, such as WiFi and Bluetooth, require continuous scanning of the mobile terminal to guarantee a reasonable percentage of connection time. In order to discover available networks, the terminal needs to perform a technology-specific scan function. In general, this results in such intensive battery consumption, that the mobile terminals functionality is drained at unacceptable rates.
In the case of networks where the terminal receives advertisements (for instance, beacons), such as in WiFi, the scanning time may be considered as the period in which the wireless card is listening on the radio link and can receive such advertisements. During the rest of the time, the device is considered as non listening. When a protocol does not provide any advertisements, such as Bluetooth Inquiry or WiFi active Probe Request modes, a scan is considered as the initiation of the scanning process.
Certain strategies have been developed, such as the MIH (Media Independent Handover), which communicate available networks within a given area to mobile terminals. Consequently, the terminal does not have to perform a scanning process, but can directly attempt to connect to the known networks in its vicinity. However, devices that are not MIH-enabled need to periodically scan for available networks, resulting in rapid battery consumption as mentioned above. MIH-enabled devices, on the other hand, can save battery and scanning time when using the information regarding available networks provided by the MIH service. In the context of the MIH service, this information is usually provided by an information server (IS) to which existing networks are registered.
However, there will always be situations in which mobile devices can not use the information provided by the information server, either because the information is incomplete or outdated. This may be due to the fact that networks that do exist have not been registered yet in the IS. In such cases, the terminal is reduced to non-MIH functionality, which typically involves periodical scans according to the policies implemented in the terminal. Such a situation can be described as a non-MIH operation of MIH-enabled devices, in which terminals act as they were not MIH-enabled, i.e. they have to periodically scan in order to discover available networks to which connection is possible.
SUMMARY OF THE INVENTION
It is therefore an object of the present invention to improve and further develop a method of the initially described type for optimizing the scanning process of a mobile terminal in such a way that by employing mechanisms that are readily to implement a high level of connectivity with a power consumption as low as possible is achieved.
In accordance with the invention, the aforementioned object is accomplished by a method characterized in that the scanning period of the mobile terminal is dynamically adjusted on the basis of information provided by the server.
According to the invention is has been recognised that by using information regarding available networks, which is provided by a server to which existing networks can be registered, a dynamic adaptation of the scanning period of a mobile terminal can be performed. By specifying the scanning period depending on information provided by the server regarding available networks, at least the same level of connectivity as with traditional scanning methods can be achieved, but with an optimized power consumption and, therefore, with an increased battery life.
The method according to the invention can be suitably applied, for instance, in MIH environments according to the IEEE 802.21 standard. In such a case, the MIH Information Server (IS) would function as the server to which existing networks can register and which provides its information regarding the registered networks to the mobile terminal. However, it is to be understood that the invention is applicable in any scenario in which a server is provided to which networks can register, and wherein said server is enabled to provide information regarding registered networks to mobile terminals. Consequently, when the invention is described with respect to MIH in the following, this reference is to be understood as an exemplary reference only, and it is to be expressly pointed out that it is in no way intended to limit the invention in any way.
In an especially advantageous embodiment a probability P R of a network to be registered in the server is estimated and the mobile terminal's scanning period is determined on the basis of said estimated probability P R . When P R is the probability of a particular network being registered in the server, P R gives, in other words, the percentage of networks that are known to the server or, in the special application scenario of MIH technology, to the MIH Information Server (IS), respectively. P R is always lower as one, or equal to one in the case that all existing networks within a specified area are known to the server. To optimally adjust the scanning period of a terminal, the scanning period is shortened the lower the estimated probability value P R . The estimation of the probability value P R may be performed either by each terminal on the basis of the information received from the server or by the server itself which constitutes a more centralized approach. In the latter case it may be provided that the probability values P R are transmitted from the server to mobile terminals upon special requests from the part of the terminals.
In a further advantageous embodiment users are enabled to report networks to the server, the reports being employed by the server to update its knowledge of existing networks, and the probability P R is dynamically recalculated by the server on the basis of said network reports received form users. By enabling users to send messages to the server in order to report networks to the server, a high degree of freshness, richness, and completeness of information stored in the server is achieved. The communication nodes updating the information in the server may be individual users, preferably costumers of the operator of the server, or other network operators. By allowing users to conduct the updates of the server by themselves, the system is very dynamic and loyal to the current state of the network with the information in the server being always fresh and thorough due to periodically updates by users in the field.
In a concrete embodiment, it may be provided that the server employs reports on the part of users only after having performed a plausibility check according to configurable criteria. In other words, the server decides about the acceptance of messages received form a user/communication node according to configurable criteria. Only in cases in which specified criteria are fulfilled, the server employs the content of a message in order to conduct an update operation. Otherwise the message may be discarded. For example, the plausibility check may include a measurement to identify a network reported by user as a moving network, that is, a network that is not affixed to a static location. Additionally, mechanisms may be implemented to prevent simple spam from being reported. Furthermore, the configurable criteria may, for example, include the kind of authorization of the communication node, i.e. the server may be configured in such a way that only messages from authorized communication nodes are further processed. The authorization may be due to the fact that the respective communication node is registered as a customer of the operator which is responsible of managing the server.
In addition to authorization issues, the server may conduct further plausibility checks. For example, the server may use information forwarded to it by a communication node for an update only in such cases in which it receives a configurable number of messages from different communication nodes containing the same (or essentially the same) readings within a configurable time period. In reverse this means, that an isolated message will be condemned as untrustworthy. For example, if a communication node reports on a network not yet registered in the server, the server will attend to the registration of this network only if the existence of this network is confirmed by other communication nodes from the same geographical region. This mechanism strongly supports the detection of intentionally faked information from certain users.
Regarding the adjustment of the probability P R it may be provided, that the probability P R is decreased each time the server receives a user report (which, where appropriate, has being checked and qualified as being trustworthy) regarding a network of which the server had not yet previous knowledge. By decreasing the probability P R it is taking into consideration that, obviously, there are (many) existing networks which are not yet registered to the server.
On the other hand, the probability P R may be slightly increased towards the value 1, if the server receives no user reports of yet unknown networks over a long period of time. In such a case, it is very likely that all existing networks are already registered to the server. However, the probability P R may be decreased in the case the server does not receive any user reports at all over a long period of time. By this means one can take into account the lack of freshness of the information stored in the server regarding available networks. The time period after which the probability P R will be increased/decreased may be implemented as a configurable parameter.
An additional parameter to be considered in the calculation of the probability P R may include a prediction of the amount of unknown networks. Such a prediction could be made, for instance, by means of machine learning techniques.
With respect to a high accuracy it proves to be advantageous to perform the estimation of the probability P R specific to a certain geographic area. The smaller the geographical area for which a probability value is generated, the better is the information for an individual mobile terminal which will choose, in order to adjust its scanning period, a probability value that fits to the geographic area where the mobile terminal is currently located. The degree of granularity may be determined depending on the positioning mechanism provided by the server. The areas will usually be bigger than the maximum resolution of the positioning system.
With respect to an effective storage of the individual probabilities, it may be provided that the individual probabilities P R for each specified area are stored by the server in a spatial database or by means of the GIS (Geo Information Service) storage mechanisms.
Advantageously, for each specified area an individual probability P R is calculated for each of the different access technologies. By this means it is possible for a mobile terminal which, for instance, exclusively searches for a WiFi network (maybe because the terminal supports only such a network interface) to adjust its scanning period on the basis of a probability P R value which takes into consideration only the local situation regarding existing WiFi networks.
It may be provided that a probability P R that is valid for a certain area is also transmitted to areas neighboured to said area. The user is thus enabled to change his geographical position to a neighboured area if he finds that the probability P R is higher in that area and, therefore, a connection to a network may be established by applying a longer scanning period and, consequently, by consuming less battery power. Moreover, it can be provided that the user is enabled to choose whether he wishes to receive a probability value P R that is averaged for a large area, or rather fine grained values for a set of smaller, adjacent areas.
Advantageously, it may be provided that the calculated probability value P R is transmitted to the mobile terminal and that the scanning period T S is calculated on the part of the mobile terminal on the basis of the received probability value P R . Alternatively, it is possible that the scanning period T S is calculated by the server or by an external application and that the calculated scanning period T S is transmitted to the mobile terminal.
Regarding the transmission of the probability P R estimations and/or scanning period T S calculations from the server to mobile terminals the MIIS (Media Independent Information Service) as defined in the IEEE 802.21 Standard may be employed. To this end, a new Information Element (IE) may be added to the MIIS. There are no further problems on doing that, since the 082.21 protocol reserves certain number of bits with the purpose of allowing vendors and operators to add their proprietary IEs. For example, in this context a new IE called “Networks Knowledge Estimation” could be introduced. The process of how this information is inserted in the frame and sent to the mobile nodes may be just following the normal 802.21 rules.
It is noted once again that the methods as described herein are not exclusive of MIH as defined in the IEEE 802.21 specification. It becomes clear to someone skilled in the art that the method as described above applies to any existing or upcoming protocol with similar mechanisms or functionalities.
There are several ways how to design and further develop the teaching of the present invention in an advantageous way. To this end it is to be referred to the following explanation of preferred embodiments of the invention by way of example, illustrated by the figures. In connection with the explanation of the preferred embodiments of the invention by the aid of the figures, generally preferred embodiments and further developments of the teaching will we explained.
BRIEF DESCRIPTION OF THE DRAWING FIGURES
In the drawings:
FIG. 1 is a schematic view of a typical network architecture illustrating the MIH communication model in general,
FIG. 2 is a schematic illustration of a static network search process according to the state of the art with a long scan period,
FIG. 3 is a schematic illustration of a static network search process according to the state of the art with a short scan period,
FIG. 4 is a schematic illustration giving a comparison of battery consumption and wasted time according to various scanning scenarios, and
FIG. 5 is a flow diagram showing an embodiment of an algorithm to dynamically recalculate the probability P R .
DETAILED DESCRIPTION OF THE INVENTION
FIG. 1 illustrates a network model including MIH services in which the method according to the invention is generally applicable. More particularly, FIG. 1 gives an illustration of the MIH communication reference points in a typical network architecture. The model includes an MIH capable communication node 1 which supports multiple wired and/or wireless access technology options.
The model shown in FIG. 1 includes four exemplary access networks 1 - 4 . The access networks 1 , 2 and 4 are connected to a core network (Operator 1 - 3 Core, respectively), whereas access network 3 is a cellular network which is coupled to a core network that is labelled as Visited/Home Core Network. In this context the terms visited and home indicate the provisioning service provider or enterprise. Any of the illustrated networks can be either a Visited or Home Network depending on the relation of the operator to the provisioner of the communication node 1 . The Operator 1 - 3 Core each might represent a service provider or corporate intranet provider.
Network providers offer MIH services in their access networks (Access Networks 1 - 4 ) to facilitate handover into their networks. Each access technology either advertises its MIH capability or responds to MIH service discovery. Each service provider for the access network allows access to one or more MIH Points of Service (PoS). These PoS may provide some or all of the MIH services as determined during MIH capabilities discovery. The location or node of an MIH PoS is not fixed by the standard. The PoS location may vary based on operator deployment scenario and the technology-specific MIH architecture.
An MIH PoS may reside next to or be co-located with the point of attachment (PoA) in the access network (in this regard Access Networks 1 , 2 , and 4 are typical). Alternatively the PoS may reside deeper inside the access or core network (in this regard Access Network 3 is typical). As shown in FIG. 1 , the MIH entity in the communication node 1 communicates with MIH network entities either by R 1 , R 2 or R 3 over any access network. According to the 802.21 the communication reference points R 1 -R 5 shown in FIG. 1 are defined as follows:
R 1 refers to MIHF (Media Independent Handover Function is a functional implementation of MIH services as defined in the 802.21 specification) procedures between the MIHF on the communication node 1 and the MIH PoS on the Network Entity of its serving PoA.
R 2 refers to MIHF procedures between the MIHF on the communication node 1 and the MIH PoS on the Network Entity of a candidate PoA. Candidate PoAs are PoAs that the communication node 1 is aware of but not currently attached to; it becomes the target PoA if a handover eventually occurs. R 1 and R 2 may encompass communication interfaces over both L 2 and L 3 and above.
R 3 refers to MIHF procedures between the MIHF on the communication node 1 and the MIH PoS on a non-PoA Network Entity. R 3 may encompass communication interfaces over L 3 and above and possibly L 2 transport protocol like Ethernet bridging, MPLS, etc.
R 4 refers to MIHF procedures between an MIH PoS in a Network Entity and an MIH non-PoS instance in another Network Entity. R 5 refers to MIHF procedures between two MIH PoS instances in distinct Network Entities. R 4 and R 5 may encompass communication interfaces over L 3 and above. MIHF content passed over R 1 -R 5 may be related to MIIS (Media Independent Information Service), MIES (Media Independent Event Service), or MICS (Media Independent Command Service).
The interaction of visited and home network could be either for control and management purposes or for data transport purposes. It is also possible that due to roaming or SLA agreements, the home network may allow the communication node 1 to access the public Internet directly through a visited network. As illustrated, two MIH network entities may communicate with each other via R 4 or R 5 reference connections. The MIH capable PoA may also communicate with other MIH network entities via R 3 and R 4 reference points. The MIH capable communication node 1 could have a MIH communication with other PoA in the candidate access networks via R 2 reference points to obtain information services about the candidate network.
With regard to the MIH Information Service (MIIS) the providers offer access to their information server located in a MIH PoS node (upper far left). The operator provides the MIIS to communication nodes so they can obtain pertinent information including but not limited to new roaming lists, costs, provider identification information, provider services, priorities and any other information that would enable to select and utilize services. It is possible for the communication node 1 to be pre-provisioned with MIIS data by its provider. Also possible is for the communication node 1 to obtain MIH information services from any access network of its provider. MIIS could also be available from another overlapping or nearby network, using that network's MIIS point of service. A provisioner's network (depicted here as coupled with Access Network 3 ) may utilize R 3 and R 4 interfaces to access other MIH entities like the provisioner's or visited network's MIH information server.
With regard to the MIH Command Service (MICS) the Information Database (far left, mid-way down) depicts a command service PoS. The communication node's 1 MIHF typically communicates with this server using a layer three transport.
As mentioned above, the 802.21 standard provides, amongst several other features, a mechanism to communicate available networks to a terminal in a given area, and so, the terminal does not need to scan but directly attempt to connect to the known networks in its vicinity.
While MIH goes a long way to spare the terminal certain scans, it is still common to be in a situation where no networks are available, either because they are not previously registered on the MIH Information Service, or because the information is outdated. In these cases, the terminal is reduced to non-MIH functionality, which in the following is called non-MIH operation of MIH-enabled devices. In these situations (or when a terminal is not MIH-enabled at all) the terminal typically has to scan periodically according to the policies implemented in the terminal in order to detect the available networks.
FIG. 2 and FIG. 3 illustrate this situation for the case of a long scanning period (low scan frequency in FIG. 2 ) and a short scanning period (high frequency scans in FIG. 3 ). In both cases the user who moves from point A to point B leaves the coverage area (indicated by the dashed line circle) of network A, and becomes suddenly disconnected. This happens at point C. Due to lacking information on available networks, either because of being not MIH-enabled or because of being MIH-enabled, but in a non-MIH operation mode, the mobile terminal sets on a periodical scan which is indicated by the triangles. The scanning period T S in FIG. 2 has been chosen much longer than the scanning period T S ′ in FIG. 3 , i.e. the time interval between two subsequent scans is longer in the embodiment of FIG. 2 than in the embodiment shown in FIG. 3 .
After entering the coverage area of network B (at point D), the next scan (at point E) detects the network. As can be obtained from FIGS. 2 and 3 , in the case of a long scan period the terminal performs only 5 scans between the disconnection from network A and connection to network B. However, the terminal is not aware of network B, until the next scan after having entered the coverage area of network B occurs. This results in a long interval with no connection, as indicated by the stripy area, in spite of the network being available. In a worse case scenario, the scan period T S could be so long that the user could pass through network B without detecting it, which obviously is not the desired behaviour.
In the case of the shorter scan period T S ′ of FIG. 3 , network B is discovered much earlier after having entered network B, however, at the cost of many more scans. This results in faster battery depletion. Thus, a clear trade-off between battery consumption and connectivity time is to be observed.
Statistically, the expected wasted time (represented by the stripy area in FIG. 2 and FIG. 3 , respectively), defined as the average time until the network is discovered, once it becomes available, is:
E wasted =T S /2,
where T S is the scanning period. The longer the scanning period, the bigger the wasted time, i.e. the time the mobile terminal is not connected although a connection would be available. In the general formula it is assumed that the networks are uniformly randomly distributed
Now the case of MIH is considered, in which Network B is registered in the Information Service. In this case, the terminal already knows the whereabouts of Network B, and does not need to perform any scan. Furthermore, as soon as it enters the area where network B is known to be available, it will immediately connect. This is an optimal solution, according to which a minimum number of scans is realized, resulting in the shortest possible wasted time. However, it is to be considered the stretch with no networks. The terminal knows that MIH doesn't have information of any network being available there, but it has no way of checking. If it is intended to provide connectivity for as long as possible, one will still have to scan.
This results in a hybrid scheme, where the terminal does not scan when near a known network, but performs regular scans when no network is known in the area. In this case, the wasted time is the same as already described above when the network is not known to MIH, and 0 (or non significant) when the network is registered in the MIH information server. This is expressed as:
E wastedMIH =( P R ·0)+[(1− P R )· T S /2]=(1− P R )· T S /2,
wherein P R is the probability that a particular network is registered in the Information Service of MIH or, in other words, the percentage of networks known to MIH. P R is lower or equal to one and, consequently, 1−P R is smaller than 1. Thus, the wasted time with MIH will always be at most the same as without MIH, but for any known network that is registered to the Information Service, the wasted time will become smaller.
FIG. 4 illustrates the wasted time as a function of the scanning period T S . Without MIH, i.e. P R =0, the wasted time increases with a slope of ½ as the scanning period T S increases. In the case where P R is bigger than 0, however, the slope decreases. In other words, with a certain probability value P R bigger than 0 it is possible to reach a wasted time equal to an arbitrary threshold by employing a longer scanning period T S . The arbitrary threshold is indicated by the dashed line.
Furthermore, the plot in FIG. 4 illustrates an estimate of the battery consumption, which is closely linked to the scanning period T S . The more often the scanning is carried out by the terminal (small T S ), the more battery will be used. This effect is illustrated by the dotted line. Given an arbitrary threshold, when P R is bigger than 0, one can achieve significantly lower power consumptions than in the case where P R is 0, or there is no MIH available, respectively. Thus, if the probability P R was known, it would be possible to calculate an optimal scanning period as that which provides the same wasted time as without MIH. By equaling both equations indicated above one obtains:
E wastedMIH =E wasted
(1− P R )· T SMIH /2 =T S /2
T SMIH =T S /(1− P R )=> T SMIH ≧T S
This constitutes a value for the scanning time that depends on the expected threshold, given by T S and P R . Using such a scanning period optimizes the usage of battery and still provides the same level of connectivity as without MIH.
The proposed formula is a simple embodiment on how T S can be calculated in relation to a target performance, provided by the wasted time without MIH. More advanced methods could consider, for instance, to allow the user to configure his scanning more aggressively (and battery consuming) by choosing a shorter scanning period, as a deviation of the optimally calculated period. In normal deployments, where the scanning period T S without MIH might not be available, the period can be calculated using a constant which is empirically adjusted. Moreover, the scanning period T S is specific to the area in which the user is at the moment. Larger or smaller areas could be considered for the purpose of the estimation of P R .
Regarding a possible calculation of the probability values P R , an estimation of how many of the existing networks (in a given area) MIH really knows about is conducted. In this context it is especially advantageous to provide a mechanism that enables users to upload information regarding the networks they really detect in their surrounding area. Using this information, the MIH Information Service can check if it already knows about this network, and, in the case it doesn't, keep the information.
If the Information Service is updated by messages on the part of users in the field reporting on networks, which were not yet known to the Information Service, P R will be increased, thus improving the gain in terms of lower battery consumption of scanning mobile terminals due to reduced scanning periods. By checking how many of the reported networks were already known, and how many were new, the Information Service can produce an estimate of the probability value P R and send it down to the terminals, which then will adjust their scan periods accordingly.
A basic state diagram of the algorithm running at the Information Server to calculate P R in a given area according to an exemplary embodiment is depicted in FIG. 5 .
FIG. 5 just shows a simple example of how P R estimation is dynamically recalculated by the Information Server, based only in the fact of having previous knowledge or not of the network the user is uploading to the server. Additionally, more advanced algorithms can make use of further parameters in order to make the estimation of P R more accurate. For instance, when no new networks are discovered in an area over a long period of time, i.e. the Information Service doesn't receive any reports of not yet known networks, this can be interpreted as a strong hint that no networks exist further to the ones already registered to the Information Server. As a reaction, in such a case the probability value P R can steadily increase towards 1 . The value can be transmitted to a user's terminal, thus enabling the user to adjust his scanning period T S , in the case described by reducing T S in order to save battery power. However, if no user at all reports on available networks in the area for a long period of time, the P R should decay, to represent the lack of freshness of the information.
To further increase the accuracy of the P R estimation, terminal capabilities may be considered in the measurements, so that, for instance, extraordinarily long ranged cell phones do not report networks from distant areas, which would decrease P R although the reported network in fact is not available. In a similar way certain measurements can be conducted before a network is considered as new. By these measurements e.g. moving networks or simple spam is prevented from being reported.
The estimation of P R is specific to each area, wherein the area boundaries are established according to configurable criteria. In particular, the boundaries can be adapted from time to time. For instance, the areas for which a specific probability value is P R estimated may be broadened in case of a low density of user population (with only few user reports to the Information Service during a given time interval). Additionally, the determination of the area will depend on the positioning mechanism provided by MIH. The areas will usually be bigger than the maximum resolution of the positioning system. Furthermore, for a given area P R may be different for each of the different access technologies (Wimax, WiFi, etc. . . . ).
The mobile terminal will use the P R estimation to adapt its scanning period T S . This is, as an example, for a very low P R estimation the scanning period T S will be rather high. In other words, since the mobile node knows that the knowledge of the networks around him is poor, it decides to scan very frequently searching for possible networks to connect to. On the other hand, if the P R estimation is very high, the user will drastically reduce his scanning period T S , as he is already almost completely aware of the situation of available networks in his vicinity. It is to be noted that the sending of the probability value P R from the Information Service to the user terminals might include not only the current area, but also the neighbouring ones. Additionally the particular embodiment can choose whether to send an averaged P R for a large area, or rather transmit more fine grained values for a set of smaller, adjacent areas. In this context it can be provided that users are enabled to specify their individual preferences regarding the area they wish to receive information about from the Information Service.
Until now it has been assumed that the probability P R is calculated by the Information Service and is then (maybe upon a request by a user's terminal, as the case may be) transmitted from the Information Service to the terminals where the scanning period T S is optimized. This implementation is highly individualized as each terminal can calculate its own scanning period thereby taking into consideration not only the probability P R itself, but additional parameters as described above. The drawback, however, is slightly increased energy consumption on the terminal side due to the necessary calculation operation (which is, however, overcompensated by the energy savings due to the optimally adjusted scanning period). In another implementation it is also possible, that the scanning period T S is calculated in the server side and is then transmitted to the terminals.
It is important to highlight that, even though the exemplary embodiment has been explained using MIH, it is to be understood that the invention expands to any mechanism or protocol of similar functionality as MIH, which on the one hand allows for reporting network information to users and, on the other hand, allows users to upload network information based on their own network measurements.
Many modifications and other embodiments of the invention set forth herein will come to mind the one skilled in the art to which the invention pertains having the benefit of the teachings presented in the foregoing description and the associated drawings. Therefore, it is to be understood that the invention is not to be limited to the specific embodiments disclosed and that modifications and other embodiments are intended to be included within the scope of the appended claims. Although specific terms are employed herein, they are used in a generic and descriptive sense only and not for purposes of limitation.
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A method for optimizing the scanning process of a mobile terminal, the scanning process being performed by the mobile terminal in order to discover an available network to which a connection is possible, wherein at least a part of existing networks is registered to a server, wherein the server provides its information regarding the registered networks to the mobile terminal, is characterized in that the scanning period of the mobile terminal is dynamically adjusted on the basis of information provided by the server.
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BACKGROUND OF THE INVENTION
[0001] 1. Field of Technology
[0002] The present invention relates to a light emitting diode (LED) illumination/signal lamp, and, more particularly, to a LED illumination unit which is similar to, even better than, a conventional daylight lamp in fluorescent effect. The present invention further relates to the application of the fluorescence-like LED illumination unit.
[0003] 2. Background
[0004] Compared with conventional illumination lamps, such as, incandescent lamps and daylight lamps, LED illumination lamps are characterized by long service life, high light efficiency, low power consumption, no fluorescent dye contamination, and so on, and are easily replaced. However, for existing LED lamp tubes for illumination, a circuit board and a LED array are disposed in the tube body of the lamp tube, LED illuminants are generally arranged in an axial direction of the tube body, and light emitting centers of the LED illuminants face a tube wall of the tube body. Such LED daylight lamps have problems such as, exposure of spotted light sources, small irradiation angle of the light path, string of bead-like LED spotted light sources forming the daylight lamp, dazzling light rays, significant difference from a light emitting mode of existing daylight lamps, and dizziness caused by multiple overlapping projections formed on the wall or ground by irradiating an irradiated object with multiple light spots. These LED daylight lamps fail to meet people's long-term use experience of conventional daylight lamps, have low comfortability, and thus are not suitable for domestic illumination.
[0005] To make the light emitting mode of the LED illumination lamps be close to that of the existing daylight lamps, many inventors are devoted to the research of the light emitting mode of the LED illumination lamps and produce many patents.
[0006] For example, a typical solution is to dispose two LED illuminants in opposite directions at two ends of an LED lamp tube and dispose a double-sided reflective sheet or light guide material or light reflecting material in the tube body, so that light emitted by the LED illuminants are reflected through the double-sided reflective sheet or the light reflecting material or scattered through the light guide material, so as to approximate the light emitting mode of the existing daylight lamps. Such a typical solution is, for example, an LED daylight lamp disclosed in Chinese Invention Patent Publication No. CN101144591A, an LED daylight lamp disclosed in Chinese Utility Model Patent Granted Publication No. CN200993322Y, or the like. However, such LED daylight lamps use a small number of LED illuminants with low illumination intensity, and thus are difficult to be used for daily illumination.
[0007] Another typical manner is to mix a certain amount of light scattering powder or light guide powder into the raw material of a PC or PV lamp tube uniformly during injection molding of the lamp tube and to form a hollow lamp tube by injection molding, so that light emitted by LED illuminants is transmitted through the PC or PV lamp tube. Such a patent is, for example, a soft LED daylight lamp with multiple light emitting angles disclosed in Chinese Utility Model Patent Granted Publication No. CN201293218Y. However, such an LED daylight lamp still can not solve the problems such as exposure of spotted light sources, large light path loss, and low illumination intensity in LED daylight lamps.
[0008] Still another typical manner is to use LED illuminants with lenses added therein, for example, a high-power LED daylight lamp disclosed in Chinese Utility Model Patent Granted Publication No. CN201330956Y. However, such an LED daylight lamp still can not solve the above relevant problems existing in LED daylight lamps well.
SUMMARY OF THE INVENTION
[0009] To solve the above technical problems existing in LED daylight lamps, the present invention is directed to a LED illumination unit more similar to a conventional fluorescent lamp and illumination lamps manufactured by using the LED illumination unit and suitable for domestic use, which have light color, light emission uniformity, and softness basically not different from those of the existing fluorescent lamps, and meet the long-term using habit and approval of people. According to the definition of light utilization efficiency, since emitted light of an optical model used by the LED illumination unit in the present invention has a certain directivity, the ratio of luminous flux in the illuminated effective area to light source luminous flux is high, so that the lamps have a higher light utilization efficiency than that of the conventional fluorescent lamps. The technical problems to be solved by the present invention may be implemented through the following technical solutions.
[0010] Said technical problems can be resolved by the following solutions:
[0011] A fluorescence-like LED illumination unit is provided, which includes a radiator, an LED substrate fixed on an inner surface of the radiator and extending axially along the radiator, and multiple LED illuminants arranged axially along the radiator and encapsulated on the LED substrate, in which the inner surface of the radiator is in the shape of a paraboloid with reflective effect; a bar-shaped convex lens with radial converging effect is disposed in the space surrounded by the paraboloid with reflective effect on the inner surface of the radiator; the bar-shaped convex lens is located in front of the multiple LED illuminants and extends axially along the radiator; and the bar-shaped convex lens radially converges part of light rays emitted by the multiple LED illuminants but axially diffuses them.
[0012] The bar-shaped convex lens is located near a location in front of the LED illuminants with light converging effect for the LED illuminants.
[0013] The fluorescence-like LED illumination unit of the present invention further includes a light distribution lampshade connected to the radiator and located in front of the bar-shaped convex lens.
[0014] The bar-shaped convex lens is a bar-shaped light converging Fresnel lens.
[0015] The light distribution lampshade of the present invention is a transparent lampshade, or a mist-like soft light lampshade, or a light distribution lampshade having various straight or irregular stripes with light scattering effect distributed on inner and outer surfaces thereof, or any other dedicated light distribution lens so that the fluorescence-like LED illumination unit becomes LED signal lamps with other functions.
[0016] In the present invention, heat dissipation fins are disposed on an outer surface of the radiator to improve a heat dissipation effect.
[0017] In the present invention, multiple mounting posts are disposed in a spaced arrangement axially along the radiator on the inner surface of the radiator, and the bar-shaped light converging convex lens is fixedly mounted on the mounting posts by screws or other means.
[0018] In the present invention, a strip-shaped mounting groove for embedding the LED substrate is disposed on the inner surface of the radiator, the LED substrate is embedded in the strip-shaped mounting groove, and the multiple mounting posts are arranged in the strip-shaped mounting groove.
[0019] The LED illuminants in the present invention may be high-power patch LEDs or conventional low-power in-line LEDs required for corresponding colors according to different lamp functions, or bat-shaped light distribution LEDs, or LED illuminants equipped with other special lenses; the LED illuminants may be single-chip LEDs or multi-chip LEDs.
[0020] The fluorescence-like LED illumination unit of the present invention may be used as an LED daylight lamp, the radiator and the light distribution lampshade of the LED daylight lamp define and form a circular lamp tube, lamp holders are mounted on two ends of the circular lamp tube, the lamp holder has electrodes connected to an external power source, the LED substrate is electrically connected to the electrodes on the lamp holders; slots for mounting the light distribution lampshade are disposed on two sides of the strip-shaped mounting groove, insertion edges are disposed on two axial sides of the light distribution lampshade, and the insertion edges are inserted into the slots from one end of the radiator, so that the light distribution lampshade and the radiator are connected to form the lamp tube.
[0021] The fluorescence-like LED illumination unit in the present invention may be used as a warning lamp light emitting unit, the radiator of the warning lamp light emitting unit is of a plate-like structure, a bar-shaped reflective bowl is disposed on the inner surface of the radiator, an inner surface of the bar-shaped reflective bowl is in the shape of a paraboloid with reflective effect; the light distribution lampshade is of a basket-shaped structure, a pressed edge is arranged on the periphery of the light distribution lampshade, and the pressed edge is pressed and connected on the radiator by a pressing ring; and a sealing strip for sealing a seam between the pressed edge and the radiator is disposed on the pressed edge.
[0022] The fluorescence-like LED illumination unit of the present invention may be used as a beacon lamp (pharos) light emitting unit, the radiator of the beacon lamp light emitting unit is of a plate-like structure, a bar-shaped reflective bowl is disposed on the inner surface of the radiator, an inner surface of the bar-shaped reflective bowl is in the shape of a paraboloid with reflective effect; the light distribution lampshade is of a basket-shaped structure, a pressed edge is arranged on the periphery of the light distribution lampshade, and the pressed edge is pressed on the radiator by a pressing ring; and a sealing strip for sealing a seam between the pressed edge and the radiator is disposed on the pressed edge.
[0023] The beacon lamp light emitting unit may be used for manufacturing a beacon lighthouse lamp, the beacon lighthouse lamp includes a base and a beacon lamp light emitting unit fixing frame fixed on the base, and multiple beacon lamp light emitting units may exist according to requirements of different sight distances, and are fixed on the beacon lamp light emitting unit fixing frame in an annular arrangement with multiple layers.
[0024] The fluorescence-like LED illumination unit of the present invention may be used for manufacturing a car decorative illumination lamp or household ceiling lamp, the car decorative illumination lamp or household ceiling lamp includes a basket-shaped lamp housing, multiple fluorescence-like LED illumination units exist, the multiple fluorescence-like LED illumination units are arranged in the lamp housing, and the light distribution lampshade is mounted at an opening of the lamp housing.
[0025] The fluorescence-like LED illumination unit of the present invention may be used for manufacturing a road lamp light emitting unit, the radiator of the road lamp light emitting unit is of a plate-like structure, the light distribution lampshade is of a basket-shaped structure, a pressed edge is arranged on the periphery of the light distribution lampshade, and the pressed edge is pressed on the radiator by a pressing ring; and a sealing strip for sealing a seam between the pressed edge and the radiator is disposed on the pressed edge.
[0026] With the above technical solutions, through a combination of a bar-shaped convex lens having radial light converging effect but blending greatly diffused light in the axial direction and a paraboloidal reflective mirror together with improvements to a light distribution lampshade, the present invention completely solves the problems such as exposure of spotted light sources, small irradiation angle of a light path, beaded LED light sources forming the illuminant, dazzling light rays, and the like in an existing LED illumination lamp, especially, an LED daylight lamp. The illumination unit emits more uniform and soft light rays, with a higher brightness in an irradiated region and a light emitting mode which is basically not different from that of a conventional daylight lamp, and meets the long-term using habit of people. In addition, the light efficiency of lamps is greatly improved by disposing the bar-shaped convex lens with radial converging effect. Upon preliminary detection, a fluorescence-like LED illumination lamp of 8 W achieves a ground illumination of 120-150 lux when having a vertical distance of 2.5 m from the ground.
[0027] The present invention is further illustrated below with reference to accompanying drawings and specific embodiments in the specification.
BRIEF DESCRIPTION OF THE DRAWINGS
[0028] The present invention will become more fully understood from the detailed description given herein below for illustration only, and thus are not limitative of the present invention, and wherein:
[0029] FIG. 1 is a schematic structural view of an LED daylight lamp in the present invention;
[0030] FIG. 2 is an A-A sectional view of FIG. 1 ;
[0031] FIG. 3 a is a schematic front view of a warning lamp light emitting unit in the present invention;
[0032] FIG. 3 b is an A-A sectional view of FIG. 3 a;
[0033] FIG. 3 c is a B-B sectional view of FIG. 3 a;
[0034] FIG. 4 a is a schematic front view of a beacon lamp light emitting unit in the present invention;
[0035] FIG. 4 b is an A-A sectional view of FIG. 4 a;
[0036] FIG. 4 c is a B-B sectional view of FIG. 4 a;
[0037] FIG. 5 is a schematic view of a large-scale beacon lighthouse lamp manufactured by using the beacon lamp light emitting unit in the present invention;
[0038] FIG. 6 a is a schematic front view of a car decorative illumination lamp or ceiling lamp in the present invention;
[0039] FIG. 6 b is an A-A sectional view of FIG. 6 a;
[0040] FIG. 7 a is a schematic front view of a road lamp light emitting unit in the present invention;
[0041] FIG. 7 b is an A-A sectional view of FIG. 7 a ; and
[0042] FIG. 7 c is a B-B sectional view of FIG. 7 a.
DETAILED DESCRIPTION OF THE INVENTION
[0043] To make the technical means, features, purposes, and effects of the present invention comprehensible, the present invention is further elaborated below with reference to specific embodiments and drawings.
Embodiment 1
[0044] Referring to FIG. 1 , a fluorescence-like LED daylight lamp of the present invention includes a lamp tube formed by an axial radiator 100 , a bar-shaped light converging Fresnel lens 500 , and a light distribution lampshade 200 , in which the radiator 100 is made of an aluminium alloy material. Lamp holders 300 are mounted on two ends of the lamp tube, and the lamp holder 300 has electrodes 310 thereon.
[0045] Referring to FIG. 2 , an inner surface 110 of the radiator 100 is a paraboloid with reflective effect so as to reflect part of light emitted by LED illuminants 410 . A strip-shaped mounting groove 120 for embedding an LED substrate 400 is disposed on the inner surface 110 of the radiator 100 , the LED substrate 400 is mounted in the strip-shaped mounting groove 120 , and a heat conductive adhesive is used on a bonding surface between the LED substrate 400 and the radiator 100 for heat conduction. The LED substrate 400 is electrically connected to the electrodes 310 fixed on the lamp holders 300 and extends axially along the radiator 100 . The LED substrate 400 may be one piece or formed by multiple pieces connected in series.
[0046] Multiple LED illuminants 410 are encapsulated on the LED substrate 400 . The LED illuminants 410 are preferably high-power patch LEDs currently commercially available, and may also be conventional low-power in-line LED illuminants according to different energy configuration requirements of lamps.
[0047] On the inner surface 110 of the radiator 100 , multiple mounting posts 130 may be disposed in a spaced arrangement axially along the radiator 100 in the strip-shaped mounting groove 120 , and the bar-shaped light converging Fresnel lens 500 radially converging light but blending greatly diffused light axially is fixed on the mounting posts 130 by screws or other means. The bar-shaped Fresnel lens 500 radially converging light but blending greatly diffused light axially not only can converge light but also can eliminate obvious light spots, which, together with the light distribution lampshade 200 having mist-like soft light or any other light distribution lampshade 200 having various straight or irregular stripes with light scattering effect distributed on inner and outer surfaces thereof, can completely solve the problems such as exposure of spotted light sources, small irradiation angle of a light path, overlapping projections formed by irradiation with a multi-point light source, dazzling light rays, and the like in the existing LED daylight lamp, and further improve the uniformity and softness of light.
[0048] A slot 141 axially extending along the radiator 100 is respectively opened at end portions of two free ends 140 of the radiator 100 , and insertion edges 210 are disposed on two sides of the light distribution lampshade 200 . The insertion edges 210 are inserted into the slots 141 from one end of the radiator 100 so as to combine the light distribution lampshade 200 with the radiator 100 to form the entire lamp tube of the fluorescence-like LED illumination lamp. The light distribution lampshade 200 of the present invention may also be a milky white lampshade or frosted lampshade with a light diffusing agent added therein. Certainly, the light distribution lampshade 200 of the present invention may also be a transparent diffusion light distribution lampshade with straight stripes. For example, the purpose of the present invention can also be achieved by using a transparent light distribution lampshade with diffusion particles or irregular stripes.
[0049] To improve the heat dissipation effect of the radiator 100 , heat dissipation fins 150 are disposed on the outer surface of the radiator 100 .
Embodiment 2
[0050] Referring to FIG. 3 a to FIG. 3 c , a warning lamp light emitting unit of the present invention is formed by a plate-like radiator 100 a, a bar-shaped light converging Fresnel lens 500 , a LED substrate 400 , and a light distribution lampshade 200 a. The plate-like radiator 100 a is made of an aluminium alloy material. A bar-shaped reflective bowl 160 is mounted in an axial direction of the radiator 100 and on an inner surface 110 a of the plate-like radiator 100 a, and an inner surface of the bar-shaped reflective bowl 160 is a paraboloid 161 with reflective effect. The LED substrate 400 is mounted on the inner surface 110 a of the plate-like radiator 100 a, and a heat conductive adhesive is used on a bonding surface between the LED substrate 400 and the inner surface 110 a of the plate-like radiator 100 a for heat conduction.
[0051] The LED substrate 400 extends axially along the radiator 100 a, and the LED substrate 400 may be one piece or formed by multiple pieces connected in series. Multiple LED illuminants 410 are encapsulated on the LED substrate 400 . The LED illuminants 410 are preferably high-power patch LEDs currently commercially available, and may also be conventional low-power in-line LED illuminants according to different energy configuration requirements of lamps. On the inner surface 110 a of the radiator 100 a, multiple mounting posts 130 are disposed in a spaced arrangement axially along the radiator 100 a, and the bar-shaped light converging Fresnel lens 500 is fixed on the mounting posts 130 by screws. The bar-shaped Fresnel lens 500 radially converging light but blending greatly diffused light axially not only can converge light but also can eliminate obvious light spots, which, together with light distribution lampshades 200 a of different light distribution performance or different colors, for example, the light distribution lampshade 200 a having appropriate arc stripes 230 a arranged thereon, can accurately control the light distribution requirement of a warning lamp in the vertical direction as required, in which the high luminous intensity, large view angle in the horizontal direction, and efficiency of the warning lamp far exceed those of LED warning lamp products of the same kind The light distribution lampshade 200 a is of a basket-shaped structure. A pressed edge 220 a is arranged on the periphery of the light distribution lampshade 200 a, and the pressed edge 220 a is pressed and connected on the radiator 100 a by a pressing ring 600 ; a sealing strip 230 for sealing a seam between the pressed edge 220 a and the radiator 100 a is disposed on the pressed edge 220 a for preventing water from entering the light distribution lampshade 200 a.
[0052] To improve the heat dissipation effect of the radiator 100 a, heat dissipation fins 150 a are disposed on the outer surface of the radiator 100 a.
Embodiment 3
[0053] Referring to FIG. 4 a to FIG. 4 c , a beacon lamp light emitting unit of the present invention is formed by a plate-like radiator 100 b, a bar-shaped light converging Fresnel lens 500 , an LED substrate 400 , and a light distribution lampshade 200 b. The plate-like radiator 100 b is made of an aluminium alloy material. A bar-shaped reflective bowl 160 is mounted in an axial direction of the radiator 100 b and on an inner surface 110 b of the plate-like radiator 100 b, and an inner surface of the bar-shaped reflective bowl 160 is a paraboloid 161 with reflective effect. The LED substrate 400 is mounted on the inner surface 110 b of the plate-like radiator 100 b, and a heat conductive adhesive is used on a bonding surface between the LED substrate 400 and the inner surface 110 b of the plate-like radiator 100 b for heat conduction.
[0054] The LED substrate 400 extends axially along the radiator 100 b, and the LED substrate 400 may be one piece or formed by multiple pieces connected in series. Multiple LED illuminants 410 are encapsulated on the LED substrate 400 . The LED illuminants 410 are preferably high-power patch LEDs currently commercially available, and may also be conventional low-power in-line (direct insertion) LED illuminants according to different energy configuration requirements of lamps. On the inner surface 110 b of the radiator 100 b, multiple mounting posts 130 are disposed in a spaced arrangement axially along the radiator 100 b, and the bar-shaped light converging Fresnel lens 500 is fixed on the mounting posts 130 by screws. The bar-shaped Fresnel lens 500 radially converging light but blending greatly diffused light axially not only enables a beacon lamp designed in this way to have a small divergence angle in the vertical direction and have high light converging efficiency, but also can increase annular blending of lamplight to improve light emission uniformity of the beacon lamp in the horizontal direction in a ring of 360°, in which the effective view angle, light intensity index, and photoelectric efficiency of the lamp far exceed those of LED beacon lamp products of the same kind The light distribution lampshade 200 b is a planar light transmitting lampshade of a basket-shaped structure. A pressed edge 220 b is arranged on the periphery of the light distribution lampshade 200 b, and the pressed edge 220 b is pressed on the radiator 100 b by a pressing ring 600 ; a sealing strip 230 for sealing a seam between the pressed edge 220 b and the radiator 100 b is disposed on the pressed edge 220 b for preventing water from entering the light distribution lampshade 200 b.
[0055] To improve the heat dissipation effect of the radiator 100 b, heat dissipation fins 150 b are disposed on an outer surface of the radiator 100 b.
Embodiment 4
[0056] Referring to FIG. 5 , a large-scale beacon lighthouse lamp with high light intensity shown in FIG. 5 is manufactured by using the beacon lamp light emitting unit shown in FIG. 4 a to FIG. 4 c , and has a luminous intensity meeting the requirement of far sight distance of 16-20 sea miles and a luminous efficiency greater than 50 cd/w, thus filling up a gap of LED beacon lamp products of the same kind The large-scale beacon lighthouse lamp with high light intensity includes a base 700 and a beacon lamp light emitting unit fixing frame 710 fixed on the base 700 . Multiple beacon lamp light emitting units 720 may exist according to requirements of different sight distances, and be fixed on the beacon lamp light emitting unit fixing frame 710 in an annular arrangement with multiple layers in the vertical direction.
Embodiment 5
[0057] Referring to a car decorative illumination lamp or household ceiling lamp shown in FIG. 6 a to FIG. 6 b , the car decorative illumination lamp or household ceiling lamp includes a basket-shaped lamp housing 800 , multiple fluorescence-like LED illumination units 810 exist, the multiple fluorescence-like LED illumination units 810 are arranged in the lamp housing 800 , and a light distribution lampshade 200 c is mounted at an opening of the lamp housing 800 .
[0058] The fluorescence-like LED illumination unit 810 is formed by a plate-like radiator 100 c, a bar-shaped light converging Fresnel lens 500 , and an LED substrate 400 . The plate-like radiator 100 c is made of an aluminium alloy material. A bar-shaped reflective bowl 160 is mounted on an inner surface 110 c of the plate-like radiator 100 c and in an axial direction of the plate-like radiator 100 c, and an inner surface of the bar-shaped reflective bowl 160 is a paraboloid 161 with reflective effect. The LED substrate 400 is mounted on the inner surface 110 c of the plate-like radiator 100 c, and a heat conductive adhesive is used on a bonding surface between the LED substrate 400 and the inner surface 110 c of the plate-like radiator 100 c for heat conduction.
[0059] The LED substrate 400 extends axially along the radiator 100 c, and the LED substrate 400 may be one piece or formed by multiple pieces connected in series. Multiple LED illuminants 410 are encapsulated on the LED substrate 400 . The LED illuminants 410 are preferably high-power patch LEDs currently commercially available, and may also be conventional low-power in-line LED illuminants according to different energy configuration requirements of lamps. On the inner surface 110 c of the radiator 100 c, multiple mounting posts 130 are disposed in a spaced arrangement axially along the radiator 100 c, and the bar-shaped light converging Fresnel lens 500 is fixed on the mounting posts 130 by screws. The bar-shaped Fresnel lens 500 radially converging light but blending greatly diffused light axially not only can converge light but also can eliminate obvious light spots, which, together with light distribution lampshades 200 c of different light distribution performance, completely solves the problems such as exposure of spotted light sources, overlapping projections formed by irradiation with a multi-point light source, dazzling light rays, and the like in the existing LED car decorative illumination lamp or ceiling lamp, and achieves luminous intensity, view angle, and efficiency far exceeding those of LED car decorative illumination lamps or ceiling lamps of the same kind
[0060] To improve the heat dissipation effect of the radiator 100 c, the radiator 100 c may also be designed as the lamp housing 800 , and a heat conductive adhesive is used directly between the inner surface of the radiator 100 c and the LED substrate 400 for heat conduction.
Embodiment 6
[0061] Referring to FIG. 7 a to FIG. 7 c , a road lamp light emitting unit of the present invention is formed by a plate-like radiator 100 d, a bar-shaped light converging Fresnel lens 500 , an LED substrate 400 , and a light distribution lampshade 200 d. The plate-like radiator 100 d is made of an aluminium alloy material. A bar-shaped reflective bowl 160 is mounted on an inner surface 110 d of the plate-like radiator 100 d and in an axial direction of the plate-like radiator 100 d, and an inner surface of the bar-shaped reflective bowl 160 is a paraboloid 161 with reflective effect. The LED substrate 400 is mounted on the inner surface 110 d of the plate-like radiator 100 d, and a heat conductive adhesive is used on a bonding surface between the LED substrate 400 and the inner surface 110 d of the plate-like radiator 100 d for heat conduction.
[0062] The LED substrate 400 extends axially along the radiator 100 d, and the LED substrate 400 may be one piece or formed by multiple pieces connected in series. Multiple LED illuminants 410 are encapsulated on the LED substrate 400 . The LED illuminants 410 are bat-shaped light source LEDs or LED illuminants encapsulated by bat-shaped optical LED lenses. On the inner surface 110 d of the radiator 100 d, multiple mounting posts 130 are disposed in a spaced arrangement axially along the radiator 100 d, and the bar-shaped light converging Fresnel lens 500 is fixed on the mounting posts 130 by screws. The bar-shaped Fresnel lens 500 radially converging light but blending greatly diffused light axially not only can converge light but also can eliminate obvious light spots, which, together with light distribution lampshades 200 d of different light distribution performance, for example, the light distribution lampshade 200 d having no stripes or having fine stripes thereon, completely solves the problems such as exposure of spotted light sources, overlapping projections formed on the ground by irradiation with a multi-point light source, dazzling light rays, and the like in some existing LED road lamp illuminants, and achieves luminous intensity and light utilization efficiency far exceeding those of LED road lamp products of the same kind The light distribution lampshade 200 d is of a basket-shaped structure. A pressed edge 220 d is arranged on the periphery of the light distribution lampshade 200 d, and the pressed edge 220 d is pressed on the radiator 100 d by a pressing ring 600 ; a sealing strip 230 for sealing a seam between the pressed edge 220 d and the radiator 100 d is disposed on the pressed edge 220 d for preventing water from entering the light distribution lampshade 200 d.
[0063] To improve the heat dissipation effect of the radiator 100 d, heat dissipation fins 150 d are disposed on an outer surface of the radiator 100 d. Certainly, the radiator 100 d may also be designed as a lamp housing of the road lamp, and a heat conductive adhesive is used directly between the inner surface of the radiator 100 d and the LED substrate 400 for heat conduction.
[0064] The above embodiments show and describe the basic principle, main features, and advantages of the present invention. Persons skilled in the art should understand that, the present invention is not limited to the above embodiments, the above embodiments and the specification merely describe the principle of the present invention, and the present invention can further be applied in the field of LED lamps of other functions without departing from the spirit and scope of the present invention. The variations and improvements all fall into the scope of the present invention for which protection is sought. The scope for which protection is sought by the present invention is defined by the claims and equivalents thereof.
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A fluorescence-like light emitting diode (LED) illumination unit is provided, which includes a radiator, an LED substrate fixed on the radiator, and multiple LED illuminants encapsulated on the LED substrate. A first surface of the radiator is in the shape of a paraboloid with reflective effect. A bar-shaped convex lens with radial converging effect is disposed in the space surrounded by the paraboloid. The bar-shaped convex lens is located in front of the multiple LED illuminants and radially converges part of light rays emitted by the multiple LED illuminants but axially diffuses them. The illumination unit completely solves the problems such as exposure of spotted light sources, small irradiation angle of a light path, beaded light spots of the LED light sources as the lamp illuminant, visual dizziness caused by multiple projections formed by irradiating an irradiated object with a multi-point light source, dazzling light rays, and the like in an existing LED illumination lamp. The illumination unit emits more uniform and soft light rays, with a higher brightness in an irradiated region and a light emitting mode which is basically not different from that of a conventional daylight lamp, and meets the long-term using habit and approval of people. Various applications of the fluorescence-like LED illumination unit are further provided.
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CROSS REFERENCE TO RELATED APPLICATIONS
This application is a national stage filing under section 371 of International Application No. PCT/GB2007/050052, filed on Feb. 7, 2007, and published in English on Aug. 16, 2007 as WO 2007/091104 and claims priority of Great Britain application No. 0602679.3 filed on Feb. 10, 2006, the entire disclosure of these applications being hereby incorporated herein by reference.
TECHNICAL FIELD
The present invention relates to improvements in or relating to walls, in particular to illuminated transparent or translucent walls.
BACKGROUND OF THE INVENTION
A “wall” in this context is taken to mean a wall of a building or similar fixed construction, either internal or external. The term also encompasses internal partitions for a building, which may extend only part way between the floor and ceiling of a room in a building.
There are a number of different construction materials available for the formation of a building's walls. One material, which can be chosen, is glass. Its light transmission properties can create a spacious light and airy aspect within a building.
Because of the transparency of glass, it is known to provide illumination to further improve the appearance of a building or to increase its visibility. However, this requires the installation of separate illumination apparatus, which must be separately installed and powered and arranged close to the wall.
BRIEF SUMMARY OF INVENTION
According to a first aspect of the present invention there is provided a transparent or translucent wall comprising internal illumination means.
According to a second aspect of the invention there is provided a transparent or translucent wall component that comprises illumination means.
Preferably, the wall is formed from a glass or plastic material.
Preferably, the wall comprises a plurality of nested channel members.
Preferably, the illumination means is provided at a side flange of at least one channel member.
Preferably, the illumination means comprises an electroluminescent strip.
Preferably, the electroluminescent strip is adhesively bonded to the channel flange.
Preferably, the electroluminescent strip has a split electrode structure.
Alternatively, the electroluminescent strip has a parallel electrode structure.
Preferably, the illumination means comprises one or more light emitting diodes (LED's).
Preferably, a DC-AC inverter is provided to power the illumination means.
Preferably, the wall comprises an upper housing member and a lower housing member for receiving the channel members.
Preferably, the upper and/or lower housing members comprises power connection means for the illumination means.
Preferably, a frame member is provided for housing the upper and lower housing members and the wall structure.
According to a third aspect of the invention there is provided a building comprising a wall structure according to the first aspect.
BRIEF DESCRIPTION OF THE DRAWING FIGURES
The present invention will now be described, by way of example only, with reference to the accompanying drawings, in which:
FIG. 1 shows an exploded view of a wall according to the first embodiment of the invention;
FIG. 2 shows an exploded view of how the wall of FIG. 1 is assembled to include the illumination mean; and
FIG. 3 shows the arrangement of the first embodiment; and
FIG. 4 shows an orthographic view of the wall in FIG. 1 containing a sectional view showing the means of illumination.
DETAILED DESCRIPTION
One particular type of currently available profiled glass wall system is the U channel glass wall system. Within this system, translucent cast glass U channels are fitted into an extruded metal perimeter frame and are fixed in place by the use of a silicone sealant.
The channels can be installed either vertically or horizontally and are supplied in a variety of colours and textures with varying translucency. The system can be single glazed or dual glazed, and can be used to form walls of any chosen profile or curvature.
In the first embodiment of the present invention a wall structure comprises a plurality of interlocking channel members and an electroluminescent strip is provided along the edges of the channels. FIG. 1 shows a specific implementation of this embodiment with a profiled glass wall system, specifically, the U-channel system previously identified. A number of panels ( 5 ) are enclosed within the frame ( 1 ).
An exploded view is shown in FIG. 2 . The glass wall system comprises a plurality of panels ( 5 ), which are formed in a nested channel formation, and an electroluminescent strip ( 6 ) is provided at the sides of the channels. The pieces ( 5 ) are held between a lower plastic insert ( 7 ) and a top plastic insert ( 2 ) which comprises holes for housing the power connectors ( 3 ) for the electroluminescent strip ( 6 ). A packing material ( 8 ) and frame ( 1 ) completes the system.
As seen in FIG. 2 , a plurality of outward facing channels (with flanges pointing into the page) are placed side-by-side, with a plurality of inward facing channels (with flanges pointing out of the page) providing a nested interlock.
FIG. 3 shows the incorporation of the electroluminescent strips ( 6 ) on the channels ( 5 ). An outward facing channel ( 5 a ) has an electroluminescent strip ( 6 ) adhesively bonded to the inner edge of its right hand flange, while the inward facing channel ( 5 b ) has an electroluminescent strip ( 6 ) adhesively bonded to the inner edge of its left hand flange. Thus, the space enclosed by the two interlocked channels ( 5 ) is directly illuminated by the electroluminescent strips ( 6 ).
Female power connectors ( 3 ) are provided on a flange of the top plastic insert ( 2 ) for connection with the male power connectors ( 4 ) at the top of each electroluminescent strip ( 6 ).
In one embodiment a single strip is provided which has connectors in another embodiment each vertical channel has a connector provided at the top of each strip ( 6 ) provided thereon. A wiring loom (not shown) is provided which runs through the frame ( 1 ), for providing power to the electroluminescent strip ( 6 ) by means of an Inverter (not Shown).
The scope of the invention is not limited to any particular type of illumination. However, the use of an electroluminescent strip is advantageous. An incandescent lamp or a tungsten lamp has a very low energy efficiency—approximately 85% of the energy is given off as heat, and they also have a short lifetime—approximately 1000 hours. Halogen bulbs are an improvement but still provide relatively high heat losses and have a relatively short lifetime.
Fluorescent lamps are 4 to 5 times more efficient than tungsten lamps and have an improved lifetime of up to 10,000 hours. However, for the current application the required area of the electrodes combined with the transformer used to run the lamps is excessively large does not make them an attractive option, and there are also environmental issues to do with safe disposal of the mercury used in the lamps.
Light emitting diodes (LED's) have a long lifetime and low power requirement, but because they act as point sources of light, generating a specific light pattern that is not always desirable.
An electroluminescent light, also known as a light emitting capacitor (LEC) produces light when phosphor crystals are excited by being exposed to an AC electric current. Electroluminescent panels and strips can be found as back lighting for LCD's in pagers, cell phones, watches and control panels as well as strip lighting for egress decor architecture, broadcast sets and others.
Because no filament is included, the strips have a very long life, are flexible, cool to the touch and highly visible in darkness, smoke and fog etc. The strips also have a very low energy consumption, contain few hazardous materials and require no maintenance.
Electroluminescent film is powered either by parallel electrodes or split electrodes. An electroluminescent lamp comprises a phosphor layer interposed between a clear conductive ITO layer and a rear electrode. In a parallel plate electroluminescent lamp, voltage is applied between the top ITO layer and the rear electrode whereas in a split electroluminescent lamp, a split is made in the rear electrode and a voltage is applied across the two created sides of the electrode.
A power inverter is provided to convert DC power or direct current to standard AC power or alternating current. A compensating inverter can maximise a lamp life by maintaining a variable output as the lamp goes through the normal ageing process.
Other power sources can also be used with a limiting resistor to step down the power of a transformer to step it up as in the case of using a low power amplifier.
Electroluminescent film comes in ten basic colours but some colours will vary depending on the frequency used to power them. Another method of colouring the lamps are by the use of gels, these are simply coloured plastic films. Different colours can be spliced together with wire cutters.
Since in the present embodiment the film runs on a parallel circuit it only needs to be properly terminated when trimmed. This can be accomplished by using super glue, epoxy or other types of sealers to protect the film from moisture. After a period of time the electroluminescent film will become dimmer. This happens more quickly when powered by a higher voltage and or frequency.
The wall structure of the present invention can incorporate other features of known glass walls to give specific optical characteristics such as a different opacities for different light transmission level or different diffuseness of light, acoustic properties giving sound insulation up to appropriate levels or thermal insulation for example giving double glazing or having special coatings on the glass, such as hard pyrolytic surface coatings. The pyrolytic coating creates a very slight coat sheen coat to the glass but does not affect the intrinsic colour of the glass channels. Also, specialised glass types with a solar control coating to reduce the amount of solar energy transmitted through the glazing can be provided.
Connections to the electroluminescent lamp can be flexible printed circuits solderable metal strip, contact pads, solder pads, or other customised designs according to a customer's individual requirements.
The inverter can also be linked to a control means to provide special animation effects for the light—cycling the colour, pattern and timing of various strips.
The glass panels can be used for a number of different installation techniques such as vertical and horizontal glazing (single or double) curved glazing, glass corners, wind tankers, horizontal glazing, roof glazing and window casements.
Due to its flat profile, the electroluminescent film can be incorporated into existing profiled glass systems without interfering with the existing structure. All that is required is a slight modification to the upper plastic inserts to incorporate wiring connectors for a wiring loom; the addition of protection grommets attached to the aluminium frame to protect the power cable; and a mounting frame for the inverter.
Thus the present invention provides for the creation of distinctive light effects which can be enhanced by using sand blasted glass giving a near constant wash of light across the glass systems' compartments. It is also possible to use a clear glass structure to highlight the internal structure.
The invention is not limited to the described embodiment. The limitations of the invention are set out in the attached claims. Various improvements and embodiments can be made to the above without the parting from the scope of the invention.
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A glass or plastic wall structure with nested channel members is provided with electroluminescent strips running along the channel flanges to provide an internal illumination. In particular, it relates to illuminated transparent walls or internal partitions of a building or similar fixed construction.
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FEDERALLY SPONSORED RESEARCH
Not Applicable.
SEQUENCE LISTING OR PROGRAM
Not Applicable.
1. Background—Field of Invention
My invention relates to digital halftone compression and decompression, specifically to delineating variable-length runs using a “none-of-the-above” method
2. Background—Description of Prior Art
Digital halftone files have proven to be quite diffcult to compress. Within the monochrome bitmap, each picture element, or pixel, is designated one of two “colors,” usually black or white. Due to the complexity of the image to be reproduced, the probability of any individual pixel being one color or the other is 50-50. This unpredictability affects the production of “runs.” large groups of pixels of the same “color.” Common compression methods based on run-length encoding prove inefficient, occasionally yielding “compressed” files even larger than the original input file.
Presently the digital halftone industry works around this problem by waiting until the last minute to create the monochrome bitmap. Complex image files utilizing a number of different file formats are compressed, stored or transmitted, and decompressed prior to being “rasterized” into a digital halftone file at the final output stage, the digital printer or monitor display.
OBJECT AND ADVANTAGES
Several objects and advantages of the present invention are:
(a.) to encode and compress a monochrome bitmap into a smaller binary file that my be efficiently stored or transmitted.
(b.) to decode and decompress this smaller binary file into a reproduction of the original monochrome bitmap that then may be displayed on a digital computer monitor or printer.
(c.) to store and transmit as a single file complex documents previously consisting of two or more different file formats.
(d.) to accomplish the above efficiently by means of a digital computer.
SUMMARY
According to the present invention, a digital halftone efficiently is compressed for storage or transmission, and then efficiently decompressed for display on a digital computer monitor or printer.
DRAWINGS
Drawing Figures
FIG. 1 shows a flow chart of the method of the invention as performed by a binary computing device.
FIG. 2 shows a method of reducing the patterns of two-pixel-by-two-pixel monochrome digital halftone cells.
FIG. 3 shows a method of parsing the revised input bitmap.
FIG. 4A shows an input bitmap in which the patterns of the two-pixel-by-two-pixel cells have been reduced.
FIG. 4B shows the input bitmap of 4 A parsed into smaller bitmaps that have been recombined.
FIG. 5 shows a compressed bitmap created by converting the parsed input bitmap of 4 B utilizing the preferred embodiment of the method of the invention.
FIG. 6 shows a compressed bitmap created by converting the parsed input bitmap of 4 B utilizing an alternative embodiment of the method of the invention.
DETAILED DESCRIPTION
Description—FIG. 1 —Flow Chart
A Monochrome Input Bitmap contains an input image's pixels displayed at a binary depth of one bit. Each pixel is described by either a 0 or a 1 to designate one of two “colors,” normally black or white. This bitmap is of certain dimensions in pixels high and wide, and a number of equal-sized multi-pixel halftone cells are contained wholly within.
A Revised Input Bitmap is derived by slightly rearranging the black and white pixels in each of the Monochrome Input Bitmap's contained two-pixel-by-two-pixel halftone cells to reduce the number of possible patterns. This pattern reduction maintains the ratio of black pixels to white pixels, or gray level, within the cell.
A Parsed Input Bitmap is derived by dividing the pixels within each contained two-pixel-by-two-pixel halftone cell into two or more separate bitmaps that maintain the spatial relationship of each pixel to similarly positioned pixels within the. cell. These separate bitmaps then are combined into a global bitmap containing the same number of pixels as its predecessor and the same ratio of black pixels to white pixels, or global gray level.
A “none or the above” or NOTA Coder then acts on this Parse Input Bitmap to yield a binary file that is smaller than that used to describe the preceding bitmaps.
Following retrieval of this file, a NOTA Decoder then acts to reverse the coding process and yield an exact duplicate of the Parsed Input Bitmap, now redesignated a Parsed Output Bitmap. This bitmap contains the same number of pixels and the same ratio of black pixels to white pixels as the Revised Input Bitmap but not in the same order.
A Revised Output Bitmap is derived by reversing the previous parsing method to yield a bitmap that is an exact duplicate of the Revised Input Bitmap, including the same number of global pixels and the same ratio of black pixels to white pixels within each two-by-two-pixel cell. This bitmap then is sent to a binary computer's Monitor or Printer Display.
FIGS. 2 - 5 —Preferred Embodiment
FIG. 2 shows sixteen possible patterns for each two-pixel-by-two-pixel halftone cell in columns 1 & 3 . Seven allowed patterns of the preferred embodiment of the present invention are shown in column 2 as a result of a reduction method.
FIG. 3 shows a four-pixel-by-four-pixel section of a larger image in the center of the drawing. The four two-pixel-by-two-pixel halftone cells within are parsed into the four smaller bitmap sections on either side.
FIG. 4A shows a section of a Monochrome Input Bitmap that has had its two-pixel-by-two-pixel cell patterns reduced. This Revised Input Bitmap is 512 pixels of dimensions 16 pixels wide and 32 pixels high. This Revised Input Bitmap is identical to a derived Revised Output Bitmap (FIG. 1 ).
FIG. 4B shows this Revised Input Bitmap ( FIG. 4A ) parsed into four smaller bitmaps that have been combined to derive a Parsed Input Bitmap. This bitmap is 512 pixels of dimensions 8 pixels wide and 64 pixels high. For the purpose of illustration, the image has been halved and the upper half shown on the left, the lower half shown on the right. This Parsed Input Bitmap is identical to a derived Parsed Output Bitmap (FIG. 1 ).
FIG. 5 shows a Compressed File derived from the Parsed Input Bitmap ( 4 B) following processing by the NOTA Coder utilizing a Fibonacci sequence to encode run length. It is a binary file of 387 bits expressed as a bitmap of 387 pixels, shown 16 pixels wide for comparison with the Revised Input Bitmap (FIG. 4 A).
Alternative Embodiment
FIG. 6 shows a Compressed File derived from the Parsed Input Bitmap ( 4 B) following processing by the NOTA Coder utilizing an alternative sequence to determine run length. It is a binary file of 392 bits expressed as a bitmap of 392 pixels, shown 16 pixels wide for comparison with the Revised Input Bitmap (FIG. 4 A). In this embodiment, a series based on an 8-bit byte is utilized ( 1 , 2 , 5 , 8 . 16 , 24 . . . )
Advantages
From the description above, a number of advantages of my none-of-the-above digital halftone compression and decompression become evident.
(a) The actual size of the resultant encoded and compressed binary file is smaller than the size of the original monochrome bitmap file upon which it is based.
(b) Due to this reduction in size, the resultant file may be stored and transmitted more efficiently than the original file by using a binary computer.
(c) Unencoding and decompressing the resultant file provides a faithful reproduction of the revised input monochrome bitmap file.
(d) The none-of-the-above encoding and decoding method efficiently uses fewer resources of the binary computer system.
Operation
The subject of the operation of the current invention is an image expressed as a Monochrome Input Bitmap (FIG. 1 ). This bitmap is of specified dimensions expressed in pixels wide and high. These dimensions wholly accommodate a number of equal-sized multi-pixel halftone cells completely within. Each pixel within this bitmap is one of two “colors,” normally white or black, and may be designated by a single binomial, 1 or 0.
The smallest square digital halftone cell capable of depicting shades of gray measures two-pixels-by-two-pixels. While said cell may convey five shades, all pixels black plus the incremental addition of four white pixels, the number of possible patterns within the cell numbers sixteen. A method of the present invention is to reduce the number of allowed patterns within the two-pixel-by-two-pixel cells.
Operation—Pattern Reduction
In FIG. 2 , the sixteen possible patterns within a two-pixel-by-two-pixel cell are shown in the first and third columns. The reduction method's seven patterns are shown in the second column. The pattern of four pixels white (column 1 , row 1 ) does not change (column 2 , row 1 ). The pattern for four pixels black (column 3 , row 8 ) also does not change (column 2 , row 7 ). The six possible patterns for two pixels white and two pixels black shown in column 1 , rows 6 - 8 & column 3 , rows 1 - 3 , all are assigned to one allowed checkerboard pattern (column 2 , row 4 ).
The four possible patterns for three pixels white, one pixel black (column 1 , rows 2 - 5 ), are assigned to two allowed patterns (column 2 , rows 2 & 3 ) by shifting the single black pixel horizontally as necessary to partially maintain the checkerboard pattern. The four possible patterns for one pixel white, three pixels black (column 3 rows 4 - 7 ), similarly are assigned to two allowed patterns (column 2 , rows 5 & 6 ) by shifting the single white pixel horizontally as necessary to partially maintain the checkerboard pattern (Note that the derived four patterns also may be created by moving the required pixels vertically and that the checkerboard pattern also may be the inverse.)
Once all the two-pixel-by-two-pixel cells similarly are processed, the Revised Input Bitmap ( FIG. 1 ) is the same dimensions in pixels high and wide as its predecessor and the total number of black pixels and the total number of white pixels remains the same globally. FIG. 4A shows such a Revised Input Bitmap of dimensions 16 pixels wide by 32 pixels high with only seven patterns allowed for each two-pixel-by-two-pixel cell. A method of the present invention is to parse this bitmap to achieve longer runs of all black or all white.
Operation—Parsing
This revised bitmap now is processed to yield several smaller bitmaps which are recombined into a Pared Input Bitmap ( FIG. 1. ) Within each two-pixel-by-two-pixel cell, each of the four monochrome pixels is reassigned to one of four smaller bitmaps of specific dimensions half of the pixels wide and half of the pixels high of the preceding bitmap. Globally, all of the two-pixel-by-two-pixel cells' upper left pixels are grouped, all of the cells' lower right pixels are grouped, all of the cells' upper right pixels are grouped, and all of the cells' lower right pixels are grouped.
FIG. 3 shows a method of transferring the pixels of each two-pixel-by-two-pixel cell of the input bitmap into one of four parsed bitmaps which are then combined to create the Parsed Input Bitmap. Four two-pixel-by-two-pixel cells of the Revised Input Bitmap are shown in the center of FIG. 3 . In each cell, the upper left pixel is transferred to the smaller bitmap in the upper left of FIG. 3 , maintaining its relative position to similarly positioned pixels in adjoining cells. The lower right pixel of each cell similarly is transferred to the smaller bitmap in the lower left of FIG. 3 . The upper right pixel of each cell and the lower left pixel of each cell similarly is transferred to the smaller bitmaps in the upper right and lower left, respectively, of FIG. 3 . Note that the checkerboard pattern depicted will yield two all black bitmaps and two all white bitmaps.
The four parsed files now are arranged sequentially in a file that may be visualized as a bitmap of dimensions half the number of pixels wide and twice the number of pixels high as the original input bitmap. Again, the global relationship of white to black pixels remains constant. FIG. 4B depicts such a Parsed Input Bitmap of dimensions 8 pixels wide by 64 pixels high derived from the Revised Input Bitmap in FIG. 4A Note that for positioning on the page, the image has been halved with the upper half (of dimensions 8 pixels wide by 32 pixels high) on the left and the lower half (of dimensions 8 pixels wide by 32 pixels high) on the right. A method of the present invention is to encode this bitmap to create a compressed file.
Operation—Encoding
This Parsed Input Bitmap ( FIG. 1 ) then is processed by a “none-of-the-above” or NOTA method designated as NOTA Coder (FIG. 1 ). In this method, variable length binomials representing runs of all of one “color” are triggered sequentially by one of the immediately preceding binomial's permutations. Similar to the use of “none of the above” as an answer to a multiple choice question, said permutation instead of designating a run length indicates that the actual run-length is not among those possible within that particular binomial, but is among those possible within a subsequent binomial.
Observing the first run's color and length in FIG. 4B , note that it is black and four pixels long. (From this point forward it is assumed that the next successive run is the opposite color or white, and that each of the following successive runs will alternate in color.)
The smallest possible run is one pixel long. The smallest possible binomial that may depict such a run is one bit in length. Said one bit may depict two states, designated by one or zero. In this method, one of the states is the “none-of-the-above” designation which means that the current binomial does not contain the actual run-length and the next successive binomial must be examined. The second state is the actual run length which acts as a signal to start over again with the smallest possible binomial.
The size of the variable length binomials triggered by the NOTA state may be designated by any consecutive series of numbers. The preferred embodiment utilized in FIG. 5 is the well-known Fibonacci order in which the next successive number in the series is created by summing the previous two numbers in the series. Beginning with a nominal 0 and the first actual number of the series as a 1 , the second series number is 1 , the third 2 , the fourth 3 , the fifth 5 , the sixth 8 , and so on.
Operation—Coding a Run
Taking the first black run of four pixels in FIG. 4B , a variable-length binomial is created that contains it. The run is greater than the run of 1 pixel that may be contained in the first Fibonacci-length binomial of 1 bit. Thus the first position of the variable length binomial is designated 0 which means “none of the above contained runs (1 pixel), go on to the next binomial in the series”. The run of four also is greater than the run of 2 pixels that may be contained in the second Fibonacci-length binomial of 1 bit. Thus the second position of the variable length binomial is designated 0 which means “none of the above contained runs (2 pixels), go on to the next binomial in the series.”
Now, however, the run of four is contained in the third Fibonacci-length binomial of 2 bits. Thus the third and fourth positions of the variable length binomial are designated 10 (containing a 1 ), which means “the second of the contained runs (3, 4, or 5 pixels), start over.” The run of four is thus designated by a four place binomial: 0010. A Compressed File equal in pixel width to the Revised Input Bitmap in FIG. 4A (16 pixels) is shown in FIG. 5 as a bitmap in which a bit designated 0 is white and a bit designated 1 is black. The first four places in said file being 0010 are displayed as white-white-black-white,
Operation—Coding the Following Runs
Taking the next white run of one pixel in FIG. 4B , a variable length binomial is created which contains it. The run of one is contained in the first Fibonacci-length binomial of 1 bit. Thus the first position of the variable length binomial is designated 1 which means “the contained run ( 1 ), start over.” The run of one is thus designated by the single place binomial of 1. In FIG. 5 , the next place (after the first 4-place binomial) being 1 is displayed as black.
Taking the next black run of 31 pixels in FIG. 4B , a variable length binomial is created which contains it. The run of 31 is greater than the run of 1 pixel that may be contained in the first Fibonacci-length binomial of 1 bit. Thus the first position of the variable length binomial is designated 0 which means “none of the above contained runs (1 pixel), go on to the next binomial in the series.” The run of 31 also is greater than the run of 2 pixels that may be contained in the second Fibonacci-length binomial of 1 bit. Thus the second position of the variable length binomial is designated 0 which means “none of the above contained runs (2 pixels), go on to the next binomial in the series.”
The run of 31 is greater than the runs of 3-5 pixels that may be contained in the next Fibonacci-length binomial of 2 bits. Thus the third and fourth positions of the variable length binomial are both designated 0 which means “none of the above contained runs (3-5 pixels), go on to the next binomial in the series.” The run of 31 also is greater than the runs of 6-12 pixels that may be contained in the next Fibonacci-length binomial of 3 bits. Thus the fifth, sixth and seventh positions of the variable length binomial are each designated 0 which means “none of the above contained runs (14 12 pixels), go on to the next binomial in the series.”
The run of 31 , however, is contained in the next Fibonacci-length binomial of 5 bits. Thus the ninth through thirteenth positions of the variable length binomial are designated 10011 (containing a 1) which means “one of the contained runs (31 pixels), start over.” The run of 31 thus is designated by a 12 place binomial: 0000 0001 0011. In FIG. 5 the next 12 places (after the first 4-place binomial and the second 1-place binomial) being 0000 0001 0011 is displayed as 7 white, 1 black, 2 white, and 2 black.
The remaining portion of FIG. 4B is converted in the same manner until the Compressed File in FIG. 5 is completely processed. Comparing FIG. 4A to FIG. 5 , note that a file of 512 bits has been converted into a file of 387 bits, a reduction in size of 24.4%. This file may be further compressed using the same or any other compression method. The resulting reduced-size file now may be stored or transmitted more efficiently. A method of the present invention is to decode this file.
Operation—Decoding a Run
Upon retrieval of s file, each encoding step is sequentially reversed To recreate FIG. 4B from FIG. 5 , the NOTA process is reversed, designated as Nota Decoder (FIG. 1 ). In FIG. 5 , this time taking the file's last three runs and their variable length binomials of 4, 2 and 20 places, 26 places are counted back to a start position The first place from this start point, 1 bit, is white, 0 , meaning “a run greater than 1, take the next binomial.” The next Fibonacci-length binomial, 1 bit, is white, 0 meaning “a run greater than 2, take the next binomial.” The next binomial, 2 bits, contains at least one black pixel, a 1, meaning “the run is contained within, start over.” The 2 place binomial is black-white, 10 , which means a run of 4 (colored white as designated by the previous run, not shown.) This is the third from the last run of 4 white pixels in FIG. 4 A.
Operation—Decoding the Following Runs
In FIG. 5 , the next binomial place, 1 bit, is white, a 0 , meaning “a run greater than 1, take the next binomial.” The next binomial, 1 bit, contains one black pixel, a 1, meaning a run of 2, start over.” This is the second from the last run of 2 black pixels in FIG. 4 A.
In FIG. 5 , the next binomial place, 1 bit is white, a 0 , meaning “a run greater than 1, take the next binomial.” The next binomial place, 1 bit, is white, a 0 , meaning “a run greater than 2, take the next binomial.” The next binomial places, 2 bits, are both white, 00, meaning a run greater than 5, take the next binomial. “The next binomial places, 3 bits, are all white, 000, meaning a run greater than 12, take the next binomial.” The next binomial places, 5 bits, are all white, 00000, meaning a run greater than 43, take the next binomial. “The next binomial places, 8 bits, contain at least one black pixel, a 1 , meaning the run is contained within, start over.” The combined 20-place binomial is 0000 0000 0000 0001 1011, meaning a run of 70. This is the last run of 70 white pixels in FIG. 5 .
As shown in FIG. 1 , after all of the Compressed File has been similarly processed with the Nota Decoder, the resulting bitmap will be an exact duplicate of the Parsed Input Bitmap which is now redesignated the Parsed Output Bitmap (FIG. 4 B). Please note that it is 512 pixels in the same dimensions of 8 pixels wide by 64 pixels high and maintains the same number of black and white pixels in the same relative positions.
Operation—Recombining the Parsed File and Sending to a Display Device
Also as shown in FIG. 1 , this file then is processed by reversing the parsing method previously used. Each pixel of the Parsed Output Bitmap is reassigned to its original position in the Revised Input Bitmap now redesignated the Revised Output Bitmap (FIG. 4 A). Note that it is 512 pixels in the same dimensions of 16 pixels wide by 32 pixels high and maintains the same number of black and white pixels in the same relative positions.
This file then is displayed either on a personal computer screen or by a printer, designated as Screen or Printer Display (FIG. 1 ). Please note that the above method does not recreate the Monochrome Input Bitmap ( FIG. 1 ) with its two-pixel-by-two-pixel cells' sixteen patterns. Additionally, the invention's use of a Fibonacci series of successively larger binary numbers to contain run-lengths is only one of numerous possible methods of generating such a number series.
Conclusion, Ramifications and Scope
Accordingly, the reader will see that the none-of-the above method of this invention more efficiently compresses and decompresses a revised monochrome bitmap file. In addition, the method produces a compressed binary tile that more efficiently may be stored and transmitted between digital computing devices. And, the method faithfully reproduces the revised input monochrome bitmap file for accurate display on a digital computer monitor or printer.
By using one permutation of a variable-length binary number to designate the parameters of a successive monochrome color run and any of the remaining permutations to designate the actual run and a return to the smallest variable-length binary, conservation of available resources of a binary computer relative to processing, storage and transmission is achieved. Such conservation relies on the method of this invention including the revision of the input monochrome bitmap and the parsing of the revised binary bitmap file to promote longer runs. The resulting compressed file results in a demonstrated saving over the size of the input file.
Although the description above contains many specificities, those should not be construed as limiting the scope of the invention but as merely providing illustration of some of the presently preferred embodiments of this invention.
Thus the scope of the invention should be determine by the appended claims and their legal equivalents, rather than by the examples given.
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An improved method of encoding and compressing digital halftones that utilizes a “none-of-the-above” method for designating variable-length runs. A monochrome input bitmap is rearranged slightly to reduce the patterns possible in contained digital halftone cells. This revised monochrome bitmap is parsed into subfiles to optimize run-lengths. The parsed subfiles are combined into a single file whose alternating runs of 1's and 0's are converted into successive variable-length binary numbers. One of the permutations of an antecedent binary is designated “none-of-the-above” and its use triggers a subsequent variable-length binary. All other permutations within each variable-length binary may designate a specific contained run-length and such use triggers a return to the initial binary in the series. The above method is reversed to decode and uncompress the encoded file to reproduce the original revised monochrome bitmap for display by a computer monitor or printer.
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FIELD OF THE INVENTION
[0001] This invention relates to the field of therapeutics and in particular relates to the treatment of arthritis.
PRIOR ART
[0002] The following is a list of prior art, which is considered to be pertinent for describing the state of the art in the field of the invention. Acknowledgement of these references herein will be made by indicating the number from their list below within brackets.
[0003] (1) Olah M. E. and Stiles G L. The role of receptor structure in determining adenosine receptor activity, Pharmacol. There., 85:55-75 (2000);
[0004] (2) Poulsen S. A. and Quinn R. J., Adenosine receptors: new opportunities for future drugs. Bioorg. Med Chem., 6:619-641 (1998);
[0005] (3) Fang X. et al. Phosphoxylation and inactivation of glycogen synthase kinase 3 by protein kinase A., Proc. Natl. Acad. Sci. USA, 97:11960-11965 (2000);
[0006] (4) Fishman, P., et al., Involvement of Wnt Signaling Pathway in IB-MECA Mediated Suppression of Melanoma Cells, Oncogene 21:4060-4064 (2002);
[0007] (5) Ferkey, D. M., and Kinmelman, D. GSK-3: New Thoughts on an Old Enzyme, Dev. Biol., 225:471479 (2000);
[0008] (6) Bonvini, P., et al. Nuclear beta-catenin displays GSK-3beta- and APC-independent proteasome sensitivity in melanoma cells, Biochim Biophys. Acta., 1495:308-318 (2000);
[0009] (7) Olah, M E. and Stiles, G K, The role of receptor structure in determining adenosine receptor activity, Pharmacol. Ther., 85:55-75 (2000);
[0010] (8) Szabo C., et al. Suppression of macrophage inflammatory protein (MIP)1□ producing and collagen induced arthritis by adenosine receptor agonists., British Journal of Pharmacology, 125:379-387 (1998);
[0011] (9) U.S. Pat. No. 5,773,423.
BACKGROUND OF THE INVENTION
[0012] A3 adenosine receptors belong to the family of the Gi-protein associated cell surface receptors. Receptor activation leads to its intention and the subsequent inhibition of adenylyl cyclase activity, cAW formation and protein kinase A (PKA) expression, resulting in the initiation of various signaling pathways (1,2) . PKA contains a catalytic subunit PKAc which dissociates from the parent molecule upon activation with cAMP Recent studies have demonstrated that PKAc phosphorylates and inactivates the enzme glycogen synthase kinase 3β (GSK-3β) (3) .
[0013] Recently, it has been shown that 1-deoxy-1-[6[[(3-iodophenyl)methyl]amino]-9H-purine-9-yl]-N-methylβ-D-ribofira-nuronaminde IB-MECA) disclosed in U.S. Pat. No. 5,773,423 incorporated herein by reference, a stable agonist to A3AR, alters the expression of GSK-30 and O-catenin, key components of the Wnt signaling pathway. Consequently it let to the inhibition of the expression of the cell cycle progression genes, c-myc and cyclin D1 (4) .
[0014] Szabo et at, ( 8) reported that IB-MECA suppresses the production of MIP-1α in macrophages in a dose dependent manner, and was shown to inhibit, also in a dose dependent manner, the production of the cytokines IL-1, IL-2, IL-6 as well as NO. According to this publication, administration of 0.5 mg/kg of IB-MECA a day reduced the severity of joint inflammation in a model of collagen-induced arthritis in mice.
[0015] Rheumatoid arthritis is a common rheumatic disease, affecting more than two million people in the United. States alone. The disease is three times more prevalent in women as in men but afflicts all races equally. The disease can begin at any age, but most often starts between the ages of forty and sixty. In some families, multiple members can be affected, suggesting a genetic basis for the disorder. The cause of rheumatoid arthritis is unknown. Even though infectious agents such as viruses, bacteria, and fungi have long been suspected, none has been proven as the cause. It is suspected that certain infections or factors in the environment might trigger the immune system to attack the body's own tissues, resulting in inflammation in various organs of the body. Regardless of the exact trigger, the result is an immune system that is geared up to promote inflammation in the joints and occasionally other tissues of the body, Lymphocytes are activated and cytokines, such as tumor necrosis factor/TNF and interleukin-1/IL-1 are expressed in the inflamed areas.
[0016] The clinical expression of rheumatoid arthritis is manifested by chronic inflammation of the joints, the tissue surrounding the joints such as the tendons, ligaments, and muscles, as well as other organs in the body such as the eyes. The inflammation process of causes swelling, pain stiffness, and redness in the joints. In some patients with rheumatoid arthritis, chronic inflammation leads to the destruction of the cartilage, bone and ligaments causing deformity of the joints.
SUMMARY OF THE INVENTION
[0017] The invention is described in the following SUMMARY with reference to a therapeutic method for the treatment of inflammatory arthritis. It should be noted that in addition to said therapeutic method, also encompassed within Me present invention is an oral pharmaceutical composition for the treatment of inflammatory arthritis that comprises an effective amount of the active agents as defined bellow and a carrier pharmaceutically acceptable for oral administration; as well as the use of said active agent for the preparation of a pharmaceutical composition for oral administration to a subject suffering of inflammatory arthritis and being in need for an anti-inflammatory treatment. As will be appreciated, the effective amount in the pharmaceutical composition will depend on the intended therapeutic regiment and the desired therapeutic dose. By way of example were the dose is 1 mg per day and the desired administration regiment is once daily administration, the amount of active agent in the pharmaceutical composition will be 1 mg where it is intended to divide his daily dose in 2 daily administrations, the amount of the active agent in he pharmaceutical composition will be 0.5 mg.
[0018] In the following, the term “anti-inflammatory” will be used to denote the disease modifying effect of IB-MECA or Cl-IB-MECA in alleviating the inflammatory response in inflammatory arthritis. The anti-inflammatory response may be determined on the basis of histological parameters, the extent of swollen and tender joints, motility parameters, reduction in pain, a number of different overall performance scoring systems, etc.
[0019] The present invention is based on the surprising finding that oral administration of specific A3-receptor agonists, N 6 -(3-iodobenzyl)-adenosine-5′-N-methyl-uronamide (IB-MECA) or 2-chloro-N-6-(3-iodobenzyl)-adenosine-5′-N-methyl-uronamide (Cl-IB-MECA) alleviated symptoms of inflammatory arthritis at doses which are lower than those previously described, particularly by Szabo et. al (8) .
[0020] The above findings were corroborated by clinical data showing that oral administration of low doses of IB-MECA to humans led to improvements in some of the disease manifestations in rheumatoid arthritis patients.
[0021] In the following, unless otherwise indicated, dosages are indicated in weight/Kg meaning to denote weight of administered agent (IB-MECA or Cl-IB-MECA) per kilogram of body of weight in each ministration: mg/Kg and microgram/Kg denoting, respectively milligrams of administered agent and micrograms of administered agent per kilogram of body weight of the treated subject.
[0022] It was also shown that the anti-inflammatory effect of these two drugs appears to be manifested with a surprising dose dependency relationship that is different than might have been expected from the prior art. In particular, it was shown that a potent anti-inflammatory activity is observed over a range of dosages without any dose clear correlation between the dose and the anti-inflammatory effect. Thus, for example, in some anima experiments an oral administration of a dose of 10 microgram/Kg had a stronger anti-inflammatory effect than a dose of 100 microgram/Kg; in some other experiments these two doses had a response that was essentially the same. Typically, pharmaceutically active substances have a classic dose-dependent effect so that the higher the dose the more pronounced the is the therapeutic effect, with the highest dose limitation being usually dictated by undesired side effects (toxicity) that become evident in higher doses. Such a classical dose-response behavior was previously reported for IB-MECA in the suppression of MIP-1 alpha production by Szabo et. al (8) .
[0023] A clinician or an investigator wishing to administer IB-MECA or Cl-IB-MECA to a subject as a drug for the treatment of inflammatory arthritis or develop these drugs as a therapy for such disease would have concluded from the prior art dose-response relationship that a dose that is higher than 0.5 milligram/Kg and possibly even much higher, would be suitable for such treatment. Against this, according to the unexpected findings of the present invention, it has been demonstrated that the effect of IB-MECA and Cl-IB-MECA in the alleviation of arthritis occurs with a different dose response curve as could have been envisaged based on the prior art, as also pointed out above. According to the invention, the dose dependent curve features a very strong effect at dosages that are considerably lower than the lowest effective dose reported by Szabo et. al, with a very marked effect seen a dosages as low as 25 times lower than lowest one in the Szabo publication. This is particularly so seeing that the administration accordance with the prior art, and particularly the said Szabo publication were intraperitoneal while the administration according to the invention is oral in which case the plasma level is limited by absorption.
[0024] These findings pave the way to the development of a therapeutic regiment were effective treatment of arthritis can be achieved by administering low oral doses of IB-MECA or Cl-IB-MECA with significantly lower risk of undesired side effects.
[0025] Thus, the present invention concerns, by one embodiment, a method for the treatment of inflammatory arthritis (IA) in a human subject, comprising: orally administering to an individual in need of such treatment an effective amount of N 6 (3-iodobenzyl)adenosine-5′-N-methyl-uronamide (IB-MCA) or 2-chloro-N 6 -(3-iodobenyl)-adenosine-5′-N-aethyl-uronamide (CL-IB-MECA);
[0026] wherein the effective amount is an amount which is preferably less than the maximal tolerated dosage (MID) and is an amount in a range between D x and D y ; D x being an amount lower than D MAX and D Y being an amount higher than D MAX ; D MAX being an amount that yields a maximal therapeutic effect; both D X and D Y yield a therapeutic effect that is substantially less than that obtained at D MAX .
[0027] The term “therapeutic effect that is substantially less” refers to the fact that one or more of the beneficial effects mentioned bellow in reference to the definition of “treatment” (decreased swelling, decreased pain, improved motility, slowing of the progression of the disease, increase in the time period of the remission between acute attacks of the disease, decrease in the time period of the acute attack prevention of the deterioration of the joints etc) is substantially less than that obtained at D MAX . The term “substantially less” refers preferably to a therapeutic effect in the treatment of inflammatory arthritis (IA) that is at least about 50% of that that can be achieved with D MAX . As can be appreciated, D MAX and accordingly also D X and D Y , may depend on the age, gender, overall heath condition, co-administered drugs and other factors. A preferred dose is D MAX or a dose close to it may be appreciated, in practice, the effective dose may be set as an average, for example based on dose-finding clinical studies. The design of such studies is a routine undertaking of those versed in the art of clinical drug development.
[0028] The term: “inflammatory arthritis” (IA) refers in the context of the present invention to chronic inflammation, (regardless of the cause but typically due to an autoimmume process that affects the joints), in the tissue around the joints, such as the tendons, ligaments, and muscles, as well as other organs in the body. This term includes rheumatoid arthritis, psoriatic arthritis, IBD-associated arthritis, reactive wapitis, vasculities and SLE. A preferred therapy target in accordance with the invention is rheumatoid arthritis.
[0029] The term “treatment” in the context of the present invention refers to any improvement in the clinical symptoms of the disease, as well as any improvement in the well being of the patients, in particular an improvement manifested by at least one of the following: decreased swelling and tenderness of the joints, decrease in pain in the joints, improved motility, slowing of the deterioration of the joints and the surrounding tissue, increase in the remission period between acute disease attacks; decrease in the time length of the acute attack; prevention of the onset of severe disease, etc.
[0030] The effective amount in accordance with the present invention is defined as an amount that is between DX and DY, as defined above. Additionally, this amount should also be less than the maximal tolerated dosage (LTD).
[0031] The term “maximal tolerated dosage” or “MTD” refers to the highest dosage of the active substance that most people can tolerate without side effects. In accordance with clinical trials the maximal tolerated dose of IB-MCA was found to be a dose of about 5 mg (about 70-micro ram/Kg; calculated on-the-basis of average individual human weight of 70 Kg.) for once daily administration and a dose of about 4 mg (about 57 microgram/Kg) for twice daily administration.
[0032] The “effective amount” can be readily determined, in accordance with the invention, by administering to a plurality of tested subjects various amounts of the active agent and then plotting the physiological response (for example an integrated “arthritic index” combining several of the therapeutically beneficial effects) as a function of the amount. The amount above which the therapeutic beneficial effects begin to decrease (but is still lower than the MTS) is the “effective amount”. Due to statistical distribution typically the “effective amount” is not a single parameter but a range of parameters.
[0033] In murine the effective amount is typically less than about 400 microgram/g. A typical dose would be in the range of about 1 microgram/Kg to about 200 microgram g, with a preferred dose being in the range of about 5 microgram/Kg to about 150 microgram/Kg. The corresponding effective amount in human will be an equivalent amount to that observed in murine, which may be determined in a manner as explained bellow.
[0034] The present invention thus concerns, by another embodiment, a method for the treatment of inflammatory arthritis (IA) in a human subjetc, comprising orally administering to a mammal in need of such treatment an effective amount of N 6 -(3-iodobenzyl)adenosine-5′-N-methyl-uronamide (IB-MECA) or 2-chloro-N 6 -(3-iodobenzyl)-adenosine-5′-N-methyl-uronamide (CL-IB-MECA), wherein the effective amount is an amount which the human equivalent of a murine dose of 0.001 mg/Kg to 0.4 mg/Kg administered once or more, preferably twice a day.
[0035] The term “human equivalent” refers to the dose that produces in human the same effect as featured when a dose of 0.001-0.4 mg (Kg of IB-MECA or Cl-IB-MECA is administered to a mouse or a rat. As known, this dose depends and may be determined on the basis of a number of parameters such as body mass, body surface area, absorption rate of the active agents clearance rate of the agent, rate of metabolism and others.
[0036] The human equivalent may calculated based on a number of conversion criteria as explained bellow; or may be a dose such that either the plasma level will be similar to that in the murine following administration at a dose as specified above; or a dose that yields a total exposure (namely area under the curve—AUC—of the plasma level of said agent as a function of time) that is similar to that in murine at the specified dose range.
[0037] It is well known that an amount of X mg/Kg administered to rats can be converted to an equivalent amount in another species (notably humans) by the use of one of possible conversions equations well known in the art. Examples of conversion equations are as follows:
Conversion I: Species Body Wt. (Kg) Body Surf. Area (m 2 ) Km Factor Mouse 0.2 0.0066 3.0 Rat 0.15 0.025 5.9 Human Child 20.0 0.80 25 Adult 70.0 1.60 37
[0038] Body Surface area dependent Dose conversion: Rat (150 g) to Man (70 Kg) is 1/7 the rat dose. This means that in the present case 0.001-0.4 mg/Kg in rats equals to about 0.14-56 microgram/Kg in humans; assuming an average weight of 70 Kg, this would translate into an absolute dosage of about 0.01 to about 4 mg.
[0039] Conversion II:
[0040] The following conversion factors: Mouse=3, Rat=67. Multiply the conversion factor by the animal weight to go from mg/Kg to mg/m 2 for human dose equivalent
Species Weight (Kg) BSA (m 2 ) Human 70.00 1.710 Mouse 0.02 0.007 Rat 0.15 0.025 Dog 8.00 0.448
[0041] According to this equation the amounts equivalent to 0.001-0.4 mg/Kg in rats for humans are 0.16-64 μg/Kg; namely an absolute dose for a human weighing about 70 Kg of about 0.011 to about 4.4 mg, similar to the range indicated in Conversion I.
[0042] Conversion III:
[0043] Another alternative for conversion is by setting the dose to yield the same plasma level or AUC as that achieved following administration to an animal. Based on measurement made in mice following oral administration of IB-MECA and based on such measurements made in humans in a clinical study in which IB-MECA was given to healthy male volunteers it was concluded that a dose of 1 microgram/Kg-400 microgram/KG in mice is equivalent to a human dose of about 0.14-57 microgram/Kg, namely a total dose for a 70 Kg individual of 0.01-4 mg. This is again similar to the dosages calculated according to Conversion I and I.
[0044] Based on the above conversion methods, the preferred dosage range for IB-MECA and Cl-IB-MECA would be less than 4 mg, typically within the range of about 0.0-1 to about-2 mg (about 0.14-28 micrograms-Kg, respectively) and desirably within the range of about 0.1 to 1.5 mg (about 1.4-21 micrograms/Kg, respectively). This dose may be administered once, twice or at times several times a day. Human studies showed (data not shown herein) that the level of IB-MECA decays in the human plasma with a half life of about 8-10 hours, as compared to a half life of only 1.5 hours in mice, in case of multiple daily administration, correction in the dosages for accumulative effects needs to be made at times (a subsequent dose is administered before the level of a previous one was decayed and thus there is a build-up of plasma level over that which occurs in a single dose. On the basis of said human trials twice daily administration appears to be a preferred administration regiment. However this does not rule out other administration regiments.
[0045] The present invention discloses for the first time clinical trials in humans showing the effectiveness of IB-MECA, in a specific dosage range, in the treatment of rheumatoid arthritis. In this human study IB-MECA was administered to patients in dose ranging between 0.1 to 4 mg twice daily.
[0046] The administration of said agent to a patient may be together with a pharmaceutically carrier acceptable for oral administration.
[0047] By the term “pharmaceutically acceptable carrier” it is meant any one of inert non-toxic materials, which do not react with the IB-MECA or Cl-IB-MECA and which can be added to oral formulations as diluents or carriers or to give form or consistency to the formulation. The formulation may be in the form of a pill, capsule, in the form of a syrup, an aromatic powder, and other various forms. The carrier is selected at times based on the desired form of the formulation. The carrier may also at times have the effect of the improving the delivery or penetration of the active ingredient to the target tissue, for improving the stability of the drug, for slowing clearance rates, for imparting slow release properties, for reducing undesired side effects etc. The carrier may also be a substance that stabilizes the formulation (e.g. a preservative), for providing the formulation with an edible flavor, etc. The carriers maybe any of those conventionally used and is limited only by chemical-physical considerations, such as solubility and lack of reactivity with IB-MECA or CL-IB-MECA, and by the route of administration. The carrier may include additives, colorants, diluents, buffering agents, disintegrating agents, moistening agents, preservatives, flavoring agents, and pharmacologically compatible carriers. In addition, the carrier may be an adjuvant, which, by definition are substances affecting the action of the active ingredient in a predictable way. Typical examples of carriers include (a) liquid solutions, where an effective amount of the active substance is dissolved in diluents, such as water, saline, natural juices, alcohols, syrups, etc.; (b) capsules (e.g. the ordinary hard- or soft-shelled gelatin type containing, for example, surfactants, lubricants, and inert fillers), tablets, lozenges (wherein the active substance is in a flavor, such as sucrose and acacia or tragacanth or the active substance is in an inert base, such as gelatin and glycerin), and troches, each containing a predetermined amount of IB-MECA or CL-IB-MECA as solids or granules; (c) powders; (d) suspensions in an appropriate liquid; (e) suitable emulsions; (f) liposonme formulation; and others.
[0048] The invention will now be exemplified in the following description of experiments that were carried out in accordance with the invention. It is to be understood that these examples are intended to be in the nature of illustration rather than of limitation. Obviously, many modifications and variations of these examples are possible in light of the above teaching. It is therefore, to be understood that within the scope of the appended claims, the invention may be practiced otherwise, in a myriad of possible ways, than as specifically described hereinbelow.
BRIEF DESCRIPTION OF THE DRAWINGS
[0049] In order to understand the invention and to see how it may be carried out in practice, some preferred embodiments will now be described, by way of non-limiting examples only, with reference to the accompanying drawings, in which:
[0050] [0050]FIG. 1A: shows the effect of PO administered IB-MECA 10 microgram/kg a day (square), or 100 microgram/kg a day (circle), or control untreated mice (diamond), on the inflammatory intensity in an animal model of adjuvant arthritis.
[0051] [0051]FIG. 1B: shows the effect of PO administered IB-MECA 1 microgram a day (square), or control untreated mice (diamond), on the inflammatory intensity in n animal model of adjuvant arthritis;
[0052] FIGS. 2 A and 2 B: show pictures of rats of FIG. 1, having adjuvant induced arthritis, untreated ( 2 A) and treated with 10 microgram/kg a day IB-MECA (treatment starts 7 days after disease induction ( 2 B));
[0053] FIGS. 3 A and 3 B: show histological sections of a slice from a rat's joint having adjuvant induced arthritis: untreated ( 3 A) and treated with 10 microgram/kg a day IB-MECA, treatment starting 7 days after disease induction ( 3 B);
[0054] [0054]FIG. 4: shows inflammatory intensity in a model of adjuvant arthritis as a function of time for control untreated rats (dark circles); rats treated with 10 microgram/kg a day Cl-IB-MECA (squares) and rats treated with 100 microgram/kg a day of Cl-IB-MECA (triangles); treatment started 7 days after disease induction;
[0055] [0055]FIGS. 5A to 5 D: shows pictures of rats ( 5 A & 5 C) and an enlarged picture of their paws ( 5 B & 5 D, respectively), having adjuvant induced arthritis treated (SA) and untreated ( 5 C) with CL-IB-MECA 10 microgram/kg a day, treatment staring 7 days after disease induction;
[0056] [0056]FIG. 6: shows the effect of administration of 10 microgram/kg of IB-MECA (CF-101) on joint swelling in a collagen-induced-arthritis (CIA) model in mice;
[0057] [0057]FIG. 7A: shows a histological section of joints of normal mice;
[0058] [0058]FIG. 7B: shows histological cross section of joints of untreated collagen-induced-arthritic mice;
[0059] [0059]FIG. 7C: shows histological cross section of collagen-induced-arthritic mice treated with 10 μg/kg IB-MECA;
[0060] [0060]FIG. 8: Chows a combined histological score of CIA mice not treated (control) and CIA mice treated with 10 microgram/kg of IB-MECA;
[0061] [0061]FIG. 9: shows the change in semi-recumbent heart rate as a function of plasma IB-MECA concentration after single doses of IB-MECA; and
[0062] FIGS. 10 A and 10 B: show the change in standing heart rate as a function of plasma B3-MECA concentration after repeated doses of IB-MECA.
DETAILED DESCRIPTION OF THE INVENTION
EXAMPLE 1
Experimental Procedures
[0063] Materials and Methods
[0064] IB-MECA and Cl-IB-MECA were purchased from RBI/Sigma (Natick, MA, USA). For both reagents, a stock solution of 10 μM was prepared in DMSO and further dilutions in KPMI medium were performed.
[0065] 1. Adjuvant Arthritis-Induction
[0066] Animal: Rats: LEWIS. Age: 9-12 Weeks. Sex: Female
[0067] Disease induction: 10 microgram/ml Heat killed Mycobacterium tuberculosis H37Ra (Difco, Detroit, Mich., USA) present in /IFA=Incomplete Freund's Adujvant (Sigma), were injected in an amount of 100 microliter at the tail base, S.C. (Sub Cut) In accordance with the ref; Current Protocols in Immunology ed. John E. Coligon, (1996) Unit 15.5.
[0068] 2. Collagen-Induced-Arthritis
[0069] Male DBA mice, aged 10 weeks, were injected SC with 100 μl of Type II collagen 200 μg in complete Freund's adjuvant (CFA). On day 21 a booster injection of the same emulsion was administered. Mice were inspected daily for symptoms of clinical arthritis.
[0070] 3. Arthritis Evaluation
[0071] The inflammatory intensity, presented as joint swelling, was measured by Caliper (Mitatoyo Co., Tokyo, Japan). Histopathological sections of these decalcified whole joints were stained with bematoxylin-cosin. Slides were screened for the following arthritic characteristics: inflammatory cell infiltration, synovial cell lining hyperplasia and pannus formation. The histological assessment of the knees inflammation intensity was divided to four parameters:
[0072] 1. Lymphatic follicle like formation-graded—0-4
[0073] 2. Inflammatory cells infiltration—graded 0-4
[0074] 3. Synovial cells hyperplasia- graded—0-4
[0075] 4. Pannus formation—graded 0-4
[0076] The arithmetic sum of these four parameters above all together designated-“Total Arthritic Score” (Goldenberg et al, J. Rheumatol. 1: 5-11,1983). The white blood cell (WBC) count and the serum levels of the pro-inflammatory cytokine TMF-α served as humoral markers of the immune system activation. Tumor necrosis factor-α sera level was determined, in accordance with the manufacturer's guidelines, by ELISA kit “Quantikine M,” (R&D Systems, Minneapolis, Minn., USA).
[0077] 4. Statistical Analysis
[0078] The results were statistically evaluated using the Student's t-test. Comparison between the mean values of different experiments was carried out. The criterion for statistical signficance was p<0.05.
Example 1A
Effect of 10 and 100 μg/kg IB-MECA on Inflammatory Intensity-Adjuvant Model
[0079] Rats were induced with adjuvant arthritis as described above. Animals were divided into three groups each consisting of 10 rats. Group 1 served as control while group 2 was administered with 100 μg/kg PO IB-MCA a day, and group 3 was administered with 10 μg/kg PO IB-MECA a day. Treatment with the active substance began 7 days disease induction. The results are shown in FIG. 1A. As can be seen, administration of 100 μg/g or 10 μg/kg a day was effective in abolishing almost completely the inflammation as assessed by the inflammation intensity score. FIG. 1B shows the same experiment repeated with 1 μg/day. As can be seen even in this low dose a significant reduction was evident. FIGS. 2A and 2B show pictures of a control untreated rat induced with adjuvant arthritis ( 2 A) and a rat treated with 10 μg/kg a day IB-MECA ( 2 B). As can be seen while the paws of the untreated rat appear extremely swollen and red, the treated animal featured normal appearing paws.
[0080] [0080]FIGS. 3A and 3B show histological pictures of the joint of an untreated rat ( 3 A), featuring the typical arthritis destruction of the synovial tissue and bone.
[0081] Against this the histological picture ( 3 B) of adjuvant arthritis induced rat treated with 10 μg a day of IB-MECA appeared completely normal without featuring any destructive processes
Example 1B
Effect of 10 and 100 μg/kg CL-IB-MECA on Arthritis Score—Adjuvant Model
[0082] Rats were induced with adjuvant arthritis as described above. Rats were divided to tree groups each consisting of 10 animals. Group 1 served as control 0.20 while group 2 was administered with 100 μg/kg PO Cl-IB-MECA a day, and group 3 was administered with 10 μg/kg CL-IB-MECA PO a day. Administration was initiated at day 7 after disease induction. The results are shown in FIG. 4.
[0083] As can be seen administration of 10 Gg a day was significantly more effective in improving the arthritis score than administration of 100 μg/kg a day indicating that surprisingly the active ingredient does not have a classic “dose response effect” wherein the higher the dosage the more pronounced the effect, but rather a bell-shaped curve effect, where increase in the dosage caused decrease in the therapeutical effect. FIGS. 5A to 5 D show photographs of a control untreated rat induced with adjuvant arthritis ( 5 A) and a rat treated with 10 μg/kg a day-CL-IB-MECA ( 5 C). While the paws of the untreated rat appear extremely swollen and red, the treated animal featured normal appearing paws.
Example 1C
Effect of 10 μg/kg IB-MECA on Joint Swelling and Histology Score-Collagen Induced Model in Mice
[0084] Male DBA mice were treated to produce collagen-induced-arthritis as described above. Each group contained 10 animals and each experiment was conducted at least three times.
[0085] IB-MECA (10 μg/kg) was orally administered by gavage, twice daily starting at onset of clinical arthritis. The positive control received vehicle only. The inflammatory intensity in the CIA model was determined in accordance with the increase in the mice hind paw's diameter, measured by caliper (Mitotoyo, Tokyo, Japan). The mean score in each experimental group was designated as the “Clinical Score”.
[0086] Histology Score
[0087] Animals were sacrificed, the legs were removed up to the knees level, fixed in 10% formaldehyde, decalcified, dehydrated, paraffin-embedded, cut into 4 μm sections and stained by Hematoxylin-Eosin.
[0088] The assessment of all pathologic findings were performed blind (by L.R-W and M.H) using semi-quantitative grading scales of 0 to 4 for the following parameters:
[0089] a) The extent of inflammatory cells' infiltration to the joint tissues,
[0090] b) Synovial lining cell hyperplasia,
[0091] c) Pannus formation,
[0092] d) Joint cartilage layers destruction,
[0093] e) Bone damage and erosion score was graded 0-5: 0-normal.
[0094] 1—minimal loss of cortical bone at a few sites; 2—mild loss of cortical tabecular bone; 3—moderate loss of bone at many sites; 4—marked loss of bone at many sites; 5-marked loss of bone at many sites with fragmenting and full thickness penetration of inflammatory process or pannus into the cortical bone (17,18). The mean of all the histological parameters scores were designated “Histology Score”.
[0095] Results
[0096] In the following experiments, the effect of IB-MECA (10 μg/kg/day) on the development of collagen-induced arthritis was evaluated. The mice developed the disease several days after the second immunization with Type II collagen/CFA emulsion. In each individual mouse, IB-MECA was administered at the onset of disease. In the control group a maximal hind paw swelling was observed 6 days after disease onset, whereas in the IB-MECA treated group it was noted on day 14th (FIG. 6). The intensity of the arthritis was reduced throughout the experimental period, but on day 21 this difference became statistically significant (p<0.02). In the IB-MECA treated group (FIG. 7C) histology sections showed minimal inflammatory changes compared to the extensive one in the control group (FIG. 7A) and a pattern that was similar to control (FIG. 7B). In addition, the histology score was markedly lower in the IB-MECA treated group compared to the control group (3.87±1.2 vs. 1.00.6, p<0.01) (FIG. 8).
Example 1D
Clinical Trial in Humans—Effect of IB-MECA on Rheumatoid Arthritis
[0097] Patients with active rheumatoid arthritis were chosen for the study. All chosen patients met the following criteria:
[0098] Inclusion Criteria
[0099] Rheumatoid arthritis patients that were included in the study, met the following inclusion criteria:
[0100] 1. Males and females 18 years of age or older
[0101] 2. Functional Class I, II, or III by the criteria of the American College of Rheumatology
[0102] 3. Active RA, as indicated by the presence of (a)>6 swollen joints; AND (b) 29 tender joints; AND at least one of he following: (c) Westergren ESR of ≧28 mm/hour; OR (d) CRP level of >2.0 mg/dL; OR (e) morning stiffness for >45 minutes
[0103] 4. History of unsuccessful treatment (documented intolerance or lack of efficacy as determined by the Investigator) with at least 1, but no more than 4, of the following disease modifying anti-rheumatic drugs (DMARDs): methotrexate, hydroxychloroquine, sulfasalazine, oral or injectable gold, azathioprine, leflunomide, minocycline, and penicillamine, alone or in combination
[0104] Protocol
[0105] Patients included in the study were subjected to a 1 month washout period in which they ceased to take any DMARD. Following this one months washout the patients were administered twice daily with either with 0.1 mg, 1 mg of 4 mg of IB-MECA in a double-blind fashion. The drug was formulated in a soft gel capsule containing IB-MECA dissolved in Cremophor RH. The patients received the drug for a period of up to 12 weeks.
[0106] Clinical Assessment
[0107] Disease activity was assessed using standard criteria as laid down by the American College of Rheumatlogy (ACR).
[0108] Results
[0109] 15 patients were treated and in at least half of them a significant improvement in disease symptoms was observed for a period of up to the 12 weeks of the study.
EXAMPLE 2
Determining Maximal Tolerated Dose of IB-MECA in Humans
[0110] Methods
[0111] Study design
[0112] Two clinical studies were carried out: a single dose study and a repeat dose study. Both studies were parallel-group, double-blind, dose-rising, and placebo-controlled in design.
[0113] In the single dose study, 15 healthy men (3 groups of 5) received a single oral dose of IB-MECA (1, 5 or 10 mg) or placebo. In each group, 1 subject received placebo. In the repeated dose study, 28 healthy men (4 groups of 7) received repeated oral doses of IB-MECA (2, 3, 4 or 5 mg) or placebo every 12 h for 7 days. In each group, 2 subjects received placebo.
[0114] Selection of Subjects
[0115] Healthy young men, aged 1845 years.
[0116] Study Drugs
[0117] In the single dose study, a solution with IB-MECA powder in 30% Cremophor RH40 (BASF) was used. In the repeated dose study, an aqueous 0.5% methylcellulose suspension (Nethocel A4M Premium, The Dow Chemical Company) was used. In both studies, the study medication was taken orally as a drink, followed by 50 ml of tap water.
[0118] Study Procedures
[0119] The following procedures were done:
[0120] Safety assesment: laboratory assessments (routine biochemistry and urinalysis), physical examination, 12-lead ECG, ambulatory ECG, pulmonary function testing (FEV1), vital signs (semi-recumbent in the single dose study; semi-recumbent and standing in the repeat dose study). Adverse events were recorded throughout both studies.
[0121] Determination of IB-MECA blood level: in the single dose study blood samples for assay of IB-MECA were taken immediately before and at 0.25, 0.5, 1, 2, 4, 8, 12, 24, and 48 h after dosing; in the repeat dose study—blood samples were taken immediately before and at 0.25, 0.5, 1, 2, 4, 8, and 12 h after dosing on Day 1, before dosing on Days 26, and before and at 0.25, 0.5, 1, 2, 4, 8, 12, and 24 h after dosing on Day 7.
[0122] Plasma samples were assayed for IB-MECA using LC/MS/MS. The lower limit of quantification (LLOQ) was 0.1 ng/mL. Intra-assay coefficients of variation (CV) were <5.0% and inter-assay CVs were <9.4%.
[0123] Pharmacokinetic Analysis
[0124] Maximum concentration (C max ) and time to maximum concentration (t max ) were observed values., Other pharmacokinetic parameters (half-life, t /2 ; AUC; and clearance, CL/F) were calculated by non-compartmental methods using WinNonlin® software (version 3.0, Pharsight, Mountain View, Calif., US). Accumulation indices of C max and AUC were calculated as ratio of values at steady state (Day 7) to the values on Day 1.
[0125] Statistical Analysis
[0126] Data from all subjects who received IB-MECA were included in the analysis of safety and tolerability (adverse events and laboratory safety variables). Numerical data and parameters were summarised using means or medians, and other descriptive statistics, according to the type and distribution of the data.
[0127] Results
[0128] Study population
[0129] In the single dose study, the mean (range) age, weight, and height were 28.3 (2040 years, 75.9 (6398) kg, and 177.8 (167-188) cm, respectively. In the repeat dose study, the mean (range) age, weight, and height were 25.2 (18-45) years, 75.3 (5699) kg, and 178.0 (163-189) cm, respectively. All volunteers were of Europid ethnic origin, except for 2 Asian/Indian men and 1 Europid/Oriental man.
[0130] All subjects were deemed healthy at screening, without any haematological disorder or history of splenectomy, nor splenomegaly on physical examination.
[0131] Safety and tolerability
[0132] In the single dose study, IB-MECA in doses up to 5 mg was well tolerated, as judged by vital signs, physical examination, FEV1, and 12-lead and continuous ECG. There were no clinically significant changes in safety tests of blood and urine. Four subjects had a small increase in resting heart rate after 5 mg IB-MECA; however, after the 10 mg dose, 4 subjects had substantial increases in resting heart rate, 2 of which were substantial (up to 115 beats/min) and considered drag-related. Those 2 subjects developed nausea, and 1 of them vomited once and was facially flushed. Those changes precluded our studying higher doses. In no subject was there a significant change in blood pressure, but blood pressure was not measured in the standing position. The increase in heart rate was closely related to the plasma IB-MECA concentration (FIG. 9). In the repeat dose study, IB-MECA had an acceptable safety profile, as judged by vital signs, physical examination, FEV1, and 12-lead and continuous ECG. There was a dose-related increase in heart rate on Day 1, but some tolerance developed, because that effect was clearly smaller on Day 7. On Day 1, the time course of the increase in heart rate reflected the profile of plasma IB-MECA concentrations. However, on Day 7, equivalent plasma IB-MECA concentrations were associated with smaller increases in heart rate (FIGS. 10A & 10B). There, were no clinically significant changes in safety tests of blood and urine.
[0133] Most of the adverse events occurred during the 5 mg dose regimen: headache and drowsiness were most common. Two adverse events were vascular disorders—hot flushes and dizziness on standing.
[0134] Overall, IB-MECA was well tolerated at single doses of up to 5 mg and repeat doses of up to 4 mg 12-hourly. Adverse events were related to dose and generally occurred around the time of maximal blood concentration (t max ). (After single doses of up to 5 mg IB-MECA, there were no adverse events within 12 h of dosing, but after a single dose of 10 mg, there were 8 adverse events within 12 h of dosing. After repeated doses of up to 4 mg 12-hourly, there were 2 adverse events within 12 h of dosing. However, after repeated doses of 5 mg 12-hourly, there were 13 adverse events within 12 h of dosing. Thus, based on this repeat dose study, the 4 mg dose was determined to be the maximum tolerated dose for a twice-daily therapeutic regimen.
[0135] Overall a single daily dose of 5 mg and a twice daily dose of 4 mg where considered safe and well tolerated. Given the fact that these doses gave a plasma level (C max ) of less than 160 nM (80 ng/ml)
[0136] Pharmacokinetics
[0137] The pharmacokinetics of single doses of IB-MECA are shown in the following Table 1:
TABLE 1 Mean (SD) plasma PK parameters after a single oral dose of CF101 (n = 4 per group) C max t max a AUC (0-48) AUC (inf) t 1/2 CL/F Dose (mg) (ng/mL) (h) (ng · h/mL) (ng · h/mL) (h) (L/h) 1 21.2 (2.1) 1 (1-2) 220.7 (20.9) 225.2 (21.7) 8.7 (0.7) 4.5 (0.4) 5 81.6 (23.6) 1 (1-2) 872.3 (211.6) 904.0 (221.9) 8.3 (0.2) 5.8 (1.4) 10 178.0 (46.6) 1 (1-2) 1780.0 (228.7) 1813.0 (226.5) 8.6 (0.4) 5.6 (0.7)
[0138] As can be seen IB-MECA pharmacokinetics were linear, and inter-subject variability was low. IB-MECA was absorbed rapidly: t max ranged between 1-2 h. Mean C max (maxim plasma level) and AUC 0-48 (area under the cure of blood level over 48 hours after administration) were related to dose. C max was 21.2, 81.6, and 178.0 ng/ml, and AUC 0-48 was 220.7, 872.3, and 1780.0 ng.h/ml, for doses of 1, 5, and 10 mg, respectively. The half-life of about 8.5 h was independent of dose. Apparent plasma clearance (CL/F) was low (47 LAh) and independent of dose.
[0139] The pharmacokinetics of repeated doses of IB-MECA are shown in the following Table 2:
TABLE 2 Mean (SD) plasma PK parameters on Days 1 and 7 of repeated dosing with CF101 (n = 5 per group) Dose C max t max a AUC (0-12) AUC b t 1/2 CL/F (mg) Day (ng/mL) (h) (ng · h/mL) (ng · h/mL) (h) (L/h) 2 1 22.0 (3.3) 2 (1-4) 155.2 (39.1) 207.4 (52.0) 5.52 (0.2) 10.1 (2.3) 7 30.9 (3.1) 2 (1-2) 242.4 (41.4) 346.3 (64.0) 9.83 (1.2) 4.9 (0.7) 3 1 49.3 (9.7) 2 (1-2) 304.5 (19.5) 423.5 (27.5) 6.29 (1.0) 7.1 (0.5) 7 49.0 (7.9) 1 (1-2) 341.6 (38.1) 512.1 (74.1) 9.25 (0.8) 5.0 (0.6) 4 1 46.2 (11.4) 2 (1-2) 297.0 (57.2) 400.2 (85.7) 5.77 (0.6) 10.4 (2.1) 7 58.1 (10.4) 1 (1-2) 458.3 (54.8) 640.3 (73.7) 8.93 (0.8) 5.4 (0.7) 5 1 63.6 (22.0) 2 (1-2) 461.6 (157.4) 596.1 (196.6) 4.96 (0.3) 9.3 (3.5) 7 79.5 (24.1) 2 (2-2) 601.0 (163.6) 818.4 (214.0) 9.39 (0.6) 5.4 (1.5)
[0140] IB-MECA was absorbed rapidly: t max was 1-2 h. Steady state was reached by Day 3. IB-MECA pharmacokinetics did not change after repeated dosing. Plasma concentrations of IB-MECA were dose proportional on Day 1 and at steady state (Day 7). Half-life of IB-MECA was independent of dose, and was about 9-10 h at steady state. As in the single dose study, apparent plasma clearance (CL/F) was low (5-10 L/h) and independent of dose. The accumulation indices ranged between 1-1.4 and 1.1-1.6 for C max and AUC, respectively; the accumulation indices were much as predicted from the single dose data.
[0141] Summary
[0142] Overall a single daily dose of 5 mg and a twice daily dose of 4 mg where considered safe and well tolerated. Given the fact that. These doses gave a C max of less than about 160 nM (80 ng/ml).
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The present invention concerns a method for the treatment of inflammatory arthritis, and in particular rheumatoid arthritis, by administering to the subject specific low dosages of N6-(3-iodobenzyl)-adenosine 5′-N-methyl-uronamide (IB-MECA) and 2-chloro-N6-(3-iodobenzyl)-adenosine-5′-N-methyl-uronamide (CL-IB-MECA).
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TECHNICAL FIELD OF THE INVENTION
This invention relates to the preparation of blended polyolefins using certain catalyst compositions. More particularly, this invention relates to the use of catalyst compositions comprising ionic organometallic compounds, cation forming cocatalysts, and cross-over agents, to polymerize olefins into compatible blends of polyolefins of different microtactic structures, to polymerize olefins into compatible blends of polyolefins of dissimilar isomeric and copolymer structures, and to polymerize styrene into compatible blends of polystyrenes of different microtactic structures.
BACKGROUND OF THE INVENTION
Normally, two different polymers because of the very low entropy of mixing. Sometimes, however, two different polymers can form a compatible blend with the aid of an agent. The agent can be a block copolymer of two homopolymers. One of the problems associated with the prior art agents and methods of blending is that it is not a simple task to find such an agent, to devise a commercially viable synthetic method for its preparation and to subsequently blend the components into an homogeneous material without macrophase separation. In many instances, polymer blends have useful properties which are either superior or not possessed by the constituent homopolymers. For example, many members of the family of premium materials called engineering resins, are compatibilized polymer blends.
Different polyolefins assembled from the same monomer molecules having different geometrical, chemical, or stereochemical isomeric structures are generally immiscible. A well known example is low density polyethylene manufactured at high pressure and high density polyethylene manufactured at low pressure. Other prior art examples include the products of Ziegler-Natta catalyzed propylene polymerization which include high molecular weight isotactic-crystalline polypropylene and low molecular weight amorphous polypropylene. The two polymers are immiscible and the amorphous polymer must be removed or its presence renders the crystalline polymer physically and mechanically too weak to be of any commercial value.
Well-defined organometallic compounds, such as Group IVB elements, of the Periodic Table (Handbook of Chemistry and Physics, 49th Edition, Ed. R. C. Weast, Chemical Rubber Co. Cleveland, 1968) have been found to possess stereoselectivity in the polymerization of propylene, styrene, and other α-olefins depending upon the ligand structure of the organometallic precursor.
For example, in one prior art method, chiral group IVB metallocene precursors act as catalysts for the isospecific polymerization of propylene to yield isotactic polypropylene, (See U.S. Pat. No. 4,794,096 and the articles by Kaminsky et al. Angew. Chem. Int. Ed. Engl. 1985,24, 307 and by Ewen in J. Am. Chem. Soc. 1984, 106, 6355).
In addition, Ewen et al. as disclosed in J. Am. Chem. Soc. 1988, 110, 6255 and U.S. Pat. No. 4,892,851 taught that zirconocene precursors having bilateral symmetry could produce syndiotactic polypropylene and are capable of polymerizing ethylene, α-olefins and cycloolefins with comparable activity.
Organometallic compounds having C 2v symmetry, whether as a stereorigid zirconocene or a free rotating complex as disclosed by Chien et al., Macromolecules 1995, 28, 5399, tend to catalyze propylene polymerization without profacial selectivity. Similar nonspecific polymerizations of propylene have previously been catalyzed by titanium complexes with either a single η 5 ligand or a phenolic ligand.
In the case of styrene, syndioselective polymerizations have been achieved using either mono η 5 -ligands as disclosed by Ishihara et al in Macromolecules 1986, 19, 2464, or 2,2′-thiobis(6-t-butyl-4-methylphenoxy) ligands as disclosed by Miytake et al. in Makromol Chem. Macromol. Symp. 1993, 66, 203. Other prior methods have included the use of zirconocene dichloride and hafnocene dichloride as catalysts in the production of atactic polystyrenes.
All the above precursors and other conventional precursors have been used to provide for the linear polymerization of ethylene.
Brookhart et al. disclosed in J. Am. Chem. Soc. 1995, 117, 6414 that during the polymerization of ethylene in the presence of a 1.4-diaza-1,3-butadien-2-y nickel complex and a cocatalyst, branched polyethylene are produced.
All of the above precursor are activated by a cocatalyst which transforms the former catalist into the corresponding cationic species (See U.S. Pat. No. 5,198,401 and EP 573,403). The cocatalyst comprises a cation which irreversibly reacts with at least one ligand from either the Group IVB or VIIIB metal complexes to form the catalytically active cationic Group IVB or VIIIB complex. The counter anion is non-coordinating, readily displaced by a monomer or solvent, has a negative charge delocalized over the framework on the anion or within the core thereof, is not a reducing or oxidizing agent, forms stable salts with reducible Lewis acids and protonated Lewis bases, and is a poor nucleophile.
Other prior types of cocatalyst include Lewis acids which will irreversibly react with at least one ligand from a Group IVB metal complex to form an anion possessing many but not all of the characteristics described above (See Marks et al. J. Am. Chem. Soc. 1991, 113, 3623).
High molecular weight polypropylene having a certain steric structure, prepared individually in the presence of one of the prior art catalysts described above, is generally immiscible with another polypropylene of a different steric structure. For example, a solvent-casted blend of any pair of stereoisomeric polypropylenes, e.g., isotactic and atactic, etc., tend to crumble easily and the tensile bar press molded from the blend fails with the least bit of strain. Likewise linear polyethylenes and branched polyethylenes are immiscible as are mixtures of linear polypropylene and branched polypropylenes. Syndiotactic polystyrenes are typically incompatible with atactic polystyrenes.
In another prior process, solutions of two different metallocenes are used to polymerize monomers separately as if each is unaffected by the presence of the other. This method is useful for preparing polyethylenes with bimodal molecular weight distribution using two group IVB metallocenes as disclosed by Ewen, Studies in Surface Science and Catalysis Vol 25 Catalytic Polymerization of Olefins Eds. Keii et al., Kodansha, Elsevier, 1986, pp.271, and by Ahlers and Kaminsky, Makromol. Chem.; Rapid Commun. 1988,9, 457. A polypropylene having multimodal molecular weight distribution was obtained using an ansa-hafliocene and ansa-zirconocene mixture to produce isotactic polypropylenes albeit having molar masses that are different.
Despite all of the prior processes for preparing various polymers, there are no processes that are capable of forming compatibilized polyolefin blends of the present invention.
Unlike the prior art, the present invention allows one to synthesize, directly in a “one-pot” polymerization of a single monomer, useful blends of polyolefins having different steric structures and/or geometric structures without the need for subsequent blending of the polyolefins.
Thus, one object of the invention is to provide an olefin polymerization catalyst which can give olefin polymers of different structures A n and B m as well as a third substance having blocks of the same structures (A n 1 B m 2 ) x in its chain, the latter is capable of bridging A n and B m thus compatibilizing the two isomeric homopolymers. For example, in one preferred embodiment, A n , is an isotactic polypropylene and B m is an atactic polypropylene having the microstructures shown in the following conventional projection:
The subscripts n and m indicate that the number of monomeric units in the homopolymers which are large integers (10 to 30,000); the subscripts n 1 and m 1 indicate the number of monomeric units in the block copolymers which are smaller integers (10 to 1,000), and x ranging from 10 to 100 denotes the number of AB blocks.
Another object of this invention is to provide a catalyst composition for the “one-pot” direct synthesis of materials as disclosed in projection 1 wherein A n and B m can also be syndiotactic polypropylene, and hemiisotactic polypropylene. For any combination, A n and B m will always have different microstructures.
Another object of this invention is to provide a catalyst composition for the “one-pot” direct synthesis of the materials of projection 1 wherein A n is linear polyethylene and B m is branched polyethylene.
Another object of this invention is to provide a catalyst composition for the “one-pot” direct synthesis of materials of projection 1 wherein A n is ethylene- α-olefin copolymer (commonly referred to as liner low density polyethylene) and B m is a linear ethylene homopolymer (polyethylene).
Another object of this invention is to provide novel polymer blends from two different monomers.
Another object of this invention is to provide a catalyst composition for the “one-pot” direct synthesis of materials as shown in projection 1 wherein A n is a linear polypropylene having either an isotactic, syndiotactic or atactic microstructure and B m is a branched polypropylene.
Another object of this invention is to provide a catalyst composition for the “one pot” direct synthesis of the materials of projection 1 wherein A n is syndiotactic polystyrene and B m is atactic polystyrene.
Another object of this invention is to provide novel polymer blends from a single monomer exhibiting properties of plastics with a wide range of stiffness, hardness, impact strength, and abrasion resistance.
Another object of this invention is to provide novel polymer blends from a single monomer exhibiting properties of elastomers with 0 range of modulus, elasticity and cross link density of physical nature.
Another object of this invention is to provide novel low molecular weight polyolefin mixtures from a single monomer exhibiting properties suited for lubricant and motor oil applications.
Another object of this invention is to provide novel materials from a single monomer exhibiting properties characteristic of a plastomer.
Another object of this invention is to provide novel polymer blends from a single monomer exhibiting properties characteristic of a flexomer.
Another object of this invention is to provide novel polymer blends from a single monomer exhibiting properties characteristic of a thermoplastic elastomer.
Another object of this invention is to provide novel polymer blends from a simple monomer exhibiting properties characteristic of an elastomer.
Another object of this invention is to provide novel blend exhibiting unusual properties and having the characteristics of a tough plastomer, thermoplastic elastomer, gum rubbers and lubricating fluid, wherein all these materials are processed like thermoplastics.
A name is lacking for the novel materials of the present invention. The properties of the material suggest the following terms: interfacial polymer blends, interpenetrating polymer blends, naturally compatibilized polymer blends, or simply compatible polymer blends. These terms are used herein interchangeably but do not exclude other more suitable names.
SUMMARY OF THE INVENTION
The present invention relates to metallocene catalyst compositions which are designed to provide chemical and/or stereochemical control during the polymerization of polyolefins including ethylene, propylene higher α-olefins and/or styrene. The present invention provides a novel cross-over agent that promotes the interchange of propagating chains of one type of catalytic site to another, thus providing for the formation of materials capable of bridging or compatibilizing two different homopolymers so that a “naturally” compatible blend is produced directly.
The present invention also provides for several classes of polymerization catalysts.
A first class of olefin polymerization catalyst of the present invention is formed from a chiral stereorigid metallocene (iso-P) and cocatalyst that is capable of the isospecific polymerizing of propylene into an isotactic structure.
A second class of olefin polymerization catalyst of the present invention is formed from a bilaterally symmetric stereorigid metallocene (syn-P) and a cocatalyst capable of the syndiospecific polymerizing of propylene into a syndiotactic structure.
A third class of olefin polymerization catalyst of the present invention is formed from a C 2 , symmetric stereorigid or nonrigid metallocene (ata-P) and a cocatalyst capable of the nonspecific polymerizing of propylene into an atactic structure.
A fourth class of olefin polymerization catalyst of the present invention is formed from an asymmetric stereorigid metallocene (hemi-P) and a cocatalyst capable of the polymerizing of propylene into a hemiisotactic structure.
A fifth class of olefin polymerization catalyst of the present invention is formed from a single cyclopentadienyl metal compound (syn-S) and a cocatalyst capable of the polymerizing of styrene into a syndiotactic structure.
A sixth class of olefin polymerization catalyst of the present invention is formed from a cyclopentadienyl zirconium or hafnium compound (ata-S) and cocatalyst capable of polymerizing styrene into an atactic structure.
A seventh class of olefin polymerization catalyst of the present invention is formed from a 1,4-diaza-1,3-butadien-2-yl complex of group VIIIB metal (BR) and a cocatalyst capable of the polymerizing of ethylene into a branched polyethylene and propylene into branched polypropylene.
The present invention provides a cross-over agent to promote the interchange of the propagating chain on one olefin polymerization catalyst with another propagating chain on a second different olefin polymerization catalyst.
The present invention also provides a first process for the polymerization of olefins having its characteristic feature in that propylene is polymerized or block copolymerized in the presence of a catalyst precursor selected from the iso-P, syn-P, ata-P, hemi-P classes and a second precursor selected also from these four classes but which is not the same as the former, with a common cocatalyst and cross-over agent.
The present invention provides a second process for the polymerization of ethylene having characteristic features in that ethylene is polymerized or block copolymerized in the presence of a catalyst of the BR class and another precursor selected from metallocene or monocyclopentadienyl metal complexes, with a common cocatalyst and cross-over agent.
The present invention provides a third process for the polymerization of propylene having a characteristic feature in that propylene is polymerized or block copolymerized in the presence of a catalyst of the BR class and another precursor selected from the iso-P, syn-P, ata-P and hemi-P classes, with a common cocatalyst and cross-over agent.
The present invention provides a fourth process for the polymerization of styrene having a characteristic feature in that styrene is polymerized or copolymerized in the presence of a catalyst of the syn-S class and another precursor selected from the ata-S class, with a common cocatalyst and cross-over agent.
The present invention also relates to the products offered by the novel process including compatible blends of pairs of stereoisomeric polypropylenes: isotactic and atactic, syndiotactic and atactic, syndiotactic and isotactic, hemiisotactic and atactic, hemiisotactic and isotactic, hemiisotactic and syndiotactic; compatible blends of syndiotactic polystyrene and atactic polystyrene; compatible blends of linear polyethylene and branched polyethylene; and compatible blends of branched polypropylene and linear stereoisomeric polypropylene.
Finally, the present invention provides for the types of products in varying ratios of the constituent polymers that exhibit a range of physical, thermal, mechanical, morphological, viscoelastic and elastomeric properties.
BRIEF DESCRIPTION OF THE DRAWINGS
For a better understanding of the invention, its objects, features and advantages, there follows a Detailed Description of the invention which should be read in conjunction with the following figures in which:
FIG. 1 illustrates a room temperature 13 C NMR spectra in the methyl region of polypropylene as found in Example 1 of the present invention including (a) the heptane insoluble isotactic fraction; (b) the heptane soluble but hexane insoluble stereoblock fraction; and (c) the diethylether soluble atactic fraction;
FIG. 2 illustrates the stress-strain curves of (a) a compatible isotactic/atactic polypropylene as found in Example 1 of the present invention; (b) the polypropylene obtained in the presence of Cat. 1 (iso-P) and Cat. 3 (ata-P) catalysts immobilized on silica; (c) the atactic polypropylene synthesized with Cat. 3 (ata-P) alone; and (d) the solvent casted blend of atactic polypropylene and isotactic polypropylene obtained separately with Cat. 2 (iso-P) and Cat. 3 (ata-P);
FIG. 3 illustrates the relaxation time testing of the compatible isotactic/atactic polypropylene blend in Example 1 of the present invention;
FIG. 4 illustrates the percentage of elastic recovery for the compatible isotactic/atactic polypropylene in Example 1 of the present invention;
FIG. 5 illustrates the X-ray diffraction patterns of: (a) the isotactic polypropylene obtained with Cat. 1 alone; (b) the solution-casted blend of isotactic polypropylene obtained with Cat. 1 and atactic polypropylene obtained with Cat. 3; (c) the isotactic/atactic polypropylene blend synthesized with Cat. 1 and Cat. 3 immobilized on silica; (d) the compatible isotactic/atactic polypropylene blend in example 1 of the present invention; and (e) the atactic polypropylene obtained with Cat. 3 alone;
FIG. 6 illustrates the deconvolution analysis of the XRD pattern in FIG. 5 d;
FIG. 7 illustrates the room temperature 13 C NMR spectra in the methyl region of the syndiotactic polypropylene in Example 26 of the present invention: including (a) the heptane insoluble syndiotactic fraction; (b) the heptane and hexane soluble stereoblock fraction; and (c) the diethylether soluble atactic fraction;
FIG. 8 illustrates the relaxation time testing of the compatible syndiotactic/atactic polypropylene blend in Example 26 of the present invention;
FIG. 9 illustrates the room temperature 13 C NMR spectra of the methyl region of the polypropylene in Example 46 of the present invention including: (a) the diethyl ether soluble fraction, (b) the hexane soluble fraction, (c) the heptane soluble fraction, and (d) the heptane insoluble fraction; and
FIG. 10 illustrates the room temperature 13 C NMR spectra of the secondary and tertiary carbon resonances of the polypropylene in Example 46 of the present invention including: (a) the diethylether soluble fraction, (b) the hexane soluble fraction, (c) the heptane soluble fraction, and (d) the heptane insoluble fraction.
DETAILED DESCRIPTION OF THE INVENTION
The compounds used herein are referred to by names of common usage rather than the scientifically correct names for the sake of brevity. The bis(cyclopentadienyl) group IVB metal compounds may be referred to as “metallocene” embracing all other η 5 -rings such as indenyl, tetrahydroindenyl, fluorenyl, octahydrofluorenyl, benz[e ]indenyl, benz[f]indenyl and their derivatives with substituents. The metal compound may have two identical “cyclopentadienyls” or two dissimilar η 5 -rings. Cp, Ind and Flu are used to denote respectively, the cyclopentadienyl, indenyl, and fluorenyl radicals. In addition, a “metallocene” wherein the metal is titanium may be referred to as a “titanocene”; where the metal is zirconium as a “zirconocene”; where the metal hafnium as a “hafnocene”. Other group IVB organometallic compounds having only one or none of the Cp type ligands will be referred to as metallocenes.
Preferably, the olefin polymerization catalysts of the present invention are prepared from two or more metallocene precursors and a cocatalyst, the exception being the branch rearrangement polymerization catalyst precursor of the BR class. Preferably, the metallocene precursors of the present invention are complexes of group IVB elements including Ti, Zr and Hf, having one or more pentahapto-ligands including, for example, Cp (cyclopentadienyl), Ind (indenyl) and Flu (fluorenyl) having strategically placed hydrocarbyl groups of one (1) to forty (40) carbon atoms.
In the case of two pentahapto-ligands they may be bridged by 3, 2, 1 or 0 atoms selected from the group IIIA, IVA, VA, and VIA of the Periodic Table. The number and type of bridging atoms are determined by the stereorigidity and accessability desired of the metallocene. One pentahapto-ligand complex may contain a bridge connecting it to a norhapto-group having a heteroatom selected from the group IIIA, IVA, VA or VIA suitable for covalent or dative bonding to the group IVB metal center. The remaining nonhapto-ligands are selected from groups of hydrocarbyls having 1 to 20 carbon atoms, alkoxyl groups having 3 to 30 carbon atoms, or the group VIIA atoms.
The olefin polymerization cocatalysts preferably are Bronsted or Lewis acids and nucleophilic cations. Other possible cocatalysts are hydrocarbyl or oxyhydrocarbyl compounds from the group IA to VA elements. These cocatalysts function by oxidation of an anionic non-hapto-ligand from the metallocene precursor to generate the catalytic active corresponding metallocenium species.
The olefin polymerization catalytic composition of the present invention provides a cross-over agent from one of the following: metal hydrocarbyls, metal halocarbyls, metal oxyhydrocarbyls, or metal oxyhalocarbyls of the Groups IIB and IIIA. The counter-anion formed by the cocatalysts of the present invention is bulky, inert and compatible with and noncoordinating toward the Group IVB metal cation formed from the metallocene precursor.
In the present invention, the stereochemical specificity of a metallocene catalyst during the polymerization of propylene is mainly determined by its molecular structure. In the preferred embodiment of the present invention, there are four classes of metallocene catalysts, each of which promotes a different stereoregulated propylene insertion process as follows: (1) iso-P is a racemic metallocene of C 2 symmetry which catalyzes isotactic enchainment, (2) syn-P is an achiral bilaterally symmetric metallocene of C s symmetry which produces syndiotactic enchainment, (3) ata-P is an achiral symmetric metallocene of C 2v symmetry which favors atactic enchainment, and (4) hemi-P is a chiral asymmetric metallocene of C i symmetry which favors hemiisotactic enchainment.
Examples of iso-P metallocenes which may be used in the preparation of an isospecific propylene polymerization catalyst are as follows: rac-ethylenebis(1- η 5 -indenyl)dichlorozirconium (Cat. 2), rac-ethylenebis(1- η 5 -indenyl)-dimethylzirconium, rac-ethylenebis(1- η 5 -4,5,6,7-tetrahydro-indenyl)dichlorozirconium, rac-ethylenebis(1- η 5 -4,5,6,7-tetrahydroindenyl)dimethylzirconium, rac-dimethylsilyienebis(1- η 5 indenyl)dichlorozirconium (Cat. 1), rac-dimethylsilyienebis(1- η 5 - -indenyl)dimethylzirconium, rac-ethylenebis(1- η 5 -benz[e]indenyl)dichlorozirconium, rac-dimethylsilylenebis(1- η 5 -2-methyl- benz[e]indenyl)dichlorozirconium and rac-dimethylsilylenebis (2-methyl-4-napththyl(1- η 5 -indenyl) dichlorozirconium. The above metallocenes are arranged in the order of increasing stereoselectivity and decreasing chain termination. Therefore, in the preferred embodiment, the appropriate metallocene to produce isotactic polypropylene or other poly- α-olefin having the desired stereoregularity, melting transition temperature and molecular weight may be selected.
Examples of ata-P metallocenes which may be used in the preparation of the nonspecific propylene polymerization catalyst are as follows: bis-( η 5 -cyclopentadienyl)dichlorozirconium, bis-( η 5 -cyclopentadienyl)dimethylzirconium, ethylenebis(9η 5 -fluorenyl)dichlorozirconium (Cat.3) and dimethylsilylene, bis-(9η 5 -fluorenyl) dichlorozirconium. The above metallocenes are arranged to produce atactic polypropylene in the order of increasing activity and molecular weight.
Examples of syn-P metallocenes which may be used in the preparation of a syndiospecific propylene polymerization catalyst are as follows: isopropylidene(1- η 5 -cyclopentadienyl)(9- η 5 -fluorenyl)dichlorozirconium (4), isopropylidene-(1- η 5 -cyclopentadienyl)(9- η 5 -fluorenyl)dimethylzirconium, t -butylmethylidene(1- 5 -cyclopen tadienyl)(9-i 5 -fluorenyl)dichloro-zirconium and diphenylmethylidene(1- η 5 -cyclopentadienyl)(9- η 5 -fluorenyl)dichlorozirconium (Cat. 5). The above metallocenes are arranged in the order of increasing syndioselectivity and decreasing chain termination. Therefore, in the preferred embodiment, the appropriate metallocene to produce syndiotactic polypropylene having the desired properties may be selected.
In general, non-bridged zirconocene polymerize propylene with the lowest activity to lowest molecular weight product as pointed out by Kaminsky (in History of Polyolefins , Ed. Seymour et al., Reidel Publishing Co. 1986, pp.257-270), whereas the stereorigid C 2v compounds exhibit exceedingly high activity and produce a-PP having molecular weight of between half and one million.
Other aspecific propylene polymerization catalysts may be used which do not have the metallocene framework including dimethylsilylene(1- η 5 -2,3,4,5-tetra-methy-cyclopentadienyl) (t-butylamido) dichlorotitanium, 2,2′-thiobis(6-t-butyl-4-methylphenoxy)dichlorotitanium and monocyclopen tadienyl or nonoindenyl compounds of the formula LTiX 3 , where L=Cp or Ind, X=Cl, Me, OiPr, and also attached to the η 5 ring is a substituent containing an electron donating heteroatom selected from group VA elements.
Examples of hemi-P metallocenes which may be used in the preparation of a hemiisospecific propylene polymerization catalyst are as follows: rac-isopropylidene(l- η 5 -3-methylcyclopentadienyl)(9- η 5 -fluorenyl)dichlorozirconium, rac-isopropylidene(1- η 5 -cyclopentadienyl)(l- η 5 -indenyl)dichlorozirconium, and rac-isopropylidene(l- η 5 -cyclopentadienyl)(l- η 5 -3-methylindenyl)dichlorozirconium.
Examples of syn-S precursors which may be used in the preparation of a syndiospecific styrene polymerization catalyst are monopentahapto compounds of the formula LTiX 3 (Cat. 6 where L=Cp, Ind, or benz[e]indenyl with substituents selected from groups of hydrocarbyls having 1 to 20 carbon atoms and X=C 2 , Me, OiPr, benzyl. The lower valent analogs LTiX 2 are also active syn-S precursors.
Examples of ata-S precursors which may be used in the preparation of an aspecific polymerization catalyst to produce amorphous polystyrene are zirconium compounds L′ n ZrX 4-n , where L′=CP, η-Me 5 C 5 , n=1,2 and X=Cl, Me, O-i-Pr, benzyl.
In the present invention, ethylene is polymerized which is accompanied by rearrangement to form branched polyethylene having from a few to several hundred per 1,000 carbons, the branches are hydrocarbyls of one to ten carbon atoms. Propylene or higher α-olefin is polymerized with rearrangement to form branched polyolefin having 80 to 300 hydrocarbyl branches of one to 10-carbon atoms per 1,000 carbon of the macromolecule. Examples of catalysts which may be used in the preparation of branched polyethylene or branched polyolefin of this invention are exemplified with the following formulas:
These 1,4-diaza-1,3-butadien-2-yl complexes, commonly called α, β,-dimine complexes, of group VIIIB metal, where M=Pd, Ni; R=H or aliphatic hydrocarbyl of one to ten carbon atoms; Ar =aromatic hydrocarbyl or fluorohydrocarbyl of six to twenty carbon atoms; x=BR, Cl, O-i-Pr, R.
The cocatalyst of the catalyst composition of the present invention may comprise a wide variety of species which are known to abstract anionic ligands bound to group IVB or VIIIB transition metals.
Examples for neutral reducible Lewis acids which may be used in the preparation of the catalyst of the present invention are as follows: tris(pentafluorophenyl)borane, tris(ditrifluoromethylphenyl)borane, tris (2,2,2-perfluorobiphenyl) bonane.
Examples of Bronsted acids which may be used in the preparation of the catalyst are as follows: phenylammonium tetrakis(pentafluorophenyl)borate, diphenylammonium tetrakis(pentafluorophenyl)borate and tributylammonium tetrakis (pentafluorophenyl) borate.
Examples for the oxymetalloids which may be used in the preparation of the catalyst of the present invention are as follows: oligomers of methylaluminoxane (MAO), ethylaluminoxane, propylaluminoxane and butylaluminoxane.
The main rationale for the choice of a cocatalyst is the degree of interaction between the metallocene cation and the counter-anion, either by close approach for ion pair formation or via electron deficient-methyl bridges. Strong interaction tends to lower catalytic activity, selectivity, molecular weight, and most important of all, interference with the cross-over process. Therefore, the cocatalyst employed most frequently in this work is triphenylcarbenium tetrakis (penta-fluorophenyl)-borate described by Chien et al. J. Am. Chem. Soc. 1991, 113, 8570, which is free of the drawbacks of the other cocatalysts. It is designated hereinafter as the “Cocat” unless otherwise noted.
Using any of the above catalyst compositions as a single produces only a single kind of homopolymer. Using two of the above catalysts together, there is produced a mixture of two different homopolymers that are immiscible. Thus, the present invention provides a novel component cross-over agent. If any of the above catalysts employed are isospecific and/or aspecific, they produce individually and independently isotactic polypropylene and atactic polypropylene. In the presence of a cross-over agent, as provided for in the present invention, however, the product is a naturally compatible blend of the isotactic and atactic polypropylenes. A new substance is formed in the presence of the cross-over agent that is not formed in its absence. Its presence is established by fractionation of the product and 13 C NMR determination of the polymer microstructure. In the absence of the cross-over agent, solvent extraction results in two dominant fractions with NMR spectra characteristic for the isotactic and for the atactic polypropylene. In the presence of a cross-over agent, an additional fraction is isolated whose NMR spectra is clearly the sum of the isotactic and atactic sequence (FIG. 1 ). It is, therefore, a stereoblock copolymer (see U.K. Letters Patent No. 9102679.9). The same is true for the other polymerizations of the present invention whereupon the corresponding block polymers are formed.
The role of the cross-over agent is to transfer the propagating chain on one metal center carrying it to the other metal center and vice versa. Consequently, the next monomers inserted will have the respective stereodirecting influence of the new metal center.
Therefore, the catalyst composition of the present invention provides for the use of a cross-over agent selected from the group of hydrocarbyls and oxyhydrocarbys of group IIIA metal. Illustrative of the present invention, but not limiting examples are as follows: trimethylaluminum, triethylaluminum, tri-i-propylaluminum, tri-i-butylaluminum, compounds containing two or more Al atoms linked through heteroatoms such as: (C 2 H 5 ) 2 , Al—O—Al, H 2 ) 5 2 methylaluminoxane, ethylaluminoxane, butylaluminoxane, (C 2 H 5 )2 A 1 —N(C 6 H 5 )—Al(C 2 H 5 ) 2 —Al—O(SO 2 )—O—Al(C 2 H 5 ) 2 . Group IIA hydrocarbyls may also function in crossover capacity albeit with a lowered efficiency. Finally, in the absence of a cross-over agent, the chains belonging to different metal centers may interchange directly. This probably occurs to a noticeable degree only at very high catalyst concentration, which is not an economically viable condition. Consequently, the use of the cross-over agent is required for the direct “one-pot” synthesis of compatible polymer blends.
The outstanding properties of the polymers of the present invention can be readily shown by testing. The stress-strain curves in FIG. 2 a of the compatible isotactic/atactic blend of example 1 of the present invention shows that it increases in strength with strain up to 1100% elongation which is characteristic of a crosslinked elastomer. The α-PP (curve d) does not show any yield point, but a nearly perfect stress plateau until it breaks. This phenomenom is considered to be due to the high degree of entanglement in the high molecular weight atactic polymer. The application of the high extension rate of 1000% min. does not allow the material to disentangle in experimental time, and to flow. The solution casted blend of separately prepared isotactic and atactic polypropylene is a brittle substance without strength (curve c) indicating substantial macrophase separation in this specimen.
FIG. 3 illustrates the outstanding elasticity of the compatible blend by the hysteresis curves of tensile stress measurements. Note that the expansion curve returns to the previous stress at its previous maximum strain.
FIG. 4 gives the percentage of recovery of the compatibly blended material. Although the residual expansion of the specimen was increased at higher strain, the recovery rate of the compatibly blended polymer was consistent at 97-98% between 100% to 500% elongation, which is very high compared to other polymers of this type. In contradistinction either α-PP alone or blended with i-PP is virtually without elasticity.
Thermal and X-ray diffraction (XRD) data support the conclusion that the compatible polymer blend is morphologically different from the separately synthesized homopolymers. At the same isotactic polypropylene to atactic polypropylene ratio, the two types of materials have the same heat of fusion. The XRD of the latter blend (FIG. 5 b ), however, is seen to be a superimposed isotactic polypropylene on the amorphous halo indicating large size isotactic crystallites and macrophase separation. In contrast, the XRD of the directly synthesized compatible polymer blend of example 1 of the present invention (FIG. 5 d ) barely shows a hint of the a reflections. The reflections become resolved with a deconvolution analysis (FIG. 6 ). In other words the crystallite sizes are minute indicating phase boundary mixing through interpenetration of domains and there is only microphase separation.
The present invention applies to catalyst compositions to polymerize more than one monomer to prepare compatible blends of homopolymers and copolymers of terpolymers. Ethylene-selection catalyst [Ind-Si(Me) 2 -Ind]ZnCl 2 is used to homopolymerize ethylene in the presence of other olefinic monomers and olefin copolymerization catalyst Me 2 Si(Me 4 Cp)(M-t-butyl)TiCl 2 is used to copolymerize or terpolymerize ethylene with other olefins or dienes, respectively, with a common cocatalyst and cross-over agent. This catalyst composition provides for the “one-pot” direct synthesis of materials of projection 1 wherein A is polyethylene and B is ethylene-propylene copolymer, or ethylene-hexene copolymer, or ethylene-octene copolymer, or ethylene-propylene-ethylidene norbonene terpolymer, or ethylene-propylene-butadiene terpolymer, or ethylene-propylene- 1,4-hexadiene terpolymer.
The following examples specifically illustrate the present invention.
EXAMPLE 1
An isospecific and a nonspecific catalyst were employed in the polymerization. A 250 mL crown-capped glass pressure reactor with a magnetic stirring bar was first evacuated, flushed with argon, then charged with 50 mL of toluene. The system was evacuated again and saturated with propylene for ca. 20 min. to 15 psig. Tri-i-butyl aluminum (5 mM), rac-dimethylsilyienebis(1- η 5 -indenyl)dichlorozirconium (Cat. 1, 4 μM) and ethylenebis(9- η 5 -fluorenyl)dichlorozirconium (Cat. 3, 6 μM) were injected with syringe as toluene solutions. The system was heated to the desired temperature (T p ), stirred for ca. 20 additional min. to saturate it with propylene at this temperature. Finally a toluene solution of the cocatalyst (Cocat, 10 μM) was introduced to initiate the polymerization. Upon completion, the polymerization mixture was quenched with acidic methanol (containing 2% HCL), filtered, washed with methanol, and dried at 70° C. under vacuum to a constant weight 4.38 g of a thermoplastic elastomer was obtained.
A sample was fractionated using several solvents under refluxing conditions. Acetone did not dissolve any polymer, but diethyl ether extracted 50.7 wt % of polymer, which has the 3 C NMR of atactic polypropylene (FIG. 1 c ). Pentane and hexane did not dissolve any polypropylene. Refluxing heptane extracted 7 wt %, the NMR spectra of which (FIG. 1 b ) is that of an isotactic/atactic block copolymer. The remaining 42 wt % heptane insoluble materials are the isotactic polypropylene (FIG. 1 a ). The catalytic activity of polymerization was 7.3×10 7 g PP/(mol Zr.[C 3 H 6 ].h). The product has a peak melting transition of 149.3° C., heat of fusion ΔH f =11.5 cal/g.
EXAMPLES 2-15
Example 1 was repeated except that the conditions indicated in Table I were employed.
TABLE 1 a
A × 10 −7 g
ΔHf
[Cat 1]
[Cat 3]
[TIBA]
Yield
PP/(mol Zr ·
Tm
(cal/
(μM)
(μM)
(mM)
(g)
[C 3 H 6 ] · h)
(° C.)
g)
Exam-
ple
1
4
6
5
4.38
7.3
149.3
11.5
2
5
1.3
4
1.22
3.7
152.2
19.4
3
4
4
4
1.52
4.2
152.2
16.3
4
4
6
4
1.86
4.1
151.8
15.2
5
3
7
4
0.70
1.0
151.2
5.4
6
2
8
4
1.18
1.6
152.0
7.2
7
1
9
4
0.95
1.3
151.0
3.1
8
4
1
5
1.20
3.2
151.1
14.0
9
5
3.3
5
3.10
5.0
149.8
15.7
10
2
8
5
3.24
5.4
150.0
8.9
11
5
3.3
6
1.72
6.9
152.1
11.6
12
4
4
6
1.55
6.5
151.8
9.0
13
4
6
6
2.31
6.2
150.9
5.5
14
3
7
6
2.63
7.0
150.7
3.9
15
2
8
6
1.89
5.0
150.0
2.0
a P C 3 H 6 = 15 psig, Tp = 0° C., [Cocat] = [Cat 2] + [Cat 3].
EXAMPLE 16
An isospecific and a nonspecific catalyst were employed in the polymerization. A 250 mL crown-capped glass pressure reactor with a magnetic stirring bar was first evacuated, flushed with argon, then charged with 50 mL of toluene. The system was evacuated again and saturated with propylene for ca 20 min. to 15 psig. Tri-i-butyl aluminum (5 mM), rac-ethylenebis(1- η 5 -indenyl)dichlorozirconium (Cat. 2, 1 μM) and ethylenebis(9- η 5 -fluorenyl)dichlorozirconium (Cat. 3, 9 μM) were injected with syringe as a toluene solution. The system was heated to the desired temperature (T p ), stirred for ca. 20 additional min. to saturate it with propylene at this temperature. Finally a toluene solution of the cocatalyst (Cocat. 10 μM) was introduced to initiate the polymerization. Upon completion, the polymerization mixture was quenched with acidic methanol (containing 2% HCL), filtered, washed with methanol, and dried at 70° C. under vacuum. 1.6 g of a thermoplastic elastomeric polypropylene was obtained.
A sample was fractionated using several solvents under refuxing conditions. Acetone did not dissolve any polymer but diethyl ether extracted 90% wt which has 13 C NMR for atactic polypropylene polypropylene. Refluxing hexane extracted 10% wt the NMR spectra of which is that of an isotactic/atactic block copolymer. The catalytic activity of polymerization was 7.3×10 7 g PP/(mol Zr.[C 3 H 6 ].h). The product has a peak melting transition of 149.3° C., heat of fusion ΔHf=11.5 cal/g and is a very strong thermoplastic elastomer.
EXAMPLES 17-25
Example 16 was repeated except that the conditions indicated in Table II were employed.
TABLE II a
A × 10 −7 g
PP/
[Cat
[Cat
mol Zr ·
ΔHf
2]
3]
[TIBA]
Tp
Yield
[C 3 H 6 ] ·
Tm
(cal/
(μM)
(μM)
(mM)
(° C.)
(g)
h)
(° C.)
g)
Exam-
ple
16
8
2
5
0
1.91
2.1
147.7
7.4
17
6
4
5
0
2.73
3.0
146.3
4.6
18
4
6
5
0
2.47
2.7
146.0
2.2
19
2
8
5
0
2.87
3.2
145.5
1.2
20
1
9
5
0
1.60
0.7
145.3
0.5
21
6
4
5
25
4.55
8.4
141.2
8.2
22
4
6
5
25
4.33
8.0
140.5
5.7
23
3
7
5
25
5.10
9.5
138.9
3.9
24
2
8
5
25
5.34
9.9
137.9
2.7
25
1
9
5
25
5.84
10.8
135.7
0.9
a P C 3 H 6 = 15 psig, Tp = 0° C., [Cocat] = [Cat 2] + [Cat 3].
b TPE = thermoplastic elastomer; E = elastomer.
EXAMPLE 26
A syndiospecific and a nonspecific catalyst were employed in the polymerization. A 250 mL crown-capped glass pressure reactor with a magnetic stirring bar was first evacuated, flushed with argon, then charged with 50 mL of toluene. The system was evacuated again and saturated with propylene for ca. 20 min. to 15 psig. Tri-i-butyl aluminum (5 mM), diphenylmethylidene(1- η 5 -cyclopentadienyl)(9- η 5 -fluorenyl)dichlorozirconium (Cat. 4, 10 μM) and ethylenebis(9- η 5 -fluorenyl)dichlorozirconium (Cat. 3, 15 μM) were injected with syringe as toluene solution. The system was heated to the desired temperature (T p ), stirred for ca. 20 additional min. to saturate it with propylene at this temperature. Finally a toluene solution of the cocatalyst (Cocat, 10 μM) was introduced to initiate the polymerization. Upon completion, the polymerization mixture was quenched with acidic methanol (containing 2% HCL) filtered, washed with methanol, and dried at 70° C. under vacuum to give 3.43 g of thermoplastic elastomeric polypropylene.
The catalytic activity was 7.8×10 7 g PP/(mol Zr.(C 3 H 6 ].h). The TPE polypropylene product had a peak melting transition of T m =137.6° C. and heat of fusion of ΔH f =23.9 cal/g.
A sample was fractionated using several solvents under refuxing conditions. Acetone did not dissolve any polymer but diethyl ether extracted 65.7 wt % which has 13 C NMR for atactic polypropylene (FIG. 7 c ) with [rrrr]=0.11 and total for all other pentads=0.89. Pentane did not dissolve any polypropylene. Refluxing hexane extracted 5.5 wt % and refluxing heptane extracted 16.1 wt % of the sample. Their NMR spectra (FIG. 7 b ) is that of a syndiotactic/atactic block copolymer with [rrrr] =0.67 and total for all other pentads=0.33. The remaining 12.7 wt % heptane insoluble material is the syndiotactic polypropylene with [rrrr]=1.0 (FIG. 7 a ).
EXAMPLES 27-33
Example 26 was repeated except that the conditions indicated in Table III were employed.
TABLE III a
A × 10 −7
g PP/
[Cat
[Cat
mol Zr ·
ΔHf
2]
3]
[TIBA]
Tp
Yield
[C 3 H 6 ] ·
Tm
(cal/
(μM)
(μM)
(mM)
(° C.)
(g)
h)
(° C.)
g)
Exam-
ple
26
10
15
5
0
2.3
3.43
138.5
8.05
27
5
0
5
0
0.77
2.0
150.2
20.7
28
5
20
5
0
3.09
5.5
137.6
5.7
29
5
0
5
25
0.65
3.0
138.5
20.6
30
6
4
5
25
2.91
6.7
132.7
8.05
31
4
6
5
25
3.41
6.3
130.5
4.52
32
2
8
5
25
4.79
6.7
132.9
3.82
33
1
9
5
25
4.79
6.7
129.0
1.72
a P C 3 H 6 = 15 psig, [Cocat] = [Cat 5] + [Cat 3].
b sample not annealed prior to DSC scan.
EXAMPLE 34
A syndiospecific catalyst and an isospecific catalyst were employed in the polymerizations. A 250 mL crown-capped glass pressure reactor with a magnetic stirring bar was first evacuated, flushed with argon, then charged with 50 ml of toluene. The system was evacuated again and saturated with propylene for ca. 20 min. to 15 psig. Tri-i-butyl aluminum (5 mM), diphenylmethylidene(1- η 5 cyclopentadienyl)(9- η 5 -fluorenyl) dichlorozirconium (Cat. 5, 5 μM) and rac-ethylenebis(1η 5 -indenyl)dichlorozirconium (Cat. 2, 5 μM) were injected with syringe as toluene solution. The system was heated to the desired temperature (T p ), stirred for ca. 20 additional min. to saturate it with propylene at this temperature. Finally a toluene solution of the cocatalyst (Cocat, 10 μM) was introduced to initiate the polymerization. Upon completion, the polymerization mixture was quenched with acidic methanol (containing 2% HCl), filtered, washed with methanol, and dried at 70° C. under vacuum yielding 0.67 g of plastomer. The activity of polymerization was 3.4×10 7 g PP/(mol Zr.[C 3 H 6 ].h). The plastomer has a peak melting transition of T m =148.0° C. and ΔH f =20.7 cal/g. It has a rapid isothermal crystallization rate, the slope of which is only 0.2 mwatt/g/min at 30 min. The slope of isothermal crystallization rate for pure syndiotactic polypropylene and its 1:1 blend mixture with at 109.1° and 114.3° C., respectively, is 0.7 and 0.8 mwatt/g/min.
EXAMPLES 35-37
Example 34 was repeated except that the conditions indicated in Table IV were employed.
TABLE IV a
A × 10 −7 g
ΔHf
[Cat 1]
[Cat 5]
[TIBA]
Yield
PP/(mol Zr ·
Tm
(cal/
(μM)
(μM)
(mM)
(g)
[C 3 H 6 ] · h
(° C.)
g)
Exam-
ple
34
5
5
5
0.64
3.4
148.0
13.8
35
0
5
5
0.77
2.0
150.2
20.7
36
8
2
5
0.74
2.5
140.2
14.9
37
10
0
5
2.15
1.9
152.0
30.5
a P C 3 H 6 = 15 psig, T p = 0° C., [Cocat] = [Cat 1] + [Cat 4].
EXAMPLES 38-45
Methylaluminoxane was employed as the cocatalyst for examples 38 to 45. A 250 mL crown-capped glass pressure reactor with a magnetic stirring bar was first evacuated, flushed with argon, then charged with 50 mL of toluene. The system was evacuated again and saturated with propylene for ca. 20 min. to 15 psig. Tri-i-butyl aluminum (5 mM), rac-ethylenebis(1- η 5 -indenyl))dichlorozirconium (Cat. 2, 10 μM) and ethylenebis(9- η 5 fluorenyl)dichlorozirconium (Cat. 3, 40 μM) were injected with syringe as toluene solution. The system was heated to the desired temperature (T p ), stirred for ca. 20 additional min. to saturate it with propylene at this temperature. Finally a toluene solution of methylaluminum as the cocatalyst (100 mM) was introduced to initiate the polymerization. TIBA was omitted in examples 38 to 41. The conditions are as indicated in Table V. Upon completion the polymerization mixture was quenched with acidic methanol (containing 2% HCL), filtered, washed with methanol, and dried at 70° C. under vacuum to a constant weight.
TABLE V a
A × 10 −7
g PP/
[Cat
[Cat
mol Zr ·
1]
3]
[TIBA]
T p
Time
Yield
[C 3 H 6 ] ·
(μM)
(μM)
(mM)
[MAO] b
(° C.)
(min)
(g)
h)
Ex-
am-
ple
38
10
40
0
0
0
120
0.29
0.07
39
10
40
0
0
24
60
1.81
1.2
40
10
40
0
0
50
30
3.61
9.2
41
10
40
0
0
75
30
2.07
33.0
42
10
40
5
25
0
60
0.62
0.31
43
10
40
5
25
25
30
3.60
4.8
44
10
40
5
25
50
15
7.20
38.0
45
10
40
5
25
75
15
8.3
132.
a C 3 H 6 = 15 psig,
b MAO = methylaluminoxane
Products of examples 38 to 40 contain less than 2% by weight of diethylether insoluble-heptane soluble isotactic-atactic block copolymers, whereas the products of examples 42 to 44 contain about 10% of this fraction.
EXAMPLE 46
An isospecific catalyst (Cat. 1) and a rearrangement polymerization Cat. 7 (M=Ni, X=Br, Ar=2, 4.6—C 6 M 2 Me 3 ) were employed to polymerize and block copolymerize propylene. branching catalyst (Cat. 5) were employed to polymerize and block copolymerize propylene. In one Schlenk tube a solution of Cat. 2 and MAO were mixed one hour prior to use; another Schlenk tube was used to similarly preativate Cat. 5 with MAO. A 250 mL crown-capped glass pressure reactor with a magnetic stirring bar was first evacuated, flushed with argon and charged with 50 mL of toluene. The system was evacuated again and saturated with propylene for ca. 20 min. to 15 psig. Methylaluminoxane (5 mM) was introduced. Finally the two preactivated catalyst solutions were injected to initiate the polymerization. Upon completion, the polymerization mixture was quenched with acidic methanol (containing 2% HCL), filtered, washed with ethanol and dried at 700° C. under vacuum to a constant weight.
The product of example 46 was fractionated and 13 C NMR spectra determined. The diethyl ether soluble fraction is that of branched polypropylene which has very complicated s+t carbon resonances (FIG. 10 d ) and syndiotactic methyl resonances (FIG. 9 d ). (Table VI) The hexane and heptane soluble fractions are mainly low molecular weight isotactic polypropylene. The heptane insoluble fraction contains most of the block copolymer of branched and isotactic sequences.
TABLE VI a
13 C-NMR methyl region
Fraction of
[mmmm]
All other
13 C-NMR s and t
polymer of example 46
wt %
Figure
(%)
penthads (%)
carbon Figure
Acetone soluble
3.0
Diethyl ether soluble
27.5
9d
0
100
10d
Pentane soluble
0.3
Hexane soluble
2.0
9c
100
0
10c
Heptane soluble
16.1
9b
>90
<10
10b
Heptane insoluble
58.3
9a
24
76
10a
EXAMPLES 47-49
Example 46 was repeated except that the conditions in Table VII were employed.
TABLE VII a
A × 10 −7
g PP/
[Cat
[Cat
mol Zr ·
9]
1]
[MAO] b
[C 3 H 6 ] ·
T g
T m b
T m c
ΔH f
(μM)
(μM)
(mM)
h)
° C.
1° C.
2° C.
Cal g
Exam-
ple
46
200
20
220
6.9
−20
127.8
141.9
20.1
47
100
20
120
11.7
−20
127.8
142.3
27.9
48
50
20
70
15.4
−20
127.8
143.1
25.0
49
200
0
200
1.7
−35
—
—
—
C 3 H 6 = 15 psig, T p = 20° C.;
b Shoulder;
c peak melting temperature.
EXAMPLES 50-53
Example 46 was repeated except using ethylene as the monomer and the other conditions indicated in Table VIII. The products of example 51 and 52 were extracted with refluxing solvent and examined with 13 C NMR. The diethyl ether soluble fraction exhibits the 13 C NMR spectra of branched polyethylene. The hexane soluble fraction displays the 13 C NMR spectra of isomeric block copolymer. The spectra of the hexane insoluble fraction is that of linear polyethylene.
TABLE VIII a
A × 10 −7
[Cat 8]
[Cat 2]
[MAO] b
g PP/mol Zr ·
(μM)
(μM)
(mM)
[C 3 H 6 ] · h)
Example 50
25
0
120
1.0
51
25
10
60
2.0
52
10
10
30
1.8
53
0
10
30
1.7
a P C 3 H 6 = 15 psig [TIBA] = 0.5 mM b Cat 8 (M = Pd, R = Me, X = Br, An = O —C 6 H 4 Me.
EXAMPLE 54
Styrene was the monomer polymerized by a syndiospecific and a non-specific catalyst. A 250 mL crown-capped glass pressure reactor containing magnetic stirring bar was sealed under argon. Toluene (50 mL), styrene (5 mL), and MAO (0.2 M) were injected in that order and stirred for 10 min. η 5 -Idenyltitanium trichloride (50 μM) and zirconocene dichloride (5 mM) were then injected; the polymerization mixture was stirred for 0.5 hour and quenched by addition of 150 mL of 10% HCL in methanol. After filtration, washing, and drying, 1.2 g of polymer was obtained. The polymer was extracted with refluxing pentane; the 15 wt % polymer in this fraction is atactic polystyrene. The 2-butanone soluble pentane insoluble fraction (12 wt %) contained a stereoblock copolymer. The remaining 2-butanone insoluble material of 73 wt % is the syndiotactic polystyrene.
EXAMPLE 55
An ethylene-selective catalyst (6) which does not incorporate α-olefin is used to polymerize ethylene to linear polyethylene. It is the zirconium complex with the following bridging ligand,
The second catalyst component is Cat 1 or any other bridged metallocene compound selected from the lists of sio-P and syn-P above, which copolymerizes ethylene and α-olefin efficiently. A 250 mL crown-capped glass pressure reactor with a magnetic stirring bar was first evacuated, flushed with argon, then charged with 50 mL crown-capped glass pressure reactor with a magnetic stirring bar was first evacuated, flushed with argon, then charged with 50 mL of toluene and 10 mL of hexene, the system was evacuated again and saturated with ethylene for ca. 20 min. to 15 psig. Tri-i-butyl aluminum (5 mM), Cat 6 (5 μM) and rag-dimethylsilylenebis (1- η 5 4-idenyl) dichlorozirconium (Cat. 1,5 μM) were injected with syringe as toluene solution. The system was heated to 65° C., stirred for ca. 20 additional min. to saturated it with ethylene. Finally, a toluene solution of the cocatalyst (Cocat, 10 μM) was introduced to initiate the polymerization. Upon completion, the polymerization mixture was quenched with acidic methanol (containing 2% HCL), filtered, washed with methanol, and dried at 70° C. under vacuum yielding 0.55 g of flexomer. It has two T m 's at 138° C. and 116° C. Compared with the ordinary linear low-density polyethylene synthesized using Cat. 1 alone, the flexomer of this invention has higher dart impact strength and tensile modulus.
EXAMPLE 56
Example 55 was repeated except that 1-butene was the comonmer rather than 1-hexene and that MAO was employed as the cocatalyst. The activity of polymerization was 6.8×10 6 g polymer/(mol Zr.hr).
|
This invention relates to polymer blends and the process for preparing naturally compatibilized polyolefin blends using a “one-pot” polymerization of a single monomer, whereby two homopolymers having different structures are produced as well as a third block copolymer having alternating sequences of the two structural segments of the two homopolymers. The formation of the block copolymer is established by solvent extraction and 13 C-NMR spectroscopy. The catalyst compositions enabling the direct synthesis of naturally compatibilized polymer blend is prepared by combining four components. The first two components are organometallic complexes of Group IVB or VIIIB elements. The third component is a cocatalyst which irreversibly reacts with at least one ligand on the transition metal complexes. The fourth component is a hydrocarbyl or oxyhydrocarbyl compound of Group IIIA metals, which functions as a cross-over agent.
| 1
|
BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention relates to a novel, highly effective attractant and mating control agent for the bagworm moth, Thyridopteryx ephemeraeformis (Haworth), and more particularly to synthetic 1-methylbutyldecanoate and its use as an attractant, a mating control agent and plant protectant.
2. Description of the Art
Attractants for a number of species of insects, such as those for the pink bollworm moth and for the yellow jacket, are known and some of them have been used to determine the period of mating behavior by trapping the male insects. They have also been used to disrupt the mating pattern of insects and suppress, but not control completely, the insect population.
SUMMARY OF THE INVENTION
An object of this invention is to provide a synthetic attractant for the adult male bagworm moth.
Another object is to provide a mating control agent for the bagworm moth.
Still another object is to provide a method of protecting plants from being damaged by bagworm moths.
A further object is to provide a method of suppressing the number of female bagworm moths that are mated.
A still further object is to provide a method of inhibiting completely the mating of all female bagworm moths in a selected area.
In general, the above objects are accomplished by the sex attractant, synthetic racemate 1-methylbutyldecanoate and its use as an attractant for male bagworm moths. The objects are further accomplished by applying the synthetic racemate, 1-methylbutyldecanoate, to trees and shrubs in a selected area in amounts effective to suppress or inhibit completely the mating of female bagworm moths in the treated area.
DESCRIPTION OF THE INVENTION
Landscape ornamental shrubs and trees increase greatly in value as they mature and complement the area of placement. Therefore, it is important to protect them from insects that defoliate or otherwise damage the trees and shrubs. The bagworm moth is the single most important defoliator of ornamental conifers such as juniper, arborvitae, spruce and Eastern white pine in the eastern half of the United States. Although chemical pesticides can be effective, their use is objected to in many urban residential areas and in landscaped shopping centers.
Females of most lepidopteran species attract conspecific males for reproduction by emitting a sex attractant pheromone. If the active component(s) of the pheromone is isolated and identified, the compound(s) can be used as a lure in a trap to attract and catch the male of the species. However, a very real and serious deterrent to the use of a natural pheromone is the difficulty in isolating the active material and the extremely limited amount of material that is obtained.
We isolated and identified the single compound in the female bagworm moth sex pheromone as 1-methylbutyldecanoate and determined that the R enantiomer was active while the S enantiomer was inactive as a sex attractant. We also discovered that S enantiomer does not inhibit or interfere with the attractant or the plant protectant functions of the R enantiomer. This is unusual because with known insect pheromones the antipode to the active enantiomer is inhibitory to the functions of the active enantiomer. This discovery is important because it allows the use of the synthetic racemate and eliminates the need to synthesize only the R enantiomer.
Pupae were hand collected from infested conifers in the vicinity of Beltsville, Md. and were separated to sex. The females were isolated individually in 60×15 mm petri dishes and incubated at 25°-26° C. to wait emergence. Adult females, when ready for mating, rupture the anterior end of the pupal case and extend only the head and thorax. At this time the female actively sheds deciduous setae or hairs to the bottom of the bag in which they are housed. Hairs expelled by the females were aspirated onto a plug of glasswool in a pipette and washed with 50 ml hexane. The extract was concentrated and injected onto a gas chromatographic (GC) column packed with 4% SE-30 on 80/100 mesh silica. The major constituent in the extract was trapped and found to be biologically active and was purified by gas chromatography.
Capillary GC was carried out using polar and apolar 60 meter×0.25 mm (ID) fused silica columns. Low-resolution GC-MS (mass spectroscopy) showed a molecular ion at m/e 242 (C 15 H 30 O 2 ) and intense ions at m/e 173 and 155; high-resolution MS established that these ions were C 10 H 21 O 2 and C 10 H 19 O, respectively. No reaction occurred on treatment with O 3 , NaBH 4 , or acetic anhydride/pyridine; thus olefin, aldehyde, ketone or alcohol functionalities for the compound were excluded. The infrared spectrum showed absorption at 1745 cm -1 , compatible with C═O absorption of an ester. Reduction of a few μg of the compound at 250° C. with Pt and LiAlH 4 [B. A. Bierl-Leonhardt and E. D. deVilbiss, Anal. Chem. 53, 936, 1981] yielded n-pentane, according to GC-MS. Without Pt, a similar reduction at 300° C. gave n-decane and n-pentane. The nuclear magnetic resonance spectrum of the compound showed a triplet at 2.3 ppm (CH 2 C═O) and multiplet at 4.9 ppm (CHO).
The natural ester (ca. 1 μg) was reduced with LiAlH 4 in CCl 4 and the resulting 2-pentanol was derivatized with Mosher's reagent [J. A. Dale, D. L. Dull and H. S. Mosher, J. Org. Chem. 34, 2543, 1969]. The GC retention time of this diastereomeric derivative was identical to that of the Mosher's derivative of authentic (R)-2-pentanol.
GC analysis of the diastereomers of the optically active alcohols used in synthesis of the enantiomers of the pheromone showed that each optical isomer of the alcohol contained 2% opposite enantiomer. Field tests were conducted in two open fields at the Beltsville Agriculture Research Center, Beltsville, Md.
Behavioral response assays were conducted in field tests. Male bagworm responses to the enantiomers and racemate of 1-methylbutyldecanoate were evaluated on cotton rolls or to a virgin female placed in wing sticky insect traps positioned 20 meters apart, 1.5 meters from the ground, and baited daily. The test was replicated 5 times on each of 5 days in mid-September, 1981, near Beltsville, Md. using a randomized complete-block design. The traps baited with 500 μg R enantiomer captured males at about the same rate as traps baited with 1000 μg racemate (Table 1). The small number of males attracted to the S enantiomer were most likely responding to the trace of R in the S isomer.
In tests for suppression or control, 5 to 6 ft arborvitae trees supported by soil in individual bushel baskets were placed along the perimeter of the field at 60 meter intervals. Individual bags of ten female pupae were secured at the apical tip with paper binder clips and secured to each tree with wire. Treated trees were decorated each with a spiral of plastic ribbon containing the racemic 1-methylbutyldecanoate. Ribbons were removed every four days and replaced with new ribbon.
The 1-methylbutyldecanoate in a crude extract of the females' pheromone-laden hairs was assayed by GC and field tested versus the same amount (5.5 μg/trap) of synthetic racemate. The number of males captured in traps baited with this extract was not different from those baited with the synthetic racemate. Thus, the superiority of the synthetic racemate over females in causing male capture, Table 1, is attributed to the comparatively small quantity of pheromone produced by the female.
The synthetic pheromone, is a racemic mixture, half of which is the same as the natural pheromone. The racemate is easy to synthesize and has the same attractant properties as the natural pheromone. Another great advantage of the synthetic racemate is the low production cost. Synthesizing the active component of the natural pheromone requires the optically pure alcohol which is considerably more expensive than its racemic form. As described above, isolating and purifying the active component of the natural pheromone is a time consuming and an expensive task.
Field tests were conducted as described above. Mating suppression as measured by the relatively few mated females was achieved with 1.2 grams of synthetic racemate per tree for 7 days, Table 2. A second test which showed a high degree of mating suppression on individual host plants was obtained with 1.2 grams of synthetic racemate per host plant for 17 days. Data from the second test indicates suppression occurred on control plants as well, Table 3. Complete control of mating occurred when each infested tree within the treatment area was similarly treated with 1.2 grams of synthetic racemate, Table 4.
TABLE 1______________________________________Male Thyridopteryx ephemeraeformis responses in field bioassayto racemate and R and S enantiomers of 1-methylbutyldecanoateidentified from discharged hairs from the female.Treatment.sup.1 -x male capture/trap/day.sup.2______________________________________500 μg R 27.3 a1000 μg racemate 24.6 a100 μg racemate 7.3 b50 μg R 4.1 b1 virgin female 3.0 c500 μg S 2.1 cd.sup.350 μg S 0.2 e______________________________________ .sup.1 Each enantiomer contains 2% of the opposite antipode. .sup.2 Means followed by the same letter are not significantly different from each other according to Ducan's New Multiple Range Test. .sup.3 Male responses to S enantiomer treatments were due to 2% R in the enantiomer.
TABLE 2______________________________________Mating suppression of female bagworm mothwith racemic 1-methylbutyldecanoate.sup.1 Mated Calling LiveTreatment.sup.2 Females Female Pupa Total______________________________________Racemic 0 23 17 401-methylbutyldecanoateControl 8 11 21 40______________________________________ .sup.1 September 18 through 24, 1981 (7days). .sup.2 Four of eight trees were decorated with a ribbon 0.25 in wide × 192 in long containing 25.0 mg (+,-) per in.sup.2 or 1.200 g (+,-). Trees were spaced at 60 meter intervals at one field.
TABLE 3______________________________________Mating suppression of the female bagworm mothwith racemic 1-methylbutyldecanoate.sup.1 Mated Calling; Calling; Dead Live Miss-Treatment.sup.1 Females Unmated Died Pupa Pupa ing______________________________________Racemic 6 22 57 10 0 51-methyl-butyl-decanoateControl 18 23 40 14 4 4______________________________________ .sup.1 September 8 through 24, 1982 (17 days). .sup.2 The test was conducted at 2 locations with 5 replicates each. In each replicate 10 unmated female pupae were attached to each host plant. One half of the plants were treated and decorated with a ribbon 0.25 in wide × 264 in long containing 17.5 mg (+,-) per in.sup.2 or 1.155 g (+,-). The minimum distance between plants was 60 meters.
TABLE 4______________________________________Mating control of the female bagworm mothwith racemic 1-methylbutyldecanoate.sup.1 Mated Calling; Calling; Dead Live Miss-Treatment.sup.1 Female Unmated Died Pupa Pupa ing______________________________________Racemic 0 7 41 49 3 01-methyl-butyl-decanoateControl 30 3 8 57 1 1______________________________________ .sup.1 September 27 through October 21, 1982 (25 days). .sup.2 Approximately 1 mile between treated and untreated. Each treatment included ten replicated host plants each with 10 pupae attached. Treated plants were 60 meters apart and similarly decorated with a ribbon 0.25 in wide × 192 in long containing 25 mg (+,-) per in.sup.2 or 1.2 g (+,-).
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The racemate of 1-methylbutyldecanoate is synthesized and found to be a powerful attractant under field conditions for male bagworm moths. It is also found to suppress or inhibit completely the mating of female bagworm moths when applied to trees and shrubs in an effective mating suppressant or inhibiting amount.
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CROSS REFERENCE TO RELATED APPLICATIONS
[0001] This application is a division of application Ser. No. 09/542,108, Rolled Bun Candle filed Apr. 4, 2000, and Method and Device for Producing a Rolled Bun Candle Ser. No. 09/683,672, filed concurrently herewith and incorporated by reference herein as if set forth in full.
BACKGROUND OF INVENTION
[0002] The fundamental process of making wax candies has continued virtually unchanged for more than a century, and thus requires no detailed description. However, it is desirable to develop new methods of imparting novel and aesthetically pleasing characteristics to the basic candle structure.
[0003] The present invention satisfies this need by allowing the formation of an ornamental candle of a type for which no practical method has previously existed. The present invention involves the formation and rolling of a shaped layer of candle wax to create an aesthetically appealing candle product. The candle product, hereinafter the rolled candle, is composed primarily of what one skilled in the art would recognize as a base wax.
SUMMARY OF INVENTION
[0004] In a preferred embodiment of the present invention, a method for manufacturing a shaped, rolled candle is presented. First, wax of an appropriate color and character is obtained, and is then heated until the wax is in a sufficiently liquid state. The hot, liquid wax is then poured into a substantially horizontal tray of an appropriate shape, having a first and second end. The tray preferably has an elongated base portion, first and second substantially vertical side wall portions, and first and second substantially vertical end wall portions.
[0005] The elongated base portion should be inclined such that the first end is elevated relative to said second end. The angle of incline may vary depending on the desired shape of the final rolled product, but should generally be less than 10 degrees. The first substantially vertical side wall is preferably tapered from the first end to the second end such that the separation between the first and second substantially vertical side walls is less at the second end than at the first end. The amount of taper will also vary depending on the desired shape of the final product, but will generally be less than 10 degrees. The second substantially vertical end wall may be angled so as to soften the angle of the visible end of the rolled product.
[0006] The hot candle wax is then poured into the tray. The amount of wax poured into the tray is preferably controlled such that the finished wax panel is of a particular thickness. A difference in thickness of {fraction (1/16)} of an inch could result in the finished product being an inch wider than desired after rolling. The wax is then allowed to cool, forming a shaped wax layer, and removed from the tray. The shaped wax layer is then prefer-ably rolled starting at the wide end and ending with the narrow end on the outside of the roll. It is preferred that one of the elongated edges of the shaped wax layer is kept even with each roll so as to produce a substantially planar edge of the roll which may be used as a flat bottom of the candle.
[0007] It may be necessary during any of these steps to reheat portions or all of the candle wax. This reheating may be necessary to help shape the wax, improve the workability of the wax, or improve the adhesion between rolled layers. The edges of the shaped wax layers may be rounded prior to rolling. This gives the final product a more rounded, doughy look than it may otherwise have with rectangular edges. A candlewick is then inserted into the candle using methods known or used in the art.
[0008] The wick is preferably inserted in the bottom center of the wax candle and pulled up through the candle center until a portion of the wick extends outward beyond the top center of the candle. The wick may then be cut to a desired length. Heated wax may be dripped on the top surface of the rolled candle. This dripped wax not only fills in gaps in the rolled layers, but also gives the appearance of a layer of icing on the rolled bun candle. The dripping wax is preferably a white wax, in order to improve the appearance of the icing upon cooling.
[0009] The candle product may also be sprinkled with a powdered, shaved, or granular substance. The substance may be sprinkled in the tray prior to pouring of the wax, on the wax layer prior to rolling, and/or on the rolled candle. The substance may be any appropriate substance of a desirable appearance and/or scent, such as cinnamon, sugar, flour, chocolate shavings, candied sprinkles, scented pellets, or spices.
[0010] In addition to the novel features and advantages mentioned above, other objects and advantages of the present invention will be readily apparent from the following descriptions of the drawings and preferred embodiments.
BRIEF DESCRIPTION OF DRAWINGS
[0011] [0011]FIG. 1 is a perspective view of a rolled candle that may be used in accordance with the present invention.
[0012] [0012]FIG. 2 is another perspective view of a rolled candle that may be used in accordance with the present invention.
[0013] [0013]FIG. 3 is a perspective view of a shaped tray for molding candies that may be used in accordance with the present invention.
[0014] [0014]FIG. 4 is a perspective view of a partially rolled wax layer that may be used in accordance with the present invention.
[0015] [0015]FIG. 5 is another perspective view of a rolled candle that may be used in accordance with the present invention.
DETAILED DESCRIPTION
[0016] The present invention is directed to a method for the manufacture of an ornamental, but functional wax candle having a unique and attractive outer surface, specifically having the appearance of a rolled bun.
[0017] [0017]FIG. 1 illustrates an example of a candle 1 produced by a method of the present invention. The candle is created by rolling a shaped, elongated wax layer. The elongated wax layer has a first end 2 and a second end 3 . The layer is shaped so that the first end 2 is wider than the second end 3 . The first end 2 is also thinner than the second end 3 . As such, when the layer is rolled starting with the first end 2 , the resulting candle will be taller in the center than at the outer edge, and the layer will widen as it approaches the outer edge, simulating the appearance of a baked rolled bun. The candle 1 also has a wick 4 at its center.
[0018] [0018]FIG. 2 shows the candle I produced by the present invention after having additional adornments placed upon it. The candle 1 is shown with an additional layer of wax 5 a dripped on its surface. This second wax layer 5 a, preferably comprised of a white wax, gives the appearance of icing on the rolled bun candle. The candle is preferably also sprinkled with cinnamon 5 b or any other appropriate substance to enhance its appearance. The candle may also have wax nuts 6 or other adornments, such as wax apples or blueberries, sprinkled on its surface for adornment. The candle may be packaged in any appropriate manner, such as by placing on a tin plate and shrink-wrapping the combination.
[0019] The shaped tray 7 used to mold the rollable wax layers of the present invention is shown in FIG. 3. The tray has a first end 8 and a second end 9 . The tray also has a surface on the bottom of the mold 10 that inclines from the second end 9 to the first end 8 . The resulting wax layer formed by the molding tray, assuming the tray is positioned substantially horizontal, will then be thicker at the second end 9 than at the first end 8 .
[0020] The tray also has a first side 11 and a second side 12 , each being substantially vertical. The first side 11 preferably includes a tapered region 13 , either as part of or attached to the first side 11 . The tapered region 13 preferably results in the molded wax being narrower at the second end 9 of the mold than at the first end 8 .
[0021] The method for making a candle of the present invention preferably involves first heating appropriate candle wax until in a sufficiently liquid state. A shaped tray of the present invention is preferably sprinkled with cinnamon or other similar substance, then the heated wax is poured into the tray. The tray may be either designed so that excess wax runs over at least one of the edges of the tray, or may have marks designating the proper wax level. The level of wax is important, as an extra {fraction (1/16)} inch of thickness in the wax layer can result in candles that are an inch thicker after rolling. This excess thickness may not only cause packaging problems, but raises the production cost of the candle.
[0022] As the wax starts to cool in the tray, the cinnamon or other substance is preferably again sprinkled on the wax layer, preferably putting most of the substance near the edge that will eventually be at the top of the candle. Once the wax has cooled enough to be handled as a solid, but is still pliable and workable, the wax layer may be removed from the mold and preferably laid on a flat surface. If needed, the wax can be reheated to an appropriate temperature and workability, such as by passing a propane torch over the length of the layer. The edges of the candle are then preferably rounded, such as by manually pressing on the rough edges.
[0023] The wax layer may then be rolled into the desired shaped candle, as shown in FIG. 4. Starting at the wide end 15 , the wax layer 14 is rolled at an appropriate speed, attempting to keep the edge that will become the bottom of the candle even, such that a substantially planar bottom will result. During the rolling process, the wax layer may be reheated as needed. When the roll gets to the narrow end 16 , the narrow end 16 is preferably reheated to ensure acceptable adhesion and prevent the candle from unraveling.
[0024] Once the candle has been rolled, it is preferably rotated and set on its bottom side. At this point, a candle wick is preferably inserted in the center of the candle from the underside of the candle. The top side of the candle may again be reheated, and an additional layer of the cinnamon or other substance preferably sprinkled on the top of the candle. A second wax, preferably a vanilla or other substantially white wax, may then be dripped on the surface of the candle. This second wax is allowed to fill any gaps in the candle roll, and also gives the appearance of icing on the rolled bun candle upon cooling. The candle may also have molded wax adornments placed upon it, such as wax nuts, apples, blueberries, or raisins. The surface of the candle may require reheating to improve adhesion of the wax.
[0025] As shown in FIG. 5, the candle may also be placed in ajar 18 , bottle, or other wax-appropriate container. For a candle placed in ajar 18 , a rectangular wax layer is preferably placed inside the jar and formed into a ring or circular structure. A flexible wax ring or other similar wax structure may also be used. It is preferred that the outer edge of the ring substantially contact the inner surface of the jar. The ends of the wax layer may be beveled, thereby improving the rolled appearance of the final product. This outer ring may often be desirable, as the mouth of a container such as a jar may be smaller than the inner body of the container. Then, in order to give the impression that the rolled candle fills the jar, the ring may be inserted to give the appearance of an outer layer of the rolled candle.
[0026] A thin rolled wax disc may then be inserted into the jar. The wax disc is preferably formed by rolling a thin, elongated rectangular wax piece so as to form a wax disc having a rolled appearance. The thin rolled disc is preferably of such a diameter as to fill the opening inside the wax ring at the bottom of the jar. The rolled layer is preferably no thicker than about one inch, to facilitate handling. The wax disc may then be rotated so that the outer end of the roll forming the disc substantially contacts the junction of the ends of the wax layer forming the ring. This improves the continuous roll appearance of the final product, It is preferred to use this thin wax disc, as it is easier to rotate the small disc inside the wax ring inside the jar than to rotate a larger rolled candle that substantially contacts the inner surface of the wax ring.
[0027] A rolled candle as described previously may then be inserted into the jar. The rolled candle is preferably of an appropriate diameter to substantially contact the inner surface of the wax ring. The rolled candle preferably sits on the thin rolled wax disc, and has an edge height such that the edges of the rolled candle are at or above the height of the surrounding wax ring. The candle may optionally sit directly on the bottom of the jar, if the thin wax layer is not used. The candle may then be rotated as described above to enhance the rolled appearance.
[0028] The rolled wax layer at the outer edge is preferably of a width similar to the thickness of the wax ring. The rolled candle preferably has a wick at its center, and preferably increases in height towards the center of the candle. The candle may have adornments similar to those described above. Each rolled candle preferably also has a warning label on its bottom side or the bottom of the container with candle safety instructions.
[0029] Another method of producing a contained rolled candle involves producing a rolled candle as described previously, and then placing the candle in ajar or other, appropriate container. The candle is preferably placed into the jar while the candle is still at an elevated temperature. The candle may then expand as it cools to fill the jar.
[0030] A method for simulating a contained rolled candle involves pouring or injecting liquid candle wax into an appropriate container. Once the wax is in the container, and while it is still in a fluid state, a mold may be inserted into the container onto the surface of the wax. The mold may be adapted to expand or uncoil once in the jar so to fill the entire inner area of the jar. A wick may also be inserted, preferably either before injecting the wax or while the wax is still sufficiently fluid. The mold is preferably of such a shape as to create a rolled appearance to the top of a candle removed from the mold. The mold is preferably held in place for an amount of time and with an amount of force sufficient to allow the wax to settle into the mold and sufficiently retain its shape after removal of the mold. The time needed may depend upon the type of wax used or the initial temperature of the wax, among other factors. Once the wax has cooled to a sufficiently solid body, the mold may be removed from the wax. A resultant candle should then give the appearance of having been rolled from a single layer of wax.
[0031] Another method for simulating a rolled candle in ajar involves pouring or injecting liquid candle wax into an appropriate container. A rolled wax layer or a molded wax layer having a rolled appearance may then be placed upon the surface of the candle wax. This may be done after the candle wax has sufficiently cooled, or while the wax is still primarily in a liquid state. The diameter of the wax layer is preferably approximately equal to the diameter of the container opening. When the wax layer is placed on the surface of the injected candle wax, the resultant candle will appear to extend continually from the top of the wax layer to the bottom of the container.
[0032] Another method for simulating a rolled candle in ajar involves inserting a rolled wax layer into the jar such that it sufficiently contacts the inner circumference of the jar. Heated candle wax is then poured or injected into the area inside the wax ring, preferably filling the open area. A wick may also be inserted, preferably either before injecting the wax or while the wax is still sufficiently fluid.
[0033] In a preferred container, where the inner diameter of the body of the container is greater than the inner diameter of the mouth of the container, the candle wax may also give the appearance of another outer layer of the candle. It is preferred that the container be transparent, and have a lid that will sufficiently prevent the aroma of the candle from escaping the container when sealed. The lid may be decorated with any appropriate designs or adornment, and may be of any appropriate material.
[0034] The preferred embodiments herein disclosed are not intended to be exhaustive or to unnecessarily limit the scope of the invention. The preferred embodiments were chosen and described in order to explain the principles of the present invention so that others skilled in the art may practice the invention. Having shown and described preferred embodiments of the present invention, those skilled in the art will realize that many variations and modifications may be made to affect the described invention. Many of those variations and modifications will provide the same result and fall within the spirit of the claimed invention. It is the intention, therefore, to limit the invention only as indicated by the scope of the claims.
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A rolled candle giving the appearance of a rolled or sticky bun is presented. Also included in the invention are methods and devices for producing same. An elongated wax layer is formed, having a somewhat wide, thin end and a somewhat narrow, thick end. After adding a wick to the wider end, the candle is rolled from the wide end to the narrow end. The resulting rolled candle may then have additional adornments added, such as sprinkled cinnamon, vanilla wax to simulate icing, and wax nuts. The candle may also be formed or placed in a jar or other appropriate container.
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CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] This application is a continuation of co-pending U.S. application Ser. No. 13/308,146 filed on Nov. 30, 2011, which is a continuation of U.S. application Ser. No. 12/438,808 filed on Feb. 25, 2009, now U.S. Pat. No. 8,404,566, issued Mar. 26, 2013, which is the national phase of PCT international Application No. PCT/KR2007/004587 filed on Sep. 20, 2007, and which claims priority to Korean Patent Application No. 10-2006-0092732 filed on Sep. 25, 2006. The entire contents of all of the above applications are hereby incorporated by reference.
DESCRIPTION
[0002] 1. Technical Field
[0003] Embodiments relate to a light emitting diode and a method for manufacturing the same.
[0004] 2. Background Art
[0005] Light emitting diodes (LEDs) are manufactured through a scribing process of separating a plurality of unit chips after forming a compound semiconductor on the substrate.
[0006] The scribing process is to irradiate laser onto a substrate or a compound semiconductor. The substrate or the compound semiconductor, which is adjacent to a scribing region irradiated with the laser, may be damaged during the laser irradiation.
[0007] A portion of light generated from an active layer of the LED is emitted to the outside through the scribing region. However, it is difficult for light to pass through a portion of the substrate or the compound semiconductor damaged by the laser, which degrades light efficiency of the LED after all.
DISCLOSURE
Technical Problem
[0008] Embodiments provide a light emitting diode (LED) and a method for manufacturing the same.
[0009] Embodiments provide an LED with improved light efficiency and a method for manufacturing the same.
Technical Solution
[0010] An embodiment provides a method for manufacturing a light emitting diode (LED), comprising: forming a semiconductor layer; forming a mask layer on the semiconductor layer; irradiating laser onto a scribing region of the mask layer to divide the semiconductor layer into a plurality of light emitting diodes; etching the scribing region; removing the mask layer; and separating the plurality of light emitting diodes.
[0011] An embodiment provides a method for manufacturing a light emitting diode, comprising: forming a semiconductor layer on a substrate; forming a mask layer on the semiconductor layer; irradiating laser onto a scribing region of the substrate to divide the substrate into a plurality of light emitting diodes; etching the scribing region; removing the mask layer; and separating the plurality of light emitting diodes.
[0012] An embodiment provides a light emitting diode comprising: a substrate; a semiconductor layer on the substrate; and an electrode on the semiconductor layer, wherein the substrate or the semiconductor layer has at least one etched side surface having a predetermined tilt angle.
[0013] The details of one or more embodiments are set forth in the accompanying drawings and the description below. Other features will be apparent from the description and drawings, and from the claims.
Advantageous Effects
[0014] Embodiments can provide a light emitting diode (LED) and a method for manufacturing the same.
[0015] Embodiments can provide an LED with improved light efficiency and a method for manufacturing the same.
DESCRIPTION OF DRAWINGS
[0016] FIGS. 1 to 6 are sectional views illustrating a light emitting diode (LED) and a method for manufacturing the same according to a first embodiment.
[0017] FIGS. 7 to 11 are sectional views illustrating an LED and a method for manufacturing the same according to a second embodiment.
MODE FOR INVENTION
[0018] Reference will now be made in detail to a light emitting diode (LED) and a method for manufacturing the same, examples of which are illustrated in the accompanying drawings.
[0019] FIGS. 1 to 6 are sectional views illustrating an LED and a method for manufacturing the same according to a first embodiment.
[0020] Referring to FIG. 1 , a semiconductor layer 20 , a first electrode 31 and a second electrode 41 are formed on a substrate 10 so as to form an LED.
[0021] The substrate 10 may include, for example, a sapphire substrate. The semiconductor layer 20 has a multi-stacked structure of a compound semiconductor, which will be more fully described in FIG. 6 later.
[0022] A portion of the semiconductor layer 20 may be selectively etched, and the first electrode 31 is formed on an etched portion of the semiconductor layer 20 . Accordingly, heights of the first and second electrodes 31 and 41 differ from each other even though they are formed on the same semiconductor layer 20 .
[0023] The embodiment of FIGS. 1 to 6 illustrates sectional views for convenience in description, which illustrate processes of forming first, second and third LEDs 51 , 52 and 53 .
[0024] Referring to FIG. 2 , a mask layer 60 is formed on the semiconductor layer 20 , the first electrode 31 and the second electrode 41 .
[0025] The mask layer 60 protects the semiconductor layer 20 during a scribing process, and is formed of a material which can be wet-etched or dry-etched. A material for used in the mask layer 60 will be described in detail later.
[0026] In FIG. 2 , reference numeral 61 denotes a scribing region. In this embodiment, laser is irradiated onto the scribing region 61 using a laser irradiation apparatus, thus dividing the semiconductor layer 20 into the first, second and third LEDs 51 , 52 and 53 .
[0027] Referring to FIG. 3 , when the laser is irradiated onto the scribing region 61 , the mask layer 60 , the semiconductor layer 20 and the substrate 10 in the scribing region 61 are removed.
[0028] During laser irradiation, the layers in the scribing region 61 onto which the laser is irradiated are damaged, causing a damaged region 12 with a rugged surface to be formed, as illustrated in FIG. 3 .
[0029] The light emitted from the active layer of the LED does not pass through but is absorbed at the damaged region 12 , and thus the damaged region 12 is removed so as to improve light efficiency of the LED in this embodiment.
[0030] The removal of the damaged region 12 may be performed using wet etching or dry etching process.
[0031] The wet etching process is performed using a first etchant including at least one of hydrochloric acid (HCl), nitric acid (HNO 3 ), potassium hydroxide (KOH), sodium hydroxide (NaOH), sulfuric acid (H 2 SO 4 ), phosphoric acid (H 3 PO 4 ) and aluetch (4 H 3 PO 4 +4 CH 3 COOH+HNO 3 ). A temperature of the first etchant is between 200° C. and 400° C.
[0032] The mask layer 60 prevents the semiconductor layer 20 from being etched during the etching of the damaged region 12 . The mask layer 60 may be formed of, for example, silicon nitride (Si 3 N 4 ) or an oxide-based material such as silicon oxide (SiO 2 ), which is hardly etched by the first etchant.
[0033] That is, the first etchant has a higher etch selectivity to the damaged region 12 than to the mask layer 60 .
[0034] Since the mask layer 60 is hardly etched by the first etchant, the damaged region 12 can be selectively etched while minimizing the etch amount of the semiconductor layer 20 .
[0035] The dry etching may be performed through an inductively coupled plasma /reactive ions etcher (ICP/RIE) or an RIE. In addition, the dry etching may be performed using a first etching gas including at least one of BCl 3 , Cl 2 , HBr and Ar.
[0036] The mask layer 60 configured to prevent the semiconductor layer 20 from being etched during the etching of the damaged region 12 may be formed of an oxide-based material such as SiO 2 , TiO 2 and ITO or a metallic material such as Cr, Ti, Al, Au, Ni and Pt, which is hardly etched by the first etching gas.
[0037] That is, the first etching gas has a higher etch selectivity to the damaged region 12 than to the mask layer 60 .
[0038] The wet etching and the dry etching may be performed for several minutes to several tens of minutes depending on etching environments. FIG. 4 illustrates that the damaged region 12 of the scribing region 61 is removed.
[0039] Referring to FIG. 5 , the mask layer 60 formed on the semiconductor layer 20 is removed after the removal of the damaged region 12 .
[0040] The removal of the mask layer 60 may be performed using at least one of the wet etching and the dry etching.
[0041] For example, the mask layer 60 is removed through the wet etching using a second etchant including at least one of buffer oxide etchant (BOE) or hydrofluoric acid (HF).
[0042] Because the semiconductor layer 20 is hardly etched by the second etchant, the mask layer 60 can be selectively etched while minimizing the etch amount of the semiconductor layer 20 .
[0043] That is, the second etchant has a higher etch selectivity to the mask layer 60 than to the semiconductor layer 20 .
[0044] For example, the mask layer 60 is removed through the dry etching using a second etching gas including at least one of O 2 and CF 4 .
[0045] The mask layer 60 can be selectively etched while minimizing the etch amount of the semiconductor layer 20 because the semiconductor layer 20 is hardly etched by the second etching gas.
[0046] That is, the second etching gas has a higher etch selectivity to the mask layer 60 than to the semiconductor layer 20 .
[0047] Thereafter, a physical impact is applied to the substrate 10 and the semiconductor layer 20 , so that the first LED 51 , the second LED 52 and the third LED 53 are separated from each other by the scribing region 61 .
[0048] A lapping process may be performed to reduce the thickness of the substrate 10 before applying the physical impact to the substrate 10 and the semiconductor layer 20 . The lapping process may be performed through at least one process of chemical mechanical polishing (CMP), dry etching, wet etching and mechanical polishing using slurry.
[0049] FIG. 6 illustrates the first LED 51 separated by the scribing region.
[0050] The first LED 51 includes the semiconductor layer 20 , the first electrode 31 and the second electrode 41 which are formed over the substrate 10 .
[0051] The semiconductor layer 20 includes a buffer layer 21 , an n-type semiconductor layer 22 , an active layer 23 , a p-type semiconductor layer 24 and a transparent electrode layer 25 .
[0052] The buffer layer 21 relieves stress between the substrate 10 and the n-type semiconductor layer 22 and enables the semiconductor layer to easily grow. The buffer layer 21 may have at least one structure of AlInN/GaN, In x Ga 1−x N/GaN and Al x In y Ga 1−x−y N/In x Ga 1−x N/GaN.
[0053] The n-type semiconductor layer 22 may include a GaN layer doped with silicon, and may be formed by supplying silane gas containing n-type dopant such as NH 3 , trimethylgallium (TMGa) and Si.
[0054] The active layer 23 may have a single-quantum well or a multi-quantum well (MQW) structure formed of InGaN/GaN. The p-type semiconductor layer 24 may be formed of trimethylaluminum (TMAl), bis(ethylcyclopentadienyl)magnesium (EtCp2Mg), or ammonia (NH 3 ).
[0055] The transparent electrode layer 25 is formed of a material such as ITO, ZnO, RuOx, TiOx and IrOx. The first electrode 31 may be formed of titanium (Ti) and the second electrode 41 may be formed of a metallic material such as nickel (Ni).
[0056] The first LED 51 emits light from the active layer 23 when a power is supplied to the first and second electrodes 31 and 41 .
[0057] In FIG. 6 , a point light source 70 is exemplarily illustrated. A portion of the light emitted from the point light source 70 is reflected by the substrate 10 and emitted to the outside through sides of the first LED 51 .
[0058] Since the damaged region 12 on the sides of the first LED 51 has been removed through the wet etching or the dry etching, the light is scarcely absorbed at the sides of the first LED 51 , and thus it is possible to effectively emit the light to the outside.
[0059] FIGS. 7 to 11 are sectional views illustrating an LED and a method for manufacturing the same according to a second embodiment.
[0060] Referring to FIG. 7 , a semiconductor layer 20 , a first electrode 31 and a second electrode 41 are formed on a substrate 10 so as to form an LED. In addition, a mask layer 60 and a support member 80 are formed on the semiconductor layer and the first and second electrodes 31 and 41 .
[0061] The substrate 10 may include, for example, a sapphire substrate. The semiconductor layer 20 has a multi-stacked structure of a compound semiconductor.
[0062] A portion of the semiconductor layer 20 may be selectively etched, and the first electrode 31 is formed on the etched portion of semiconductor layer 20 . Accordingly, heights of the first and second electrodes 31 and 41 differ from each other even though they are formed on the same semiconductor layer 20 .
[0063] The embodiment of FIGS. 7 to 11 illustrates sectional views for convenience in description, which illustrate processes of forming first, second and third LEDs 51 , 52 and 53 .
[0064] The mask layer 60 protects the semiconductor layer 20 during a scribing process, and is formed of a material which can be wet-etched or dry-etched.
[0065] The support member 80 prevents damages of the first, second and third LEDs 51 , 52 and 53 which may be caused by a physical force applied to the first, second and third LEDs 51 , 52 and 53 while laser is irradiated onto the substrate 10 using a laser irradiation apparatus and then the damaged region of the substrate 10 due to the laser irradiation is removed by wet or dry etching.
[0066] Further, the support member 80 prevents the separation of the first, second and third LEDs 51 , 52 and 53 caused by external impact before a process of separating the first, second and third LEDs 51 , 52 and 53 is completed.
[0067] The support member 80 may be formed of at least one of an adhesive tape, a material which can be wet-etched or dry-etched, a metallic material and a wafer substrate.
[0068] The support member 80 may be selectively formed depending on thicknesses of the substrate 10 and the semiconductor layer 20 . Thus, the support member 80 may be omitted.
[0069] In FIG. 7 , reference numeral 11 denotes a scribing region. In second embodiment, laser is irradiated onto the scribing region 11 using a laser irradiation apparatus, thus dividing the substrate 10 into the first, second and third LEDs 51 , 52 and 53 .
[0070] A lapping process may be performed to reduce the thickness of the substrate 10 before irradiating the laser onto the scribing region 11 . The lapping process may be performed through at least one process of chemical mechanical polishing (CMP), dry etching, wet etching and mechanical polishing using slurry.
[0071] Referring to FIG. 8 , when the laser is irradiated onto the scribing region 11 , the substrate 10 of the scribing region 11 is selectively removed.
[0072] During laser irradiation, the layers in the scribing region 11 onto which the laser is irradiated are damaged, causing a damaged region 12 with a rugged surface to be formed, as illustrated in FIG. 8 .
[0073] The light emitted from the active layer of the LED does not pass through but is absorbed at the damaged region 12 , and thus the damaged region 12 is removed so as to improve light efficiency of the LED in this embodiment.
[0074] The removal of the damaged region 12 may be performed using a wet etching or dry etching process.
[0075] The wet etching process may be performed using a first etchant including at least one of hydrochloric acid (HCl), nitric acid (HNO 3 ), potassium hydroxide (KOH), sodium hydroxide (NaOH), sulfuric acid (H 2 SO 4 ), phosphoric acid (H 3 PO 4 ) and aluetch (4 H 3 PO 4 +4 CH 3 COOH+HNO 3 ). A temperature of the first etchant is between 200° C. and 400° C.
[0076] The mask layer 60 prevents the semiconductor layer 20 from being etched during the etching of the damaged region 12 . The mask layer 60 may be formed of, for example, silicon nitride (Si 3 N 4 ) or an oxide-based material such as silicon oxide (SiO 2 ), which is hardly etched by the first etchant.
[0077] Since the mask layer 60 is hardly etched by the first etchant, the damaged region 12 can be selectively etched while minimizing the etch amount of the semiconductor layer 20 .
[0078] The dry etching may be performed using an ICP/RIE or an RIE. In addition, the dry etching may be performed using a first etching gas including at least one of BCl 3 , Cl 2 , HBr and Ar.
[0079] The mask layer 60 configured to prevent the semiconductor layer 20 from being etched during the etching of the damaged region 12 may be formed of an oxide-based material such as SiO 2 , TiO 2 and ITO or a metallic material such as Cr, Ti, Al, Au, Ni and Pt, which is hardly etched by the first etching gas.
[0080] The wet etching and the dry etching may be performed for several minutes to several tens of minutes depending on etching environments. FIG. 9 illustrates that the damaged region 12 of the scribing region 11 is removed.
[0081] Referring to FIG. 9 , the mask layer 60 and the support member 80 formed on the semiconductor layer 20 are removed after the removal of the damaged region 12 .
[0082] The support member 80 may be differently removed depending on kinds of the support member 80 . For example, the support member 80 formed of adhesive tape is removed by detaching it, whereas the support member 80 formed of an etchable material is removed by etching process.
[0083] The removal of the mask layer 60 may be performed using at least one method of the wet etching and the dry etching.
[0084] For example, the mask layer 60 is removed through the wet etching process using a second etchant including at least one of buffer oxide etchant (BOE) or hydrofluoric acid (HF).
[0085] Because the semiconductor layer 20 is hardly etched by the second etchant, the mask layer 60 can be selectively etched while minimizing the etch amount of the semiconductor layer 20 .
[0086] For example, the mask layer 60 is removed by the dry etching using a second etching gas including at least one of O 2 and CF 4 .
[0087] The mask layer 60 can be selectively etched while minimizing the etch amount of the semiconductor layer 20 because the semiconductor layer 20 is hardly etched by the second etching gas.
[0088] Thereafter, a physical impact is applied to the substrate 10 and the semiconductor layer 20 , and thus the first LED 51 , the second LED 52 and the third LED 53 are separated from each other by the scribing region 11 .
[0089] FIG. 11 illustrates the first LED 51 separated by the scribing region 11 .
[0090] The first LED 51 includes the semiconductor layer 20 , the first electrode 31 and the second electrode 41 which are formed over the substrate 10 .
[0091] The semiconductor layer 20 includes a buffer layer 21 , an n-type semiconductor layer 22 , an active layer 23 , a p-type semiconductor layer 24 and a transparent electrode layer 25 .
[0092] The buffer layer 21 relieves stress between the substrate 10 and the n-type semiconductor layer 22 and enables the semiconductor layer to easily grow. The buffer layer 21 may have at least one structure of AlInN/GaN, In x Ga 1−x N/GaN and Al x In y Ga 1−x−y N/In x Ga 1−x N/GaN.
[0093] The n-type semiconductor layer 22 may include a GaN layer doped with silicon, and may be formed by supplying silane gas containing n-type dopant such as NH 3 , TMGa and Si.
[0094] The active layer 23 may have a single-quantum well or a multi-quantum well (MQW) structure formed of InGaN/GaN. The p-type semiconductor layer 24 may be formed of trimethylaluminum (TMAL), bis(ethylcyclopentadienyl)magnesium (EtCp2Mg), or ammonia (NH 3 ).
[0095] The transparent electrode layer is formed of a material such as ITO, ZnO, RuOx, TiOx and IrOx. The first electrode 31 may be formed of titanium (Ti) and the second electrode 41 may be formed of a metallic material such as nickel (Ni).
[0096] The first LED 51 emits light from the active layer 23 when a power is supplied to the first and second electrodes 31 and 41 .
[0097] In FIG. 11 , a point light source 70 is exemplarily illustrated. A portion of the light emitted from the point light source 70 is reflected by the substrate 10 and emitted to the outside through sides of the first LED 51 .
[0098] In the LED and the method for manufacturing the same according to the embodiments, the LED having a PN junction is described, which includes the n-type semiconductor layer, the active layer and the p-type semiconductor layer. However, a chip separation process according to the embodiments is also available for an LED having a NPN junction where an n-type semiconductor layer, an active layer, a p-type semiconductor layer and an n-type semiconductor layer are stacked in sequence.
[0099] Further, in the LED and the method for manufacturing the same according to the embodiments, the chip separation process of an LED having a horizontal configuration is described, in which the first electrode is formed on the n-type semiconductor layer and the second electrode is formed on the p-type semiconductor layer after the p-type semiconductor layer, the active layer and the n-type semiconductor layer are partially removed.
[0100] However, the chip separation process is also available for an LED having a vertical configuration in which the substrate including a conductive substrate, the first electrode, the n-type semiconductor layer, the active layer, the p-type semiconductor layer and the second electrode are sequentially formed. That is, the first electrode is formed between the semiconductor layer and the substrate and the second electrode is formed on the semiconductor layer, respectively.
[0101] Any reference in this specification to “a first embodiment,” “an embodiment,” “example embodiment,” etc., means that a particular feature, structure, or characteristic described in connection with the embodiment is included in at least one embodiment of the invention. The appearances of such phrases in various places in the specification are not necessarily all referring to the same embodiment. Further, when a particular feature, structure, or characteristic is described in connection with any embodiment, it is submitted that it is within the purview of one skilled in the art to effect such feature, structure, or characteristic in connection with other ones of the embodiments.
[0102] Also, it will be understood that when an element is referred to as being ‘on’ or ‘under’ another element, it can be directly on/under the element, and one or more intervening elements may also be present.
INDUSTRIAL APPLICABILITY
[0103] A light emitting diode (LED) and a method for manufacturing the same according to the embodiments can be applied to a separation process of LEDs having a variety of structures.
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A light emitting device includes a substrate having a top surface and an bottom surface and a light emitting structure on the substrate, disposed closer to the substrate top surface than the substrate bottom surface, having an n-type conductive type semiconductor layer, a p-type conductive type semiconductor layer, and an active layer. The light emitting device also includes a transparent electrode layer, a first electrode, and a second electrode. The substrate has side surfaces extending from the substrate bottom surface to the substrate top surface, the side surfaces inclined outwardly as the substrate extends in a direction from the substrate bottom surface to the substrate top surface. The transparent electrode layer overlaps more than 50% of a total area of the substrate bottom surface, and a part of light generated by the light emitting structure is emitted to outside via the transparent electrode layer.
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CROSS REFERENCE TO RELATED APPLICATION
[0001] This application claims the benefit of U.S. Provisional Application No. 61/069,969, filed Mar. 18, 2008, which is incorporated by reference.
BACKGROUND
[0002] The present disclosure is directed to draft arresters for overhead retractable doors and, more particularly, to non-contact draft arresters for roll-up overhead retractable doors.
INTRODUCTION TO THE INVENTION
[0003] Exemplary embodiments include a draft arrester for an overhead door. An exemplary embodiment may include a flexible draft curtain extending between a ceiling structure and a wound-up portion of the overhead door. The draft arrester may include a follower assembly, which may include one or more rollers arranged to roll against the overhead door. An exemplary embodiment may include a repositionable arm arranged to press the rollers against the wound-up portion of the door.
[0004] In an aspect, a draft arrester for a roll-up overhead door may include a draft curtain including a lower end and an upper end; a first pair of spaced-apart rollers operatively coupled to the lower end of the draft curtain, the first pair of spaced-apart rollers biased against a portion of the roll-up overhead door; and a curtain support coupled to the upper end of the draft curtain and adapted to be mounted above the first pair of spaced-apart rollers.
[0005] In a detailed embodiment, the first pair of spaced apart rollers may be mounted approximate a first end of a first repositionable arm, and the first repositionable arm may be pivotable about a pivot located proximate a second end of the first repositionable arm. In a detailed embodiment, a draft arrester may include a spring component arranged to bias the first end of the first repositionable arm towards the portion of the door. In a detailed embodiment, at least one of the rollers may be weighted, and the weighted roller may be arranged to bias the pair of spaced-apart rollers towards the portion of the door. In a detailed embodiment, a draft arrester may include a second pair of spaced-apart rollers operatively coupled to the first end of the draft curtain, the second pair of spaced-apart rollers being biased against the portion of the door. In a detailed embodiment, a draft arrester may include a substantially horizontal rail extending along the lower end of the draft curtain and interposing the first pair of spaced-apart rollers and the second pair of spaced-apart rollers. In a detailed embodiment, the draft curtain may be substantially flexible.
[0006] In an aspect, an overhead door assembly may include a rotatable spool; an overhead door windable onto the rotatable spool, the door being arranged to at least partially cover an opening having a width, a height, and at least one overhead boundary; a first wheeled follower biased against a portion of the overhead door wound around the rotatable spool; and a draft curtain extending vertically between the wheeled follower and the overhead boundary, while at the same time the draft curtain extends horizontally approximately the width of the opening.
[0007] In a detailed embodiment, the overhead boundary may be a ceiling. In a detailed embodiment, the draft curtain may be substantially flexible. In a detailed embodiment, the first wheeled follower may include a first pair of spaced-apart rollers mounted proximate a first end of a first repositionable arm, and a second end of the first repositionable arm may include a pivot. In a detailed embodiment, the first wheeled follower may include a spring component arranged to bias the first pair of spaced-apart rollers against the portion of the overhead door wound around the rotatable spool. In a detailed embodiment, at least one of the rollers may be weighted, and the weighted roller may be arranged to bias the first pair of spaced-apart rollers against the portion of the overhead door wound around the rotatable spool. In a detailed embodiment, an overhead door assembly may include a substantially horizontal rail extending from the first wheeled follower and along the draft curtain. In a detailed embodiment, an overhead door assembly may include a second wheeled follower biased against the portion of the overhead door wound around the rotatable spool, and at least a portion of the substantially horizontal rail may interpose the first wheeled follower and the second wheeled follower.
[0008] In an aspect, a draftless overhead door may include a flexible overhead door; a rotatable spool adapted to have at least a portion of the flexible overhead door wound therearound; a motor operatively coupled to the rotatable spool to wind and unwind the flexible overhead door, where unwinding of the flexible overhead door lowers the flexible overhead door and winding of the flexible overhead door raises the flexible overhead door; a vertical door track arranged to guide movement of the flexible overhead door; a roller biased against a portion of the flexible overhead door wound around the rotatable spool; and a curtain extending vertically between an upper structure and the roller, while at the same time extending horizontally proximate a width of the overhead flexible door.
[0009] In a detailed aspect, an overhead door may include a spring component arranged to bias the roller towards the rotatable spool. In a detailed embodiment, the roller may be mounted to a first end of a repositionable arm, and a second end of the repositionable arm may include a pivot. In a detailed embodiment, the roller may include a pair of spaced-apart rollers. In a detailed embodiment, the door may have a width, and the draft curtain may extend substantially the entire width of the door.
BRIEF DESCRIPTION OF THE DRAWINGS
[0010] The detailed description refers to the following figures in which:
[0011] FIG. 1 is a cross-sectional view of a repositionable door incorporating an exemplary draft arrester, which may be operative to inhibit drafts between the door roll and the header, where the door is shown in a barrier position;
[0012] FIG. 2 is a cross-sectional view of a repositionable door incorporating the exemplary draft arrester of FIG. 1 , where the door is shown in an intermediate position;
[0013] FIG. 3 is a cross-sectional view of a repositionable door incorporating the exemplary draft arrester of FIG. 1 , where the door is shown in a retracted position;
[0014] FIG. 4 is a frontal view, from the exterior, of an exemplary building opening incorporating a repositionable door and an exemplary draft arrester;
[0015] FIG. 5 is an elevated perspective view, from the interior, of one corner of an exemplary building opening incorporating a repositionable door and an exemplary draft arrester; and
[0016] FIG. 6 is an elevated perspective view, from the exterior, of one corner of an exemplary building opening incorporating a repositionable door and an exemplary draft arrester.
DETAILED DESCRIPTION
[0017] Exemplary embodiments described and illustrated herein include apparatus and methods for inhibiting drafts over roll-up retractable doors. It will be apparent to those of ordinary skill in the art that the exemplary embodiments discussed herein are exemplary in nature and may be reconfigured without departing from the scope and spirit of the present invention. However, for clarity and precision, the exemplary embodiments as discussed herein may include optional steps, methods, and features that one of ordinary skill should recognize as not being a requisite to fall within the scope of the present disclosure as defined by the claims.
[0018] An exemplary door draft arrester 10 is shown in FIGS. 1-6 . In exemplary form, a door draft arrester 10 may be a component of a repositionable door 12 , which may selectively close off an opening of a building. In exemplary form, the building may be a drive-through car wash, and the opening may be at the end of the car wash path through the building. For purposes of explanation only, the opening may be generally rectangular with a vertical lengthwise dimension 18 and a horizontal widthwise dimension 20 . In an exemplary embodiment, the opening may be defined by generally vertically oriented left and right side walls 22 , 24 and a generally horizontal header wall 26 which may spans overhead between the side walls 22 , 24 . The plane of the opening may interpose the interior of the building and its exterior.
[0019] In an exemplary embodiment, a door frame 28 may be inset within the interior of the building proximate the opening. The door frame 28 may include opposing vertical members 30 , 32 that may be mounted respectively to the left and right side walls 22 , 24 . Each vertical member 30 , 32 may include a pair of channel guides 34 that cooperate to define a vertical channel 36 into which lateral ends 38 of a repositionable door 12 may extend. In exemplary form, a channel guide 34 may comprise a vertically oriented angle iron segment 42 having a deflector 44 mounted to its proximal end. An exemplary deflector 44 is adapted to be angled outward away from the channel 36 so that adjacent deflectors 44 cooperate to provide a tapered mouth feeding into the channel 36 . In this fashion, as the door 12 is repositioned from a retracted position toward a barrier position, the free horizontal end of the door may contact one of the deflectors 44 , which may route lateral ends 38 of the door 12 into the channel 36 . The precise dimensions of the angle iron segments 42 and deflectors 44 may be a matter of design choice. Likewise, the angle at which the deflectors 44 are oriented may be a matter of design choice; the greater the angle, the less gradual the taper.
[0020] In an exemplary embodiment, a horizontal header 46 that spans the complete widthwise dimension of the opening may be mounted on the interior side of the opening. In exemplary form, the header may comprise a Lexan or metal boxed framework that mounts directly to the header wall 26 to provide a partial enclosure for a repositionable curtain assembly 48 . The curtain assembly 48 may be mounted to the framework 46 by way of a generally horizontal molding 50 , which may extend substantially the entire width of the opening, using a plurality of fasteners 52 . A curtain 54 may be mounted to the heater 46 by the molding 50 . The curtain may be fabricated from the same material as the door 12 . Nevertheless, it is to be understood that other materials could be utilized to fabricate the curtain 54 depending upon the end application. The curtain 54 , in exemplary form, may be generally rectangular with its widthwise dimension dominating its lengthwise dimension. Specifically, it is the lengthwise dimension that may span between the molding 50 and a horizontal rail 56 mounted to a pair of opposing arms 58 mounted to corresponding perpendicular plates 60 extending from the upper portions of the left and right side walls 22 , 24 and adjacent the header wall 26 . Each arm 58 may include a pair of wheels 62 , 64 that may be interposed by the horizontal rail 56 . Each wheel 62 , 64 may be adapted to ride upon the exterior of the door 12 as it is rolled up responsive to the arm 58 being forced against the door roll. However, as the diameter of the door roll changes, whether increasing as the door is retracted or decreasing as the door is deployed, the arm 58 may force the wheels 62 , 64 against the door roll to substantially maintain a constant axial gap between the horizontal rail 56 and door roll.
[0021] In an exemplary embodiment, the door 12 may be repositioned between a retracted position and a barrier position using a motor assembly 66 . In exemplary form, one end of the door 12 may be mounted axially to a horizontal roller which may be turned either clockwise or counterclockwise by the motor assembly. The motor assembly 66 may include an electric motor 70 coupled to an output pulley 72 that repositions a belt 74 engaging a input pulley 76 coupled to the roller 68 . It is too be understood, however, that various drive mechanisms could be utilized, such as using the output shaft of the motor 70 to directly engage the roller 68 or one could easily devise a set of gears to interface between the roller 68 and the motor 70 to accomplish a similar result. In an exemplary embodiment, as the roller 68 is rotated to move the door 12 toward its retracted position, the door 12 may wind around the roller 68 to provide a cylindrical roll (i.e., a “door roll”) that gradually increases in diameter as the door is retracted until a maximum diameter is reached corresponding to substantially the entire door being wound around the roller 68 . It should be noted, however, that it may not be necessary to wind the entire door around the shaft to allow egress of automobiles through the opening as in an exemplary carwash.
[0022] The present disclosure contemplates that a problem experienced with conventional roll-up doors is the occurrence of a draft between the header and the door roll. In some conventional door systems, the gap between the door roll and the header may vary and may be quite substantial to allow air to freely pass therebetween and create a draft that in certain instances is operative to allow liquids and other flowing materials within the interior of the building to escape or conversely to allow external fluids and debris to enter the building even while the door is in its barrier position. Exemplary embodiments described herein, however, may overcome these drawbacks by arresting the draft using the repositionable curtain assembly 48 to substantially decrease fluid flow between the horizontal shaft and header, thereby substantially decreasing any draft.
[0023] In an exemplary embodiment, the repositionable curtain assembly 48 may comprise a fixed length curtain 54 that may be mounted at one end to the molding 50 and may be mounted at an opposite end to the horizontal rail 56 . In exemplary form, the horizontal rail 56 may be substantially in parallel with the door roll and/or roller 68 to maintain a substantially constant spacing between the rail 56 and door roll of approximately two inches. This constant spacing may be accomplished by providing a reactive system that starts with the reactive arms 58 .
[0024] In an exemplary embodiment, each arm 58 may include a polyethylene unibody construction having a through hole 78 that receives a bolt extending from a corresponding perpendicular plate 60 toward the door roll. The end of the bolt may also receive a series of washers and/or a lock nut to provide play and freedom of movement rotationally between the bolt and the arm 58 . In other words, this arrangement may allow each arm 58 to freely rotate/pivot around its corresponding bolt. This rotation may be caused by the change in diameter of the door roll as the door is either retracted or deployed. As discussed previously, each arm 58 may include a pair of wheels 62 , 64 adapted to ride upon the exterior of the door as it is rolled up and/or down. In order to maintain the wheels against the exterior of the door roll, the arm 58 itself may be biased towards the door roll. This biasing may be accomplished by using weighted wheels that gravity directs against the door roll or alternatively using a spring biasing structure (not shown) circumscribing the bolt to apply a spring force resisting rotation of each arm 58 . However, those skilled in the art will understand that other mechanisms may be used to maintain the wheels 62 , 64 against the door roll in accordance with the present disclosure.
[0025] As mentioned previously, an exemplary door draft arrester 10 may find application in a carwash facility. By way of illustration, and not limitation, an exemplary draft arrester may be installed at the exit of a carwash. In exemplary form, an electric motor 70 may be electrically controlled by an automated control system (not shown) and at least one position sensor for sensing the presence of an automobile in proximity to the exit. Those skilled in the art are quite familiar with automated controls and a discussion of such a system in detail, with sensors, has been omitted for purposes of brevity. In exemplary operation, the door 12 may be selectively repositioned from a barrier position to a retracted position to allow egress of automobiles through the exit. Specifically, in a carwash, the door's default position may be the barrier position and movement of the door to the retracted position may only occur when the automated system senses an automobile in proximity to the exit or opening 14 . At this time, the automated system may engage the electric motor 70 to rotate the roller 68 in the appropriate direction to retract the door from its barrier position (see FIG. 1 ) through an intermediary position (see FIG. 2 ) to a retracted position (see FIG. 3 ). As can be seen from the foregoing figures, repositioning of the door 12 does not compromise the draft arresting capabilities of the exemplary draft arrester.
[0026] In an exemplary embodiment, the curtain 54 may operate to substantially shut off the widthwise opening between the door roll and the header 46 . As can be seen by the change in position of the arms 58 , the wheels 62 , 64 may continue to ride upon the exterior of the door roll and correspondingly pivot each arm 58 as the diameter of the door roll decreases (as the door is deployed) or increases (as the door is retracted). Correspondingly, the horizontal rail 56 mounted to each arm 58 at the rail's axial ends may maintain a substantially constant spacing from the door roll, regardless of the diameter of the door roll. To accommodate the changing door roll diameter, the curtain 54 may floats and/or deform. In an exemplary embodiment, at no time, however, does the deformation of the curtain 54 result in the absence of a barrier arresting drafts between the door roll and the header 46 .
[0027] The material composition of the components of the instant invention may be a matter of design choice and may be selected from composites, metals, alloys, ceramics, plastics, or other materials. Those skilled in the art will recognize that different applications for an exemplary draft arrester may require selection of differing materials. By way of example, and not limitation, an exemplary repositionable door 12 may be fabricated from any weatherproof material and may include a series embedded horizontal ribs 80 to generally maintain the door in a planar orientation. The door material, by its nature may be flexible and able to be deformed, and may include weights (not shown) attached proximate to the exposed horizontal end of the door nearest the floor. One of the advantages of using a flexible door is that collisions with automobiles cause less damage to the door itself and the automobile.
[0028] Following from the above description and invention summaries, it should be apparent to those of ordinary skill in the art that, while the methods and apparatus herein described constitute an exemplary embodiments, the disclosure contained herein is not limited to these precise embodiments and that changes may be made without departing from the scope of the disclosure as defined by the claims (for example, and without limitation, it is within the scope of the invention that the base plate and cover plate take different forms, such as a box and a lid that are separate from each other or even connected by a hinge). Likewise, it is to be understood that it is not necessary to meet any or all of the identified advantages or objects disclosed herein in order to fall within the scope of any claim, since the invention is defined by the claims and since inherent and/or unforeseen advantages may exist even though they may not have been explicitly discussed herein. Finally, it will be apparent that additional claims may be inherent in the disclosure and may not be expressly described herein.
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A draft arrester for an overhead door. An exemplary embodiment may include a flexible draft curtain extending between a ceiling structure and a wound-up portion of the overhead door. The draft arrester may include a follower assembly, which may include one or more rollers arranged to roll against the overhead door. An exemplary embodiment may include a repositionable arm arranged to press the rollers against the wound-up portion of the door.
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FIELD OF INVENTION
This invention relates to hydrocarbylthio substituted aromatic amines and more particularly to a process for preparing them.
BACKGROUND
As disclosed in U.S. Pat. No. 4,594,453 (Ranken et al.), it is known that various (hydrocarbylthio)aromatic amines are useful as intermediates in the preparation of biologically-active materials, polyurethanes, etc.; and they can be prepared by reacting an aromatic amine with an alkyl disulfide in the presence of a catalytic amount of a Lewis acid. The preferred catalysts of Ranken et al. are metal halides, such as aluminum chloride, boron trifluoride, boron trichloride, ferric chloride, and zinc chloride.
In the case of at least some aromatic amines, it has been found that the preferred catalysts identified by Ranken et al. have the disadvantages of effecting the desired hydrocarbylthiations at too slow a rate to be completely satisfactory and of sometimes providing too low a yield of product.
In U.S. Pat. No. 4,751,330 (Davis), various alkylthio-aromatic amines are prepared by reacting an aromatic amine with an alkyl disulfide in the presence of a metal or metal halide catalyst and iodine as a promoter. These reactions are noted to have higher reaction rates and/or higher yields than the prior art reactions discussed above.
However, even the improved process of Davis requires many hours to achieve satisfactory yields.
SUMMARY OF INVENTION
An object of this invention is to provide a novel continuous process for preparing hydrocarbylthio substituted aromatic amines.
Another object is to provide such a process wherein the products are prepared by the hydrocarbylthiation of aromatic amines in the presence of metal or metal halide catalysts.
A further object is to provide such a process wherein the reaction rates and/or product yields are improved.
These and other objects are attained by reacting an aromatic amine with a hydrocarbyl disulfide in the presence of a catalytic amount of a metal or metal halide in a packed bed reactor where gaseous hydrocarbyl disulfide is allowed to flow through the liquid admixture of amine, catalyst and hydrocarbyl disulfide.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
Aromatic amines utilizable in the practice of the invention include (1) compounds having at least one amino group attached to a carbocyclic or heterocyclic ring of an aromatic compound containing one or more simple and/or fused rings, such as benzene, naphthalene, anthracene, pyrrole, pyridine, indole, etc., rings and (2) reactive heterocyclic amines, such as pyrrole, indole, imidazole, etc. The compounds may bear no substituents other than the required amino group, or they may bear substituents inert to the reaction conditions, such as one or more additional amino groups or substituents such as chloro, fluoro, alkyl, aryl, alkaryl, or aralkyl groups on any positions other than those to be substituted by hydrocarbylthio groups. In the case of coupled aromatic rings, the rings may be directly attached to one another or may be coupled through a bridge such as an oxygen, sulfur, sulfoxide, sulfone, alkyl, or another hydrocarbon link. Useful compounds include, e.g., 4,4'-methylenedianiline, 4-(phenylthio)aniline, 1,3-dimethylpyrrole, 1-methylpyrrole, 2-aminobiphenyl, 4-phenoxyaniline, 7-methylindole, aminobenzenes containing one or two amino groups, such as aniline, 4-butylaniline, 4-methylaniline, 4-chloroaniline, 2-ethylaniline, N-methylaniline, 2,4- and 2,6-diaminotoluenes or mixtures of such toluenes, 2,6-diamino-1-ethylbenzene, 2,4-diaminoxylenes, 2,6-diaminoxylenes or mixtures of such isomers, etc.
Hydrocarbyl disulfides which ma be reacted with the aromatic amines include saturated and unsaturated aliphatic, cycloaliphatic, and aromatic disulfides in which the alkyl groups optionally bear inert, such as chloro, substituents. Exemplary of such compounds are methyl, ethyl, propyl, n-butyl, sec-butyl, t-butyl, 2-chloropentyl, cyclopentyl, cyclohexyl, phenyl, benzyl, p-tolyl, and p-chlorophenyl disulfides, etc.
The reaction of the aromatic amine with the hydrocarbyl disulfide is generally conducted at a temperature in the range of about 20°-300° C. and at a pressure of atmospheric up to about 1000 psi in the presence of a catalyst. Suitable catalysts are Lewis acid catalysts, such as metal halides, e.g., aluminum chloride, boron trifluoride, ferric chloride, zinc chloride, copper iodide, etc.; and the organometallic compounds derived from the reaction of the aromatic amine with the metal halides, metal alkyls, and reactive metals such as aluminum. The preferred catalysts are the metal halides, such as copper (I) iodide, aluminum chloride, boron trifluoride, and boron trichloride. Copper iodide (I) is especially preferred. The catalyst is employed in catalytic amounts, generally in a catalyst/aromatic amine mole ratio of about 0.01-0.5/1, preferably about 0.01-0.2/1. When the catalyst is one of the more active catalysts and/or is used in a relatively large amount, the temperature and pressure conditions required are milder than when a less active catalyst and/or a lesser amount of catalyst is utilized. Thus, e.g., when about 0.01-0.1 molar proportion of aluminum chloride is employed, particularly satisfactory results are obtained when the reaction is conducted at about 100°-50° C. and atmospheric pressure, whereas higher temperatures and/or elevated pressures are required for comparable results when aluminum is used instead of aluminum chloride.
In conducting the continuous process of the present invention, it has been discovered that when a heated mixture of catalyst, aromatic amine and hydrocarbyl disulfide is allowed to flow as a thin film along a column and an inert (nonreactive) gas is permitted to flow through the moving liquid film mixture in a counter-current manner, the reaction time to produce the desired hydrocarbylthio substituted aromatic amine product is dramatically decreased in comparison to the conventional batch process where the ingredients are admixed and allowed to react in a reaction vessel. The inert (nonreactive) gas may be nitrogen, carbon dioxide or the like. Most preferably the inert (non-reactive) gas is gaseous hydrocarbyl disulfide. Reaction times are reduced to a few seconds, i.e., as little as five seconds is necessary to achieve the desired reaction. As the liquid stream emerges from the column, it is comprised principally of monohydrocarbylthio substituted aromatic amine, catalyst residue, and small amounts of unreacted hydrocarbyl disulfide and aromatic amine. Distillation readily separates the hydrocarbylthiolated product from the remainder of the product stream.
The reactant mixture is formed into a thin film by allowing it to flow along the surface of a column. The column is typically packed with granular solids, ceramic plates, screening, etc. in order to facilitate the formation of the thin reactant film.
While it is preferred that inert, granular particles are used in the column, i.e., sand, glass beads, alumina, it has been found that glass beads are most preferably employed for such packing.
The process of the invention results in the formation of alkyl aromatic amines which are useful as intermediates in the preparation of biologically-active materials, polyurethanes, etc. Some of these amines are novel compounds, e.g., those corresponding to the formulas: ##STR1## wherein R is an alkyl group; Y is an alkylthio group, Z is an inert substituent, i.e., a substituent which is inert to the reaction conditions, such as chloro, fluoro, nitro, amino, hydrocarbyl, or hydrocarbylthio; m has a value of 0-3; and n is an integer of 2-4. The hydrocarbyl groups are preferably alkyl, e.g., methyl, ethyl, etc., groups.
The following examples are given to illustrate the invention and are not intended as any limitation thereof.
EXAMPLES
Example A
A solution of 3.75 wt % of cuprous iodide (CuI) and 96.25 wt % of commercial toluenediamine (c-TDA)--a material containing 80% 2,4-diaminotoluene and 20% 2,6-diaminotoluene was fed downward at a rate of 2.3 g/min. to a 1" diameter, 11" long stainless steel column with 0.16" Pro-Pak® packing. Gaseous dimethyl disulfide (DMDS) was fed upward to the column at a rate of 15.7 g/min. DMDS was refluxed back to the column by a water-cooled dephlegmator. The column temperature was maintained at 150° C. with a heating oil jacket. By-product methyl mercaptan was vented to atmosphere and burned by a Bunsen Burner through a Grove back pressure regulator which maintained the column pressure at 28 psig. The effluent was analyzed by gas chromatography and contained 29.1 area% c-TDA, 54.8 area% mono(methylthio) derivatives of c-TDA (MMTDA), 16.1 area% di(methylthio) derivatives of c-TDA (DMTDA).
Example 8
A series of experiments were carried out using partially converted reaction crude as the feed to the column, described in Example A. The reaction crude was prepared by reacting the c-TDA and CuI solution with 50% excess DMDS in a batch reactor at 140° C. and atmospheric pressure. This reaction crude and DMDS were then fed to the column. The resulting effluent was then analyzed by gas chromatography. The feed and effluent compositions are listed in Table I.
TABLE I__________________________________________________________________________Temp. Pressure Crude DMDS c-TDA MMTDA DMTDA TMTDA*(°C.) (psig) (g/min) (area %)__________________________________________________________________________158 28 2.4 14.9 in 26.5 59.2 14.3 0.0 out 7.5 47.4 45.1 0.0156 28 2.4 14.6 in 6.1 38.3 55.6 0.0 out 1.5 30.2 68.1 0.2158 28 2.4 14.4 in 1.2 24.2 74.4 0.2 out 0.3 12.7 86.5 0.4154 28 2.7 14.2 in 0.4 13.0 86.2 0.4 out 0.0 6.6 92.9 0.5152 28 2.4 14.1 in 0.0 8.5 91.0 0.5 out 0.0 4.0 95.3 0.7__________________________________________________________________________ *tri(methylthio) derivatives of cTDA
Comparative Example A
A suitable reaction vessel was charged with one molar proportion of aniline and 0.067 molar proportion of aluminum chloride. After the reaction mixture had been stirred in a nitrogen atmosphere at 150° C. for 30 minutes and cooled to 100° C., one molar proportion of methyl disulfide was added. The reaction mixture was then stirred and heated at an initial reflux temperature of 130° C. to a final temperature of 170° C. in 25 hours to provide a crude reaction product which was cooled, worked up, and analyzed by gas chromatography, using n-undecane as an internal standard. The analysis showed that the reaction mixture contained 14 wt % methyl disulfide, 19 wt % aniline, 18 wt % 2-(methylthio)aniline, 33 wt % 4-(methylthio)aniline, and 7 wt % 2,4-di(methylthio)aniline.
Comparative Example B
Comparative Example A was essentially repeated except that 0.0085 molar proportion of iodine was added to the initial reaction mixture, and the reflux time required was only 7 hours instead of 25 hours. The reaction resulted in the formation of a reaction mixture containing 12 wt % methyl disulfide, 16 wt % aniline, i7.5 wt % 2-(methylthio)aniline), 37 wt % 4-(methylthio)aniline, and 11.2 wt % 2,4-di(methylthio)aniline.
Comparative Example C
One molar proportion of commercial toluenediamine (c-TDA) a material containing 80% 2,4-diaminotoluene and 20% 2,6-diaminotoluene was heated with 0.065 molar proportion of aluminum chloride at 150° C. for one hour. Methyl disulfide was then added in sufficient excess to maintain the reaction temperature at 135° C., and the reaction was conducted for 39 hours to achieve 100% conversion of the c-TDA. Analysis of the product showed it to contain 16 mole% mono(methylthio) derivatives of c-TDA (MMTDA), 78 mole% di(methylthio) derivatives of c-TDA (DMTDA, and 6 mole% by-products.
Comparative Example D
Comparative Example B was essentially repeated except that the initial reaction mixture contained one molar proportion of c-TDA, 0.068 molar proportion of aluminum chloride, and 0.0032 molar proportion of iodine, and the reaction time required to reach 100% conversion was only 22 hours. The product contained 10 mole% MMTDA, 83 mole% DMTDA, and 6 mole% by-products.
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A continuous process for the hydrocarbylthiation of aromatic amines is disclosed. The process involves forming an admixture of aromatic amine, hydrocarbyl disulfide and an effective amount of a Lewis acid catalyst and subsequently allowing such admixture to flow as a thin film along a column. An inert gas is passed in a counter-current manner through the admixture. The liquid thiohydrocarbyl aromatic amine product is then separated from the gaseous effluent
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BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention relates to a flexible dispensing package for liquids having a wick that acts as an applicator.
2. Description of the Related Art
Previous methods for dispensing controlled amounts of liquid include laminated foil/film packages holding a wooden, plastic or rolled paper stick with a moistened swab end. In the usual manner seen, such packages are foil/plastic film laminates and include a stick with a pad attached to an end. The package around the pad includes an iodine compound useful in disinfecting skin of patients. The package is opened, the swab is removed and the foil/film package is discarded. The stick is then held and used to apply the solution to the area desired. The disadvantage of this package is that it requires two separate operations; swab manufacture and packaging; and it is also relatively expensive to produce and the stick must be held properly to keep it sterile.
Farah, U.S. Pat. No. 4,881,278 shows a toilet seat disinfectant in which a foil package may be pulled open to expose two pads adhered to the foil sides. A folded toilet seat cover is in the upper compartment.
Laipply, U.S. Pat. No. 4,427,111 shows an alcohol wipe sealed in a foil pouch. It shows the prior art packages in which the moist towelette is removed after the foil package is torn open. The Laipply approach is to attach the towelette to the foil such that the package may be peeled open to expose the towelette secured to the inside wall(s) of the foil.
In a later issued patent, U.S. Pat. No. 5,046,608, Laipply adds additional figures showing ways to open the package and to attach the towelette to the inside of the foil. Finally, U.S. Pat. No. 4,800,904 to Kinseley et al shows a nail polish removing pouch in which a moistened towelette is attached to the interior walls of the foil pouch and a finger may be inserted into an opened end to contact the moist towelette.
The art described in this section is not intended to constitute an admission that any patent, publication or other information referred to herein is "prior art" with respect to this invention, unless specifically designated as such. In addition, this section should not be construed to mean that a search has been made or that no other pertinent information as defined in 37 C.F.R. § 1.56(a) exists.
SUMMARY OF THE INVENTION
The invention provides a sealed package that when opened presents a wet swab that is used by holding the remainder of the package, since the swab is captively held to the package. In its simplest form, a doubled over pad is inserted into a simple liquid-tight pouch, a transverse seal is applied, the desired liquid is added, and the pouch is sealed fluid tight. The improvement consists of the addition of a transverse seal intermediate from the end seals which captures the pad to the package. In this manner, when the top of the pouch is removed, a wet "swab" is exposed which may be used by grasping the remainder of the pouch. This ensures that the user will not have to touch the pad during use and provides an applicator handle.
This construction is very inexpensive to produce and allows the application of the liquids held within without contamination or leakage onto the user. The swab may carry whatever chemicals are needed, in a single use, easy-to-use pouch. The swab may be stiffened according to the needs of the user and chemicals to be used by selection of pad material, thickness, number of folds or addition of a separate stiffener.
BRIEF DESCRIPTION OF THE DRAWINGS
A detailed description of the invention is hereafter described with specific reference being made to the drawings in which:
FIG. 1 is a perspective view of the wet swab captured package of the invention;
FIG. 2 is a perspective view of the package of FIG. 1 with one side of the foil removed;
FIG. 3 shows how to remove the top head of the package to expose the swab;
FIG. 4 shows the exposed swab used to apply liquid;
FIG. 5 shows a variant of the package of FIG. 1 having a slit opening;
FIG. 6 shows a variant of the package of FIG. 1 having a peel opening;
FIG. 7 shows a prior art flow diagram for the process of making foil pouches;
FIG. 8 shows the process for making the package of the invention;
FIG. 9 shows a perspective view, patially broken-away of the package showing a stiffener pushing in the pad; and
FIG. 10 shows a cross-sectional view across lines 10--10 of FIG. 9 of the package 10 including a plastic stiffening member 52.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
The package 10 of the invention is quite simple, yet provides a wet swab applicator at very low cost that is easy to use while keeping the hands free from the wet swab. As best shown in FIGS. 1, 2 and 4, package 10 is envelope-like comprising a front panel 12 and rear panel 14 of suitable fluid impermeable material 16, e.g., metal foil, plastics, and laminates such as aluminum foil/plastic. An absorbent pad 18 is held within the package 10. The package is sealed about its perimeter, either by adhesive or by a physical seal between the front and rear panels.
The pad or towlette 18 is held to the package by a transverse seal line 20 across the package 10 which prevents the pad 18 from being readily removed from the package. Means are provided to remove a head portion 22 of the package to expose the pad 18. As shown in FIGS. 2 and 3, the head portion 22 is easily removed by tearing across notched tears 24 formed in the package. Alternatively, the head may be removed by tearing across slits 26 as shown in FIG. 5 or by peeling back the head portion 22 via a peel strip 28 as shown in FIG. 6. Note that in FIG. 6, the head portion 22 is much larger, simply to show that the amount of pad exposed versus retained in the reservoir may vary. Any of the conventional means currently used to open foil packages such as cleaning wipes, catsup packages and the like may be employed. The object is to be able to readily remove the top head portion 22 of the package to expose the wet swab 18 held thereunder.
The pad 18 under the head portion 22 is not attached to the package in any way. The remainder of the pad is attached to the package by the seal line 20 which may be immediately below the tear notch 24 or anywhere therebelow. More than one seal line may be provided, if desired. The space between the transverse seal and the bottom seal acts as a liquid reservoir.
The effect of the joining of the pad to the package below the seal line is to create a very simple, easy to use swab. When the head portion is removed, the swab is exposed. The remainder of the package may be gripped in a hand 30 while the exposed swab 18 is used to supply liquid to a surface. The package 10 may be squeezed to force additional fluid to the swab head. As shown in FIG. 4, the exposed pad 18 is being used as a swab across an arm 32 in the direction of the arrows. The package 10 operates as a holder to hold the swab away from the materials on the swab. This is important to maintain sterility or to prevent applying paint or other liquid carried therein to one's fingers.
FIG. 7 shows the typical manufacturing process for foil/film laminate packets. A process for making the wet swab captured packages 10 of the invention is shown in FIG. 8, with like reference numerals being used in FIGS. 7 and 8 where the stations are similar. The film or foil 16 to make the package 10 is supplied from a film supply roll 40. The film 16 passes over rollers 42 and is folded in two by a plow 44. The bottom is formed by the fold line and the sides are sealed by a stamping mechanism to form side seals 46. Typically, a bottom seal 36 is made over the fold to improve appearance, minimize leakage and make the package look more uniform. The bottom fold may then be cut off and the remnants of the front panel 12 and rear panel 14 may be used to make the peel strip 28, such that the user simply grasps both panels and peels the package open. Suitable machines for forming the packages of the invention are available from Klockner Bartelt, Inc. and are described in U.S. Pat. Nos. 5,080,747 and 5,058,364.
Most typically, the packages are formed from laminated foil and plastic. The foil provides added strength and rigidity while the thin plastic film provides chemical resistance. Also, the plastic film enables easy heat sealing. The plastic film of one panel is pressed against the other panel and is heated to fuse the plastics together. The combination of heat and pressure, given the proper dwell time for the plastic used provides an excellent seal. Suitable films are available from E. I. DuPont de Nemours and Company of Wilmington, Del., U.S.A. marketed under the trademark Surlyn®.
It is possible to form the packages 10 of the invention from plastic without foil. Alternatively, foil alone may be satisfactory depending on the liquid to be held. If foil alone is used, a seal may be formed by pattern printing adhesive around the periphery.
The pad or towlette 18 is formed from a towlette supply roll 48 which feeds material to a station where it is cut by a cutter 54 and inserted into the formed package, usually with a mechanical finger that pushes the v-folded pad 18 into the still open package. Liquid is then added and the top seal 50 is formed to complete the package. The individual packets are typically separated from each other after the side and bottom seals have been formed but before filling with towlette or liquid. A cutter 56 (which is shown in the FIGS. before the final package sealing) separates the individual packages.
As shown in FIG. 8, the inventive packets follow a similar manufacturing process. However, after the pad has been inserted into the package a mid seal line 20 is formed across the package to secure the towlette 18 to the package. The remainder of the steps may be identical to the prior art process. It should be noted that in the manufacturing process the bottom seal 36 is actually the last edge to be sealed, and shows in FIG. 8 as the upper edge furthest from the transverse seal 20. This is because the pad 18 is inserted with a finger, folded in a v-shape, such that the fold of the pad 18 will be closest to the top seal 50, adjacent what appears to be the bottom of the package.
If greater swab rigidity is desired, the pad material may be selected to provide greater thickness, have more folds or it may employ additional fibers in the weave that provide stiffening. Alternatively, the finger that inserts the pad may be a strip of plastic 52 that is cut after each pad 18 is inserted to leave a stiffening member surrounded by the pad within the completed package as shown in FIG. 9. In such a package, the swab exposed by removing the head portion 22 is much stiffer.
The wet swab package of this invention may be used to carry almost any liquid. It is expected to find greatest application in dispensing germicides such as povidone-iodine 10%. Other liquids may include paints, paint removers, nail polish or remover, lubricants, solvents, adhesives and ointments. The pad material is chosen based on the properties of the liquid to be dispensed. Absorbent materials will tend to hold the liquid in the pad better than non-absorbent materials. The degree of wicking is controlled by selection of the pad material. For example, application of touch-up paint to an automobile should not allow the paint to drip readily from the package. Rather, the paint should begin to ooze out, in a drop that may be touched to the auto surface, thereby transferring paint. As used herein, "liquid" encompasses compounds having greatly different viscosities and includes gels.
While this invention may be embodied in many different forms, there are shown in the drawings and described in detail herein specific preferred embodiments of the invention. The present disclosure is an exemplification of the principles of the invention and is not intended to limit the particular embodiments illustrated.
This completes the description of the preferred and alternate embodiments of the invention. Those skilled in the art may recognize other equivalents to the specific embodiment described herein which equivalents are intended to be encompassed by the claims attached hereto.
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A sealed envelope contains a moistened pad that functions as a swab. The pad is secured to the envelope by an intermediate seal line. When the top of the envelope is removed, the pad is exposed. Since the pad is still captively held to the remainder of the envelope, the liquid on the pad may be dispensed by holding the clean, dry bottom of the envelope. The pad functions as a swab and the remainder of the envelope functions as the applicator handle and reservoir.
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CROSS REFERENCE TO RELATED APPLICATIONS
The present application shares specification text and figures with he following applications, filed concurrently with the present application: application Ser. No. 09/437,187, “High Speed Lock Acquisition Mechanism With Time Parameterized Cache Coherency States,” application Ser. No. 09/437,182, “High Speed Lock Acquisition Mechanism via a “One Shot” Modified State Cache Coherency Protocol now abandoned, ” application Ser. No. 09/437,184, “An Extended Cache Coherency Protocol with a “Lock Released” State,” now U.S. Pat. No. 6,549,989, application Ser. No. 09/437,183, “An Extended Cache Coherency Protocol With a Modified Store Instruction Lock Release Indicator,” and application Ser. No. 09/437,186, “An Extended Cache Coherency Protocol With a Persistent “Lock Acquired” State.”
BACKGROUND OF THE INVENTION
1. Technical Field
The present invention generally relates to an improved data processing system and in particular to a system and method for improved cache management in a multiprocessor system. Still more particularly, the present invention relates to a system and method using specialized cache states and state sequences to provide improved cache coherency management in a multiprocessor data processing system.
2. Description of the Related Art
In order to enhance performance, state-of-the-art data processing systems often utilize multiple processors which concurrently execute portions of a given task. To further enhance performance, such multiple processor (MP) data processing systems often utilize a multi-level memory hierarchy to reduce the access time required to retrieve data from memory. A MP data processing system may include a number of processors, each with an associated level-one (L1) cache, a number of level-two (L2) caches, and a number of modules of system memory. Typically, the memory hierarchy is arranged such that each L2 cache is accessed by a subset of the L1 caches within the system via a local bus. In turn, each L2 cache and system memory module is coupled to a system bus or interconnect switch, such that an L2 cache within the MP data processing system may access data from any of the system memory modules coupled to the bus or interconnect switch.
Because each of the number of processors within a MP data processing system may modify data, MP data processing systems must employ a protocol to maintain memory coherence. For example, MP data processing systems utilizing PowerPC RISC processors utilize a coherency protocol having four possible states: modified (M), exclusive (E), shared (S), and invalid (I). The MESI state associated with each cache line (i.e., the line state) informs the MP data processing system what memory operations are required to maintain memory coherence following an access to that cache line. Depending upon the type of MP data processing system utilized, a memory protocol may be implemented in different ways. In snoop-bus MP data processing systems, each processor snoops transactions on the bus to determine if cached data has been requested by another processor. Based upon request addresses snooped on the bus, each processor sets the MESI state associated with each line of its cached data. In contrast, within a directory-based MP data processing system, a processor forwards memory requests to a directory at a lower level of memory for coherence ownership arbitration. For example, if a first processor (CPUa) requests data within a memory line that a second processor (CPUb) owns in exclusive state in CPUb's associated L1 cache, CPUa transmits a load request to the system memory module which stores the requested memory line. In response to the load request, the memory directory within the interrogated system memory module loads the requested memory line to CPUa and transmits a cross-interrogation message to CPUb. In response to the cross-interrogation message, CPUb will mark the requested cache line as shared in its associated L1 cache.
Among designers of MP data processing systems, there has been a recent interest in the use of load-reserve and store-conditional instructions which enable atomic accesses to memory from multiple processors while maintaining memory coherence. For example, load-reserve and store-conditional instructions on a single word operand have been implemented in the PowerPC RISC processor instruction set with the LARWX and STCWX instructions, respectively, which will be referenced as LARX and STCX. In MP data processing systems which support LARX and STCX or analogous instructions, each processor within the system includes a reservation register. When a processor executes a LARX to a variable, the processor, known as the requesting processor, loads the contents of the address storing the variable from the requesting processor's associated L1 cache into a register and the address of the memory segment containing the variable into the reservation register. Typically, the reservation address indexes a segment of memory, called a reservation granule, having a data width less than or equal to the requesting processor's L1 cache line. The requesting processor is then said to have a reservation with respect to the reservation granule. The processor may then perform atomic updates of the reserved variable utilizing store-conditional instructions.
When a processor executes a STCX to a variable contained in a reservation granule for which the processor has a reservation, the processor stores the contents of a designated register to the variable's address and then clears the reservation. If the processor does not have a reservation for the variable, the instruction fails and the memory store operation is not performed. In general, the processor's reservation is cleared if either a remote processor stores data to the address containing the reserved variable or the reserving processor executes a STCX instruction. Additional background information about load-reserve and store-conditional instructions in a multiprocessor environment may be found, for example, in Sites, et al., U.S. Pat. No. 5,193,167, which is hereby incorporated by reference.
FIG. 3 shows a flowchart of a process to complete a store operation to a cache in a multiprocessor environment, where a lock on the wordline must be acquired. When the store is to be done, the address of the wordline is loaded with a LARX (step 300 ). A comparison check is performed (step 305 ) to determine if a lock was acquired for that wordline (step 310 ). If the lock was acquired, we attempt a store (step 345 ), described below.
Assuming, however, that the lock was not acquired, because it is owned by another processor, the status register for that line is loaded (step 315 ), and the status of the wordline is checked (step 320 ) to determine when the lock is released, As long as the lock is not released (step 325 ), the process loops back to step 315 to keep checking.
When the lock is finally released (step 325 ), the processor again tries to acquire a lock. The address of the wordline is loaded with a LARX (step 330 ), and a comparison check is performed (step 335 ) to determine if a lock was acquired for that wordline (step 335 ). If the lock was acquired, the processor attempts a store (step 345 ); if not, the processor begins the process over again at step 300 .
When the lock is acquired, the store is attempted (step 345 ). If it is successful (step 350 ), the lock is released, and the processor resumes its normal programming. If, however, the store is unsuccessful, this will mean that we lost the lock; the process restarts at step 300 ).
This process is, of course, very expensive in terms of processor cycles. Because of the imbedded loops necessary to make sure that a lock is acquired before the store, a STCX generally consumes about 100 cycles.
Typically, MP data processing systems which include a memory hierarchy track the reservation state of each reservation granule utilizing a reservation protocol similar in operation to the memory coherence protocol discussed above. Such MP data processing systems generally record each processor's reservation at the system memory (main store) level. For example, each main memory module may include a reservation register for each processor that indicates which reservation granule, if any, is reserved by the associated processor. Because processor reservations are maintained at the system memory level, each execution of an instruction which affects the reservation status of a reserved granule requires that a reservation message be transmitted to the system memory module containing the target reservation granule. These reservation messages slow overall MP system performance because of the additional traffic they create on the interconnect switch or system bus and because of delays in determining if a requesting processor may successfully execute a STCX.
Consequently, it would be desirable to provide an improved method and system for memory updates in a MP data processing system in which reservations may be resolved at higher levels within the memory hierarchy, thereby minimizing reservation messaging and enhancing MP data processing system performance.
SUMMARY OF THE INVENTION
It is therefore one object of the present invention to provide an improved data processing system.
It is another object of the present invention to provide a system and method for improved cache management in a multiprocessor system.
It is yet another object of the present invention to provide a system and method using specialized cache states and state sequences to provide improved cache coherency management in a multiprocessor data processing system.
The foregoing objects are achieved as is now described.
A multiprocessor data processing system requires careful management to maintain cache coherency. Conventional systems using a MESI approach sacrifice some performance with inefficient lock-acquisition and lock-retention techniques. The disclosed system provides additional cache states, indicator bits, and lock-acquisition routines to improve cache performance. The additional cache states allow cache state transition sequences to be optimized by replacing frequently-occurring and inefficient MESI code sequences with improved sequences using modified cache states.
The above as well as additional objectives, features, and advantages of the present invention will become apparent in the following detailed written description.
BRIEF DESCRIPTION OF THE DRAWINGS
The novel features believed characteristic of the invention are set forth in the appended claims. The invention itself however, as well as a preferred mode of use, further objects and advantages thereof, will best be understood by reference to the following detailed description of an illustrative embodiment when read in conjunction with the accompanying drawings, wherein:
FIG. 1 depicts a multiprocessor data processing system in accordance with a preferred embodiment of the present invention;
FIG. 2 is a high level block diagram of a multilevel cache system within multiprocessor data processing system in accordance with a preferred embodiment of the present invention;
FIG. 3 is a flowchart of a lock-acquisition process inconventional multiprocessor systems;
FIG. 4 is a state transition table as in conventional multiprocessor systems; and
FIG. 5 is a state transition table in accordance with a preferred embodiment of the invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
With reference now to the figures and in particular with reference to FIG. 1, there is depicted a high level block diagram illustrating a multiprocessor data processing system 6 which may be utilized to implement the method and system of the present invention. As illustrated, multiprocessor data processing system 6 may be constructed utilizing multiscalar processors 10 which are each coupled to system memory 18 utilizing bus 8 . In a tightly coupled symmetric multiprocessor system, such as multiprocessor data processing system 6 , each processor 10 within multiprocessor data processing system 6 may be utilized to read from and write to memory 18 . Thus, systems and interlocks must be utilized to ensure that the data and instructions within memory 18 remain coherent.
As illustrated within FIG. 1, and as will be explained in greater detail herein, each processor 10 within multiprocessor data processing system 6 includes a level 1 (L1) cache memory 40 which may be utilized to efficiently and temporarily access and store selected instructions or data from system memory 18 via level two (L2) cache memory 20 . In view of the fact that each cache memory constitutes a memory space, it is important to maintain coherency among each L1 cache memory 40 and L2 cache memory 20 within multiprocessor data processing system 6 in order to assure accurate operation thereof.
Referring now to FIG. 2, there is depicted a high level block diagram of a multilevel cache system within multiprocessor data processing system 6 of FIG. 1, which may be utilized to implement the method and system of the present invention. As illustrated, processor 10 is coupled to bus 8 via a level two (L2) cache 20 . Level one (L1) cache 40 within processor 10 is utilized to temporarily store a small number of instructions or data which are utilized by processor 10 most frequently. The sizing and operation of cache memories is a well recognized specialty within the data processing art and is not addressed here.
In accordance with an important feature of the present invention, each time an atomic memory reference is attempted within processor 10 , a reservation flag 42 is set within processor 10 . Those skilled in the art will appreciate that this may simply constitute a single binary digit which is set to a value of either zero or one. This reservation signal is communicated to level two (L2) cache 20 and stored within a L2 reservation flag 46 therein. The setting of this reservation flag within the level two (L2) cache permits an indication that a valid reservation is pending within processor 10 . In order to achieve an atomic memory reference it will thus be necessary to advise processor 10 of any attempted writes to data which may occur at the reservation address.
A straightforward technique for accomplishing this filtering would be the transmittal from processor 10 to level two (L2) cache 20 of the reservation address; however, those skilled in the art will appreciate that this will constitute a severe degradation in processor performance. Thus, the address for which the reservation is pending, for cacheable data, is only maintained at reservation address 44 within processor 10 . In a manner which will be explained in greater detail herein, level two (L2) cache 20 may be utilized to monitor the activities of other processors within multiprocessor data processing system 6 by means of the so-called “snoop” protocol, graphically depicted at reference numeral 60 . By “snooping” bus 8 , level two (L2) cache 20 may transmit to processor 10 those attempted bus activities which may alter data at a reservation address.
Of course, certain data within multiprocessor data processing system 6 may be cache “inhibited,” that is, data which may not be stored within cache memory. In such a circumstance the setting of a reservation flag for that data will necessarily result in a “miss” within level one (L1) cache 40 and an attempted read of that data from level two (L2) cache 20 . In view of the fact that the data is cache inhibited, the address will be passed to level two (L2) cache 20 for a read operation and thus, the monitoring of activities which may alter the data at the reservation address is a simple affair, in the case of cache inhibited data. In such a situation, the reservation address may be transmitted from processor 10 to reservation address 48 within level two (L2) cache 20 . Thereafter, snoop protocol 60 may be simply utilized to monitor activities of the other processors within multiprocessor data processing system 6 which may alter the data at that reservation address.
As depicted within FIG. 2, level two (L2) cache 20 also preferably includes a read operation queue 50 which may be utilized to temporarily store read operations passed from level one (L1) cache 40 to level two (L2) cache 20 . Additionally, level one (L1) bus control 52 and level two (L2) bus control 54 may be utilized to control the communication of data between level one (L1) cache 40 and level two (L2) cache 20 and level two (L2) cache 20 and bus 8 , respectively. Further details of a system as described above may be found in U.S. Pat. No. 5,706,464, which is hereby incorporated by reference.
In conventional systems, each CPU ( 10 in FIG. 1) will maintain the current status of the cache. As an illustrative example, consider a system as in FIG. 1 with three processors: CPUa, CPUb, and CPUc. FIG. 4 shows MESI state table typical in conventional systems. Note that the line numbers are purely to aid in the discussion below. In this figure, S=a shared data state, E=exclusive ownership, M=a modified state, I=an invalid state, and T=a shared-ownership state.
In FIG. 4, in line 1 , the cache of each CPU is assumed to be in state I (hereinafter, references to the state of a CPU will simply be to the CPU's state, e.g., in line 1 , each CPU is assumed to be in state I). In line 2 , CPUc has loaded the cache with a memory line, and has exclusive ownership of the line. CPUc then performs a STCX, so it moves to a modified state in line 3 .
Next, CPUb takes ownership of the line, and is sharing the data with CPUc. The “T” state here for CPUb indicates that it owns the line, but other processors are sharing it. Next, when CPUa takes ownership of the line in line 5 , CPUb and CPUc move to a shared state.
Now assume that CPUc performs a STCX. In this case, CPUc will move to a modified state, and CPUa and CPUb are invalidated, as shown in line 6 . It should be noted here that the store by CPUc takes 100 cycles or more, as described above, to perform the snoop and the store.
Next, CPUb takes ownership of the line, and is sharing the data with CPUc, as in line 7 . Next, when CPUa takes ownership of the line in line 8 , CPUb and CPUc move to a shared state.
Now assume that CPUb performs a STCX. In this case, CPUb will move to a modified state, and CPUa and CPUc are invalidated, as shown in line 9 . Note that the store by CPUb takes 100 cycles or more, as described above, to perform the snoop and the store.
Next, CPUa takes ownership of the line, and is sharing the data with CPUb, as in line 10 . The three processors may remain in this state for some time, as CPUa and CPUb continue to read the same line without modifying it, as shown in line 11 .
Now assume that CPUb performs a STCX. In this case, CPUb will move to a modified state, and CPUa and CPUc are invalidated, as shown in line 12 . Note that the store by CPUb takes 100 cycles or more, as described above, to perform the snoop and the store.
Again, CPUa takes ownership of the line, and is sharing the data with CPUb, as in line 13 . When CPUa performs a STCX, CPUa will move to a modified state, and CPUb and CPUc are invalidated, as shown in line 12 . Again, the store by CPUa takes 100 cycles or more, as described above, to perform the snoop and the store.
Note that the conventional system illustrated by FIG. 3 shows several problems. First, note the case illustrated in lines 9 - 12 . In this case, CPUb modifies the cache twice, each time requiring a large snoop-and-store overhead, while no other processor has written that line in the interim. However, since CPUb gave up its lock, and CPUa took ownership, CPUb was forced to reacquire the lock, with the resultant overhead.
A similar problem can be seen in examining lines 13 - 14 . In this case it can be seen that CPUb modifies the cache in line 12 , CPUa and CPUb then share then cache, and then CPUa modifies it. Here, it should be clear that both CPUa and CPUb will probably require repeated STCX operations to the same cache line; instead of requiring that each STCX operation incur the overhead of a lock-acquisition process, it would be preferable if one processor could perform several modifications without giving up the lock.
Next, note that the conventional process to acquire the lock, as described above, can be very expensive. While a figure of 100 cycles is typically used, in many cases, the time spent trying to acquire a lock (in a conventional system as in FIG. 3) may be much higher.
The preferred embodiment presents several improvements over conventional systems. Three new processor states are introduced, as described below, a lock release flag bit is added, and the code sequence for cache coherency and lock acquisition is optimized.
FIG. 5 shows an optimized state table incorporating new states M 1 , M 2 , and M 3 . Note that the line numbers are purely to aid in the discussion below. In this figure, S=a shared data state, E=exclusive ownership, I=an invalid state, and T=a shared-ownership state. The new states are:
M 1 A speculative lock-acquired modified state. Until released, no other CPU may take ownership of the cache line.
M 2 A modified state which indicates that the speculative lock is released.
M 3 A modified state of fixed duration, which prevents “bouncing” between two CPUs.
In FIG. 5, in line 1 , the cache of each CPU is assumed to be in state I. In line 2 , CPUc has loaded the cache with a memory line, and has exclusive ownership of the line.
CPUc then performs a STCX, so it moves to a modified state in line 3 . Note that here, the modified state is new state M 1 . This new state acquires the lock to modify the cache line, modifies it, then prevents any other CPU from taking ownership. Other CPUs are invalidated.
Next, CPUb loads the cache line, in line 4 . Instead of granting CPUb ownership (T state) and moving CPUc to a shared state (S state), CPUc retains ownership, by moving to T state, and allows CPUb to share the line (S state). When CPUa tries to take ownership in line 5 , the same thing happens, leaving CPUc in T state, with CPUa and CPUb in S state.
In line 6 of FIG. 5, CPUc performs another STCX, and transitions to new modified state M 2 . Here, the store and transition is very fast; since CPUc had never given up ownership of the cache line, the snoop routine is not necessary, saving 100 cycles or more. The M 2 state also includes a lock-release, so that another CPU can hereafter take the cache line. Since a STCX has been performed, all other CPUs are invalidated.
Next, in line 7 of FIG. 5, CPUb takes ownership of the cache line, and goes into new state M 3 . State M 3 does not actually modify the cache line, but merely holds ownership of the cache line for a fixed amount of time, while forcing the other processors to remain in Invalid state. This action prevents CPUa or CPUc from trying to acquire the cache line and causing the “bouncing” effect described above.
CPUb may now execute a STCX and move directly into state M 1 , as shown in line 8 ; this is a very fast transition with no snooping required, since the previous M 3 state held the other CPUs in an Invalid state. Again, at least 100 cycles are saved. Of course, since a STCX has occurred, other CPUs have been held in Invalid state.
As described above with relation to CPUc in lines 3 - 6 , from the M 1 state, CPUb retains ownership of the cache line but allows other processors, here CPUa, to share it, as in line 9 . Next, CPUb executes a STCX with a lock release, and moves into state M 2 , as shown in line 10 .
Finally, in line 11 , another CPU, here CPUa, can take ownership of the cache line. When it does so, it again goes into state M 3 to allow it to make the stores it needs to without risking an alternating ownership bounce between different processors.
Of course, while the above exemplary state tables have been drawn to a three-processor system, the described state transitions apply to systems with any number of processors.
The three new cache states described above are advantageous when used alone, but provide the greatest increase in efficiency when used in combination.
In the preferred embodiment, a flag bit is added to the store/STCX command to indicate that it is a lock release. In this way, it is easy to differentiate between state M 2 and other store functions. By doing so, the snoop routine can be eliminated or shortened, since it is explicit when a CPU has given up its lock on a cache line.
Further, in the preferred embodiment, the snoop routine is cut short any time it takes more than 100 cycles. If a CPU attempts a store, and has not successfully acquired a lock on the cache line within 100 cycles, it gives up. The CPU may then continue processing other threads or performing other functions, and can retry acquiring the cache line after a delay period.
It is important to note that while the present invention has been described in the context of a fully functional data processing system and/or network, those skilled in the art will appreciate that the mechanism of the present invention is capable of being distributed in the form of a computer usable medium of instructions in a variety of forms, and that the present invention applies equally regardless of the particular type of signal bearing medium used to actually carry out the distribution. Examples of computer usable mediums include: nonvolatile, hard-coded type mediums such as read only memories (ROMs) or erasable, electrically programmable read only memories (EEPROMs), recordable type mediums such as floppy disks, hard disk drives and CD-ROMs, and transmission type mediums such as digital and analog communication links.
While the invention has been particularly shown and described with reference to a preferred embodiment, it will be understood by those skilled in the art that various changes in form and detail may be made therein without departing from the spirit and scope of the invention.
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A multiprocessor data processing system requires careful management to maintain cache coherency. Conventional systems using a MESI approach sacrifice some performance with inefficient lock-acquisition and lock-retention techniques. The disclosed system provides additional cache states, indicator bits, and lock-acquisition routines to improve cache performance. The additional cache states allow cache state transition sequences to be optimized by replacing frequently-occurring and inefficient MESI code sequences with improved sequences using modified cache states.
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FIELD OF THE INVENTION
The invention relates to pre-printed direct mail articles having front and rear cover sheets and one or more interior pages.
BACKGROUND OF THE INVENTION
Traditional direct mail articles take the form of an outer envelope containing one or more lettersheets, one or more reply devices and a business reply envelope. One or more of the enclosures can be personalized with the addressee's name, address and/or other demographic information. Direct mail articles have also been produced in the form of a single over-sized sheet printed on card stock that can be transmitted through the mail without an outer envelope or other wrapper. The over-sized sheet can be provided with a preformed business reply envelope and one or more reply devices. Direct mail articles of the self-mailing type are described in U.S. patent application Ser. No. 08/449,345, now U.S. Pat. No. 5,797,541.
The over-sized format is particularly effective in promoting magazine subscriptions and the like, since the cover of a current edition or a specialized replica of the magazine's cover can be reproduced to attract the attention and appeal to the interest of the addressee as the incoming mail is being examined. Although the immediate impact of the over-sized self-mailer makes the format desirable, the information that can be provided by the sponsor of the mailing is limited by the fact that the single sheet has only the obverse of the cover page to provide relevant information or other copy to induce the addressee to favorably respond to the solicitation.
It is therefore an object of this invention to provide a novel and improved direct mail article that is a self-mailer which has a plurality of pages for receiving printed fields and that is provided with a detachable business reply envelope and one or more integral detachable reply devices that can be inserted into the reply envelope, or alternatively, that can be used independently as reply postcards, all of which elements are produced from a single integral web or sheet of paper or printable stock.
It is another object of the invention to provide a direct mail article and a method for its manufacture that comprise a pair of large letter size or over-sized cover sheets joined along an intermediate fold line in the form of a brochure containing one or more interior sheets bound to the cover sheets, and that further includes a completely preformed business reply envelope that is detachably connected to an interior sheet and at least one reply device for use by the recipient, that can be detached from one of the cover or interior sheets.
A further object of the invention is to provide an efficient method for the mass production of a self-mailing direct mail article in the form of a brochure with one or more interior sheets from which a preformed reply envelope and at least one reply device can be removed for use by the recipient.
It is yet another important object of the invention to provide an improved direct mail article as described above that can be personalized with the recipient's name, address and/or other available demographic information in printed fields located on interior pages on the detachable reply devices and reply envelope, by means of a computer-directed (computer printer during printing of the web.
SUMMARY OF THE INVENTION
The above and other objects and advantages are achieved in a preprinted personalized direct mail article comprising a front and a rear cover sheet joined along a longitudinal fold line, at least one interior sheet for carrying printed informational fields that is approximately the same size as the cover sheets, and a preformed business reply envelope ("BRE") that is detachably joined to one of the at least one interior sheets. In a preferred embodiment of the invention, at least one detachable reply device of a size that will fit easily into the pocket of the BRE is formed, as by being defined by lines of perforations, in one or both of the cover sheets, and/or in one or more of the at least one interior sheets. The at least one interior sheet and detachable BRE are bound to the interior of the cover sheets along the longitudinal fold line. The binding can be by adhesive or by wire stitching or staples.
In one preferred embodiment, the detachable BRE is joined to the interior sheet by an intermediate longitudinal strip that is contiguous to the BRE flap and front panel, and the BRE and interior sheet are bound to the inside of the cover sheets by adhesive applied to this intermediate longitudinal strip.
In order to assure the safe passage of the direct mail article of the invention through the mails, releasable edge sealing means are employed to join the cover sheets. The sealing means can include a wafer seal, beads of releasable adhesive, staples and the like.
In the preferred embodiment of the invention, the direct mail article is produced from an integral preprinted web of paper or other printable stock. If the detachable reply device is to be a self-mailable reply postcard, then the entire web stock must be of a paper board of sufficient thickness to meet the regulations of the U.S. Postal Service; or the area from which the detachable reply device is to be removed can be formed from a double thickness of adhesively bound paper in accordance with methods known in the art.
The integral web is preferably printed in several fields with the recipient's personalized information, which can include demographic references. Personalization data is preferably printed on the reply device, on the BRE, and in context in the printed fields on the cover sheets and/or on one or more pages of the at least one interior sheets.
In a further preferred embodiment, the direct mail article of the invention produced with more than one interior page. By extending the length of the preprinted integral web, additional interior panels can be accordion or fan folded, or folded by overlapping the panels to a superposed position on the interior of the cover sheets. Each additional interior panel will provide two sheets joined along a longitudinal fold line, for a total of four additional pages.
In the practice of the method of the invention to produce a direct mail article having front and rear cover sheets and a single interior sheet with a detachable BRE, the method comprises the steps of:
a. providing a preprinted web defined by transverse top and bottom edges and spaced apart longitudinal edges, a first transverse fold line between the top and bottom edges that divides the web into a cover panel and an interior panel, a longitudinal fold line between the longitudinal edges of the web that divides the cover panel into front and rear cover sheets and that divides the interior panel into an interior sheet and an envelope panel, a longitudinal envelope parting line extending between the first transverse fold line and the top edge of the web, said envelope panel comprising an envelope flap defined by a second transverse fold line, the envelope panel; and front and rear envelope panels between the second fold line and the top edge of the web;
b. separating the rear envelope panel from the interior sheet along the longitudinal envelope parting line;
c. applying adhesive to the longitudinal edges of the envelope front panel, or envelope rear panel, or both;
d. applying a remoistenable adhesive to the envelope flap;
e. perforating the longitudinal envelope parting line;
f. folding the envelope rear panel along the third transverse fold line into superposed mating contact with the envelope front panel, applying adhesive to the cover sheet proximate the longitudinal fold line, thereby bonding their longitudinal edges to form an envelope pocket;
g. folding the web along the first transverse fold line to superpose the interior sheet and preformed envelope on the cover panel;
h. securing the interior sheet and envelope to the cover panel;
i. folding the cover panel along the longitudinal fold line to position the interior sheet and preformed envelope inside the front and rear cover sheets; and
j. cutting the folded web along the transverse fold line to separate the cover panel from the interior sheet and the envelope flap.
As will be understood from the above description by one of ordinary skill in the art, the one or more interior sheets can be of the same or a size different than the cover sheets, and the width of the BRE can be varied within the limitation of the width of the cover sheets. To maximize the effectiveness of the article for such uses as magazine or newspaper subscription solicitations, the cover sheets can be letter sized, or even larger. No other wrapper or cover, such as the transparent plastic film that is used with some magazines and catalogs is required, since the edges of the closed cover sheets can be joined with a releasable sealing means, such as a wafer seal.
Where more than one interior sheet is added, the bottom and top edges of the superposed panels will have to be trimmed to provide separate pages. The layout of the original integral web from which the eventual independent, personalized elements are to be formed can be varied and is well within the routine skill of the art.
BRIEF DESCRIPTION OF THE DRAWINGS
In further describing the invention, reference will be made to the drawings and the following figures in which the same number is used to refer to like elements:
FIG. 1 is a plan view of a web for use in the method of manufacture in accordance with one preferred embodiment of the invention;
FIG. 2 is a perspective view of the web of FIG. 1 illustrating schematically an intermediate step in the manufacture;
FIG. 3 is a perspective view of the web of FIG. 2 at a further intermediate step of manufacture;
FIG. 4 is a perspective view of the web of FIG. 3 illustrating schematically a further intermediate step of manufacture;
FIG. 5 is a side view taken along line V--V in FIG. 4 after the folding step has been completed and schematically illustrates the trimming along the transverse fold line;
FIG. 6 is a front and top perspective view of the finished direct mail article illustrated in FIGS. 1-5;
FIG. 7 is a plan view of a web for use in the manufacture of another preferred embodiment of the invention;
FIG. 8 is a front and top perspective view of the finished direct mail article produced from the web of FIG. 7;
FIG. 9 is a plan view of a web for use in the method of manufacture in accordance with another preferred embodiment of the invention having a plurality of interior sheets for receiving printed informational fields; and
FIG. 10 is a front and top perspective view of the embodiment of the invention produced from the web of FIG. 9.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
With reference to the drawings, in which like elements are referred to by the same number, FIG. 1 illustrates a web 10 of preprinted stock adapted for use in the method of the mass production of one embodiment of a direct mail article of the invention. As will be appreciated by one of ordinary skill in the art, the web 10 will be cut from a continuous web of paper (not shown) which can be in the form of a roll that can have line holes to facilitate the movement and control of the web through high speed, computer-directed printers and the subsequent processing steps which result in web 10. It will also be understood that in the practice of the method and preparation of the web or form blank 10 that the addition of elements, such as perforations, adhesive, fold lines and the like can be accomplished in sequences other than those that are specifically described below, which sequence can be dependent on factors unrelated to the invention, including the manufacturing equipment used, the layout or arrangement of the equipment, and the particular embodiment of the invention, to name but a few.
As illustrated in FIG. 1, web or form blank 10 is defined by top transverse edge 12, bottom transverse edge 14 and longitudinal edges 16, 16', and is divided by transverse fold line into upper interior panel 24 and lower cover panel 26. Longitudinal fold line 18 divides interior panel 24 into interior sheet 28 and envelope panel 30, and cover panel 26 into front and rear cover sheets 26A and 26B, respectively. As illustrated in FIG. 1, the transverse and longitudinal fold lines are positioned to provide quadrants 26A, 26B, 28 and 30 of essentially the same size. By shifting either or both of the transverse or longitudinal fold lines, the relative sizes of the interior sheet, envelope, front and rear covers can be varied; however, since all elements are produced from a single preprinted and personalized integral sheet, none of the eventually independent elements can be mismatched with differing personalized pages.
In the practice of the method, as illustrated in FIGS. 1 and 2, envelope panel 30 is divided by fold line 40 to define a flap 32 to which remoistenable adhesive 33 is applied; and by fold line 42 into envelope front panel 34 and rear panel 36. The longitudinal edges of either the front panel 34 (as shown), or rear panel 36, or both, are provided with adhesive 44. Rear panel 36 is separated from interior sheet 28 along longitudinal envelope parting line 19, as by die-cutting, and as shown in FIG. 2, is folded into superposed position on front panel 34 to form the envelope pocket and the preformed envelope 38. Longitudinal envelope parting line 19 is also provided with perforations 37 along envelope flap 32 and front panel 34 to enable the preformed envelope 38 to be easily separated for use by the recipient. In this embodiment, the envelope parting line 19 coincides with longitudinal fold line 18.
With continued reference to FIG. 1, a reply device 50, conveniently defined by intersecting and longitudinal perforation lines 52 and 54, is positioned in the comer of rear cover sheet 26B. The reply device 50, and additional reply devices (not shown), can be similarly defined in the front cover and/or in the interior sheet 28. The size of reply device 50 relative to the pocket in preformed envelope 38, permits the recipient to place the detached reply device 50 in the envelope pocket for mailing. If it is desired to provide a self-mailable postcard reply device, the layout of web 10 is provided with an additional section or panel (not shown) that can be superposed on web 10 to provide a multiple thickness of paper bound by adhesive.
Also as shown in FIG. 2, a bead of adhesive 48 is applied to front cover sheet 26A for eventual contact with interior panel 24. With reference to FIG. 3, interior sheet 28 and preformed envelope 38 are folded along transverse fold line 20 to superpose them on, and bind them to cover panel 26. In this embodiment, adhesive 48 is applied proximate longitudinal fold line 18 on the front cover panel so that preformed envelope 38 can be detached by the recipient. Alternatively, adhesive 48 can be replaced by one or more wire stitches or staples (not shown) to bind panels 24 and 26 during transit through the mail.
As illustrated in FIG. 4, the superposed panels are folded along longitudinal fold line 18 to close cover sheets 26A and 26B over interior sheet 18 and envelope 38. A pair of wafer seals 60 are shown attached to, and partially extending from front cover sheet 26A. FIG. 5 illustrates the step of trimming away a narrow section of the cover sheets, envelope flap 36 and the interior sheet 28 adjacent the transverse fold line 20, using, for example, scissor wheels 70. Thereafter, the free ends of wafer seals 60 are folded to contact the rear cover sheet to secure the edges for mailing. Upon receipt, the wafer seals are severed and the covers opened to provide the article illustrated in FIG. 6. The envelope 38 is separated along longitudinal envelope parting line 19 and reply device 50 is removed along the intersecting perforation lines 52 and 54 for insertion in the envelope.
In a second preferred embodiment illustrated in FIGS. 7 and 8, the web 70 is provided with an envelope parting line 19 that is displaced from the longitudinal fold line 18 in the direction of the envelope panel 30, the relation and description of the other elements being essentially as set forth above in connection with FIG. 1. The section of web 70 defined by fold line 18, parting line 19, third transverse fold line 42 and top edge 12 is removed, for example, as by die cutting. Adhesive 48 is applied to the web in the area or section 71 defined by the fold line 18 and parting line 19 adjacent envelope flap 32 and front panel 34. The web is thereafter processed, folded and cut as described above in connection with FIGS. 1-6, resulting in the embodiment of the direct mail article illustrated in FIG. 8. In this embodiment, the interior sheet 28 is secured on the interior of the cover sheets 26A and 26B by virtue of its being attached to the adhesively bound section 39 of envelope panel 30. Upon receipt, envelope 38 is removed by severing along perforation line 37 in the envelope parting line 19.
A third embodiment of the invention is illustrated in FIGS. 9 and 10, where web 90 is provided with second interior panel 29 defined by fourth and fifth transverse fold lines 46 and 47. Second interior panel 29 is comprised of second and third interior sheets, 29A and 29B, respectively, which provide four additional pages for receiving printed fields. The envelope panel 30 is configured in the same manner as described in the embodiment of FIGS. 7 and 8. Beads of adhesive 48, 48' are applied as indicated adjacent to, and along, longitudinal fold line 18.
As will be apparent to one of ordinary skill in the art, the panels 26 and 29 can either be fan folded into superposed position on the interior pages of cover panel 24, or panel 26 can be folded to align top edge 12 with fifth transverse fold line 47, followed by folding along fold line 47. Thereafter, the superposed panels are trimmed along the fold lines to separate the cover and interior sheets from each other. The embodiment shown in FIG. 10 results from fan folding of the panels to position the envelope 38 at the center fold of the folio.
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A method is provided for manufacturing a personalized direct mail article requiring no envelope or other wrapper in the format of an oversized brochure having front and rear cover sheets, at least one interior sheet and a detachable preformed business reply envelope and at least one detachable reply device, all of which are joined to the cover sheets during mailing and all of which are formed from a single integral web to insure that there can be no mismatching of the several personalized elements forming the article.
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CROSS-REFERENCE TO RELATED APPLICATION
This patent application is a continuation of U.S. patent application Ser. No. 11/506,689, filed Aug. 17, 2006, now U.S. Pat. No. 7,351,712, which is a continuation of U.S. patent application Ser. No. 10/733,215, filed Dec. 11, 2003, now U.S. Pat. No. 7,109,335, which claims the benefit of priority to U.S. Provisional Patent Application Ser. No. 60/500,742, filed Sep. 5, 2003 and U.S. Provisional Patent Application Ser. No. 60/435,670, filed Dec. 20, 2002.
BACKGROUND OF THE INVENTION
This invention relates to novel pyrimidine derivatives that are useful in the treatment of abnormal cell growth, such as cancer, in mammals. This invention also relates to a method of using such compounds in the treatment of abnormal cell growth in mammals, especially humans, and to pharmaceutical compositions containing such compounds.
It is known that a cell may become cancerous by virtue of the transformation of a portion of its DNA into an oncogene (i.e., a gene which, on activation, leads to the formation of malignant tumor cells). Many oncogenes encode proteins that are aberrant tyrosine kinases capable of causing cell transformation. Alternatively, the overexpression of a normal proto-oncogenic tyrosine kinase may also result in proliferative disorders, sometimes resulting in a malignant phenotype.
Receptor tyrosine kinases are enzymes which span the cell membrane and possess an extracellular binding domain for growth factors such as epidermal growth factor, a transmembrane domain, and an intracellular portion which functions as a kinase to phosphorylate specific tyrosine residues in proteins and hence to influence cell proliferation. Other receptor tyrosine kinases include c-erbB-2, c-met, tie-2, PDGFr, FGFr, and VEGFR. It is known that such kinases are frequently aberrantly expressed in common human cancers such as breast cancer, gastrointestinal cancer such as colon, rectal or stomach cancer, leukemia, and ovarian, bronchial or pancreatic cancer. It has also been shown that epidermal growth factor receptor (EGFR), which possesses tyrosine kinase activity, is mutated and/or overexpressed in many human cancers such as brain, lung, squamous cell, bladder, gastric, breast, head and neck, oesophageal, gynecological and thyroid tumors.
Accordingly, it has been recognized that inhibitors of receptor tyrosine kinases are useful as selective inhibitors of the growth of mammalian cancer cells. For example, erbstatin, a tyrosine kinase inhibitor, selectively attenuates the growth in athymic nude mice of a transplanted human mammary carcinoma that expresses epidermal growth factor receptor tyrosine kinase (EGFR) but is without effect on the growth of another carcinoma that does not express the EGF receptor. Thus, selective inhibitors of certain receptor tyrosine kinases, are useful in the treatment of abnormal cell growth, in particular cancer, in mammals. In addition to receptor tyrosine kinses, selective inhibitors of certain non-receptor tyrosine kinases, such as FAK (focal adhesion kinase), Ick, src, abl or serine/threonine kinases (e.g.: cyclin dependent kinases, are useful in the treatment of abnormal cell growth, in particular cancer, in mammals. FAK is also known as the Protein-Tyrosine Kinase 2, PTK2.
Convincing evidence suggests that FAK, a cytoplasmic, non-receptor tyrosine kinase, plays an essential role in cell-matrix signal transduction pathways (Clark and Brugge 1995, Science 268: 233-239) and its aberrant activation is associated with an increase in the metastatic potential of tumors (Owens et al. 1995, Cancer Research 55: 2752-2755). FAK was originally identified as a 125 kDa protein highly tyrosine-phosphorylated in cells transformed by v-Src. FAK was subsequently found to be a tyrosine kinase that localizes to focal adhesions, which are contact points between cultured cells and their underlying substratum and sites of intense tyrosine phosphorylation. FAK is phosphorylated and, thus, activated in response to extracellular matrix (ECM)-binding to integrins. Recently, studies have demonstrated that an increase in FAK mRNA levels accompanied invasive transformation of tumors and attenuation of the expression of FAK (through the use of antisense oligonucleotides) induces apoptosis in tumor cells (Xu et al. 1996, Cell Growth and Diff. 7: 413-418). In addition to being expressed in most tissue types, FAK is found at elevated levels in most human cancers, particularly in highly invasive metastases.
Various compounds, such as styrene derivatives, have also been shown to possess tyrosine kinase inhibitory properties. Five European patent publications, namely EP 0 566 226 A1 (published Oct. 20, 1993), EP 0 602 851 A1 (published Jun. 22, 1994), EP 0 635 507 A1 (published Jan. 25, 1995), EP 0 635 498 A1 (published Jan. 25, 1995), and EP 0 520 722 A1 (published Dec. 30, 1992), refer to certain bicyclic derivatives, in particular quinazoline derivatives, as possessing anti-cancer properties that result from their tyrosine kinase inhibitory properties.
Also, World Patent Application WO 92/20642 (published Nov. 26, 1992), refers to certain bis-mono and bicyclic aryl and heteroaryl compounds as tyrosine kinase inhibitors that are useful in inhibiting abnormal cell proliferation. World Patent Applications WO96/16960 (published Jun. 6, 1996), WO 96/09294 (published Mar. 6, 1996), WO 97/30034 (published Aug. 21, 1997), WO 98/02434 (published Jan. 22, 1998), WO 98/02437 (published Jan. 22, 1998), and WO 98/02438 (published Jan. 22, 1998), also refer to substituted bicyclic heteroaromatic derivatives as tyrosine kinase inhibitors that are useful for the same purpose.
U.S. Patent Application Ser. No. 60/435,670, filed Dec. 20, 2002 relates to a broad class of novel pyrimidine derivatives that are selective inhibitors of FAK. As such, these compounds are useful in the treatment of abnormal cell growth.
Accordingly, a need exists for additional selective inhibitors of certain receptor and non-receptor tyrosine kinases, useful in the treatment of abnormal cell growth, such as cancer, in mammals. The present invention provides for novel pyrimidine derivatives that are selective inhibitors of the non-receptor tyrosine kinase, FAK, and are useful in the treatment of abnormal cell growth.
SUMMARY OF THE INVENTION
The present invention relates to a compound of the formula 1
or a pharmaceutically acceptable salt, solvate, hydrate, or prodrug thereof,
wherein n is an integer from 1 to 3;
each R 1 is a substituent independently selected from the group consisting of hydrogen, hydroxy, —(C 1 -C 6 )alkyl, —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —O(C 1 -C 6 )alkyl, —O(C 3 -C 7 )cycloalkyl, —O(C 2 -C 9 )heterocyclyl, —NR 5 R 6 , —SR 7 , —SOR 7 , —SO 2 R 7 , —CO 2 R 5 , —CONR 5 R 6 , —SO 2 NR 5 R 6 , —NHCOR 5 , —NR 5 CONR 5 R 6 , and —NR 5 SO 2 R 7 ; with the proviso that a heteroatom of the foregoing R 1 substituents may not be bound to an sp 3 carbon atom bound to another heteroatom; and said R 1 substituents, —(C 1 -C 6 )alkyl, —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —O(C 1 -C 6 )alkyl, —O(C 3 -C 7 )cycloalkyl, —O(C 2 -C 9 )heterocyclyl, —NR 5 R 6 , —SR 7 , —SOR 7 , —SO 2 R 7 , —CO 2 R 5 , —CONR 5 R 6 , —SO 2 NR 5 R 6 , —NHCOR 5 , —NR 5 CONR 5 R 6 , and —NR 5 SO 2 R 7 groups are optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —CF 3 , —CN, —(C 1 -C 6 )alkyl, —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 and —CONR 5 R 8 ; with the proviso that a heteroatom of the foregoing optional R 1 moieties may not be bound to an sp 3 carbon atom bound to another heteroatom;
each R 2 is a substituent independently selected from the group consisting of hydrogen, —(C 1 -C 6 )alkyl, —(C 2 -C 6 )alkenyl, —(C 2 -C 6 )alkynyl, —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , and —CONR 5 R 6 ; with the proviso that a heteroatom of any of the foregoing R 2 substituents may not be bound to an sp 3 carbon atom that is bound to another heteroatom; and said R 2 substituents, —(C 1 -C 6 )alkyl, —(C 2 -C 6 )alkenyl, —(C 2 -C 6 )alkynyl, —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , and —CONR 5 R 6 , are optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —CF 3 , —NO 2 , —CN, —(C 1 -C 6 )alkyl, —(C 2 -C 6 )alkenyl, —(C 2 -C 6 )alkynyl, —C═N—OH, —C═N—O((C 1 -C 6 )alkyl), —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 , —CONR 5 R 8 , —SR 7 , —SOR 7 , —SO 2 R 7 , —SO 2 NR 5 R 6 , —NHCOR 5 , —NR 5 CONR 5 R 6 , and —NR 5 SO 2 R 7 , wherein said —(C 2 -C 6 )alkenyl and —(C 2 -C 6 )alkynyl R 2 moieties may be optionally substituted by one to three R 5 groups; and with the proviso that a heteroatom of the foregoing optional R 2 moieties may not be bound to an sp 3 carbon atom bound to another heteroatom;
R 1 and R 2 may be taken together with the atom(s) to which they are attached to form a cyclic group, —(C 3 -C 10 )cycloalkyl or —(C 2 -C 9 )heterocyclyl, wherein said cyclic group is optionally substituted by one to three moieties selected from the group consisting of hydrogen, halogen, hydroxy, —CF 3 , —NO 2 , —CN, —(C 1 -C 6 )alkyl, —(C 2 -C 6 )alkenyl, —(C 2 -C 6 )alkynyl, —C═N—OH, —C═N—O((C 1 -C 6 )alkyl), —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 , —CONR 5 R 8 , —SR 7 , —SOR 7 , —SO 2 R 7 , —SO 2 NR 5 R 6 , —NHCOR 5 , —NR 5 CONR 5 R 6 , and —NR 5 SO 2 R 7 , wherein said —(C 2 -C 6 )alkenyl and —(C 2 -C 6 )alkynyl moieties of said cyclic group may be optionally substituted by one to three R 5 groups, and said cyclic group is optionally interrupted by one to three elements selected from the group consisting of —(C═O), —SO 2 , —S—, —O—, —N—, —NH— and —NR 5 , with the proviso that any of the foregoing cyclic group moieties or elements may not be bound to an sp 3 carbon atom that is bound to another heteroatom;
R 3 is a suitable substituent, including, but not limited to a substituent selected from the group consisting of:
(a) hydrogen; (b) —(C 6 -C 10 )aryl or —(C 1 -C 9 )heteroaryl, optionally substituted by one to three moieties independently selected from the group consisting of halogen, hydroxy, —(C 1 -C 6 )alkyl, —(C 1 -C 6 )alkyl-P(O)(O(C 1 -C 6 )alkyl) 2 , —(C 3 -C 10 )cycloalkyl, (C 6 -C 10 )aryl, (C 2 -C 9 )heterocyclyl, —(C 1 -C 9 )heteroaryl, —NR 5 R 6 , —N H SO 2 (C 1 -C 6 )alkyl, —NHSO 2 (C 3 -C 6 )cycloalkyl, —N((C 1 -C 6 )alkyl)(SO 2 —C 1 -C 6 )alkyl), —N((C 1 -C 6 )alkyl)(SO 2 (C 3 -C 6 )cycloalkyl), —O(C 1 -C 6 )alkyl, —O—SO 2 (C 1 -C 6 )alkyl, —(CO)(C 1 -C 6 )alkyl, —(CO)CF 3 , —(CO)(C 3 -C 10 )cycloalkyl, —(CO)(C 6 -C 10 )aryl, —(CO)(C 2 -C 9 )heterocyclyl, —(CO)(C 1 -C 9 )heteroaryl, —(CO)O(C 1 -C 6 )alkyl, —(CO)O(C 3 -C 10 )cycloalkyl, —(CO)O(C 6 -C 10 )aryl, —(CO)O(C 2 -C 9 )heterocyclyl, —(CO)O(C 1 -C 9 )heteroaryl, —(CO)(C 1 -C 6 )alkyl-O(C 1 -C 6 )alkyl, —SO 2 (C 1 -C 6 )alkyl, —SO 2 (C 3 -C 6 )cycloalkyl, SO 2 CF 3 , SO 2 NH 2 , SO 2 NH(C 1 -C 6 )alkyl, —SO 2 NH(C 3 -C 6 )cycloalkyl, —SO 2 N((C 1 -C 6 )alkyl) 2 , —SO 2 N((C 3 -C 6 )cycloalkyl) 2 , —SO 2 NR 5 R 6 , and —SO 2 N(C 1 -C 6 )alkyl-(C 6 -C 10 )aryl; wherein said —(C 6 -C 10 )aryl or —(C 1 -C 9 ) heteroaryl are optionally interrupted by one to three elements selected from the group consisting of —(C═O), —SO 2 , —S—, —O—, —N—, —NH— and —NR 5 ; and R 5 and R 6 of said NR 5 R 6 R 3 (b) group may be taken together with the atoms to which they are attached to form a —(C 2 -C 9 )heterocyclyl; (c) —(C 3 -C 10 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, and —(C 1 -C 6 )alkyl-(C 2 -C 9 ) heterocyclyl, optionally substituted by one to three moieties independently selected from the group consisting of halogen, hydroxy, —(C 1 -C 6 )alkyl, —(C 1 -C 6 )alkyl-P(O)(O(C 1 -C 6 )alkyl) 2 , —(C 3 -C 10 )cycloalkyl, (C 6 -C 10 )aryl, (C 2 -C 9 )heterocyclyl, —(C 1 -C 9 )heteroaryl, —NR 5 R 6 , —NSO 2 (C 1 -C 6 )alkyl, —NHSO 2 (C 3 -C 6 )cycloalkyl, —N((C 1 -C 6 )alkyl)(SO 2 —C 1 -C 6 )alkyl), —N((C 1 -C 6 )alkyl)(SO 2 (C 3 -C 6 )cycloalkyl), —O(C 1 -C 6 )alkyl, —O—SO 2 (C 1 -C 6 )alkyl, —O—SO 2 (C 1 -C 6 )alkyl, —(CO)(C 1 -C 6 )alkyl, —(CO)CF 3 , —(CO)(C 3 -C 10 )cycloalkyl, —(CO)(C 6 -C 10 )aryl, —(CO)(C 2 -C 9 )heterocyclyl, —(CO)(C 1 -C 9 )heteroaryl, —(CO)O(C 1 -C 6 )alkyl, —(CO)O(C 3 -C 10 )cycloalkyl, —(CO)O(C 6 -C 10 )aryl, —(CO)O(C 2 -C 9 )heterocyclyl, —(CO)O(C 1 -C 9 )heteroaryl, —(CO)(C 1 -C 6 )alkyl-O(C 1 -C 6 )alkyl, —SO 2 (C 1 -C 6 )alkyl, —SO 2 (C 3 -C 6 )cycloalkyl, SO 2 CF 3 , SO 2 NH 2 , SO 2 NH(C 1 -C 6 )alkyl, —SO 2 NH(C 3 -C 6 )cycloalkyl, —SO 2 N((C 1 -C 6 )alkyl) 2 , —SO 2 N((C 3 -C 6 )cycloalkyl) 2 , —SO 2 NR 5 R 6 , and —SO 2 N(C 1 -C 6 )alkyl-(C 6 -C 10 )aryl; wherein said —(C 3 -C 10 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, and —(C 1 -C 6 )alkyl-(C 2 -C 9 )heterocyclyl are optionally interrupted by one to three elements selected from the group consisting of —(C═O), —SO 2 , —S—, —O—, —N—, —NH— and —NR 5 ; and R 5 and R 6 of said NR 5 R 6 R 3 (b) group may be taken together with the atoms to which they are attached to form a —(C 2 -C 9 )heterocyclyl; (d) —(C 1 -C 6 )alkyl optionally substituted by one to three moieties selected from the group consisting of halogen, hydroxy, —(C 1 -C 6 )alkyl, —(C 1 -C 6 )alkyl-P(O)(O(C 1 -C 6 )alkyl) 2 , —(C 3 -C 10 )cycloalkyl, (C 6 -C 10 )aryl, (C 2 -C 9 )heterocyclyl, —(C 1 -C 9 )heteroaryl, —NR 5 R 6 , —NSO 2 (C 1 -C 6 )alkyl, —NHSO 2 (C 3 -C 6 )cycloalkyl, —N((C 1 -C 6 )alkyl)(SO 2 —C 1 -C 6 )alkyl), —N((C 1 -C 6 )alkyl)(SO 2 (C 3 -C 6 )cycloalkyl), —O(C 1 -C 6 )alkyl, —O—SO 2 (C 1 -C 6 )alkyl, —(CO)(C 1 -C 6 )alkyl, —(CO)CF 3 , —(CO)(C 3 -C 10 )cycloalkyl, —(CO)(C 6 -C 10 )aryl, —(CO)(C 2 -C 9 )heterocyclyl, —(CO)(C 1 -C 9 )heteroaryl, —(CO)O(C 1 -C 6 )alkyl, —(CO)O(C 3 -C 10 )cycloalkyl, —(CO)O(C 6 -C 10 )aryl, —(CO)O(C 2 -C 9 )heterocyclyl, —(CO)O(C 1 -C 9 )heteroaryl, —(CO)(C 1 -C 6 )alkyl-O(C 1 -C 6 )alkyl, —SO 2 (C 1 -C 6 )alkyl, —SO 2 (C 3 -C 6 )cycloalkyl, SO 2 CF 3 , SO 2 NH 2 , SO 2 NH(C 1 -C 6 )alkyl, —SO 2 NH(C 3 -C 6 )cycloalkyl, —SO 2 N((C 1 -C 6 )alkyl) 2 , —SO 2 N((C 3 -C 6 )cycloalkyl) 2 , —SO 2 NR 5 R 6 , and —SO 2 N(C 1 -C 6 )alkyl-(C 6 -C 10 )aryl; wherein said —(C 1 -C 6 )alkyl is optionally interrupted by one to three elements selected from the group consisting of —(C═O), —SO 2 , —S—, —O—, —N—, —NH— and —NR 5 ; and R 5 and R 6 of said NR 5 R 6 R 3 (b) group may be taken together with the atoms to which they are attached to form a —(C 2 -C 9 )heterocyclyl;
and wherein each R 3 (b)-(d) substituent, moiety, or element is optionally substituted by one to three radicals independently selected from the group consisting of hydrogen, halogen, hydroxy, —CF 3 , —NO 2 , —CN, —(C 1 -C 6 )alkyl, —(C 2 -C 6 )alkenyl, —(C 2 -C 6 )alkynyl, —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —(C 6 -C 10 )aryl, —(C 1 -C 9 )heteroaryl, —O(C 1 -C 6 )alkyl, —O(C 3 -C 7 )cycloalkyl, —O(C 2 -C 9 )heterocyclyl, —C═N—OH, —C═N—O(C 1 -C 6 alkyl), —NR 5 R 6 , —SR 7 , —SOR 7 , —SO 2 R 7 , —CO 2 R 5 , —CONR 5 R 6 , —SO 2 NR 5 R 6 , —NHCOR 5 , —NR 5 CONR 5 R 6 , and —NR 5 SO 2 R 7 ; with the proviso that a heteroatom of the foregoing R 3 (b)-(d) substituents, moieties, elements or radicals may not be bound to an sp 3 carbon atom bound to another heteroatom; and wherein R 5 and R 6 of said —NR 5 R 6 , —CONR 5 R 6 , —SO 2 NR 5 R 6 , and —NR 5 CONR 5 R 6 groups may be taken together with the atoms to which they are attached to form a —(C 2 -C 9 )heterocyclyl;
R 4 is a substituent selected from the group consisting of hydrogen, (C 1 -C 6 )alkyl, —(C 3 -C 7 )cycloalkyl, and —(C 2 -C 9 )heterocyclyl; wherein said (C 1 -C 6 )alkyl, —(C 3 -C 7 )cycloalkyl, and —(C 2 -C 9 )heterocyclyl R 4 substituents are optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, —(C 1 -C 6 )alkyl, —CN, —NR 5 2 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , and —CONR 5 R 8 ; with the proviso that a heteroatom of the foregoing R 4 substituents may not be bound to an sp 3 carbon atom bound to another heteroatom; and wherein R 5 and R 8 of said —CONR 5 R 8 group may be taken together with the atoms to which they are attached to form a —(C 3 -C 10 )cycloalkyl or —(C 2 -C 9 )heterocyclyl;
R 5 and R 6 are each substituents independently selected from the group consisting of hydrogen, —(C 1 -C 6 )alkyl, —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —(C 6 -C 10 )aryl, and —(C 1 -C 9 )heteroaryl; wherein said —(C 1 -C 6 )alkyl, —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —(C 6 -C 10 )aryl, and —(C 1 -C 9 )heteroaryl R 5 or R 6 substituents are optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, —CF 3 , —CN, —(C 1 -C 6 )alkyl, —NH(C 1 -C 6 )alkyl, —NH(C 3 -C 7 )cycloalkyl, —NH(C 2 -C 9 )heterocyclyl, —NH(C 6 -C 10 )aryl, —NH(C 1 -C 9 )heteroaryl, —N((C 1 -C 6 )alkyl) 2 , —N((C 3 -C 7 )cycloalkyl) 2 , —N((C 2 -C 9 )heterocyclyl) 2 , —N((C 6 -C 10 )aryl) 2 , —N((C 1 -C 9 )heteroaryl) 2 , —O(C 1 -C 6 )alkyl, —O(C 3 -C 7 )cycloalkyl, —O(C 2 -C 9 )heterocyclyl, —O(C 6 -C 10 )aryl, —O(C 1 -C 9 )heteroaryl, —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 7 , —CONH 2 , —CONHR 7 , and —CONR 7 R 8 ; with the proviso that a heteroatom of the foregoing R 5 or R 6 substituents or moieties may not be bound to an sp 3 carbon atom bound to another heteroatoms; and wherein R 7 and R 8 of said —CONR 7 R 8 group may be taken together with the atoms to which they are attached to form a —(C 1 -C 9 ) heteroaryl;
R 5 and R 6 may be taken together with the atom(s) to which they are attached to form a cyclic group, —(C 3 -C 10 )cycloalkyl or —(C 2 -C 9 )heterocyclyl, wherein said cyclic group is optionally substituted by one to three moieties selected from the group consisting of hydrogen, halogen, hydroxy, —CF 3 , —NO 2 , —CN, —(C 1 -C 6 )alkyl, —(C 2 -C 6 )alkenyl, —(C 2 -C 6 )alkynyl, —C═N—OH, —C═N—O((C 1 -C 6 )alkyl), —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocycyl, —CO 2 R 5 , —CONR 5 R 6 , —CONR 5 R 8 , —SR 7 , —SOR 7 , —SO 2 R 7 , —SO 2 NR 5 R 6 , —NHCOR 5 , —NR 5 CONR 5 R 6 , and —NR 5 SO 2 R 7 , wherein said —(C 2 -C 6 )alkenyl and —(C 2 -C 6 )alkynyl moieties of said cyclic group may be optionally substituted by one to three R 7 groups, and said cyclic group is optionally interrupted by one to three elements selected from the group consisting of —(C═O), —SO 2 , —S—, —O—, —N—, —NH— and —NR 5 , with the proviso that any of the foregoing cyclic group moieties or elements may not be bound to an sp 3 carbon atom that is bound to another heteroatom;
R 7 is a substituent selected from the group consisting of —(C 1 -C 6 )alkyl, —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —(C 6 -C 10 )aryl, and —(C 1 -C 9 )heteroaryl; wherein said —(C 1 -C 6 )alkyl, —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —(C 6 -C 10 )aryl, and —(C 1 -C 9 )heteroaryl R 7 substituents are optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —CN, —(C 1 -C 6 )alkyl, —NR 5 2 , and —O(C 1 -C 6 )alkyl, with the proviso that a heteroatom of the foregoing R 7 substituents or moieties may not be bound to an sp 3 carbon atom bound to another heteroatom;
R 8 is a substituent selected from the group consisting of hydrogen, —(C 1 -C 6 )alkyl, —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —(C 6 -C 10 )aryl, and —(C 1 -C 9 )heteroaryl; wherein said —(C 1 -C 6 )alkyl, —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —(C 6 -C 10 )aryl, and —(C 1 -C 9 )heteroaryl R 8 radicals are optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —CN, —(C 1 -C 6 )alkyl, —NH 2 , —NHR 9 , —NR 9 2 , OR 9 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 10 , —CONH 2 , —CONHR 10 , and —CONR 10 R 11 ; with the proviso that a heteroatom of the foregoing R 8 substituents or moieties may not be bound to an sp 3 carbon atom bound to another heteroatom; and wherein R 10 and R 11 of —CONR 10 R 11 may be taken together with the atoms to which they are attached to form a —(C2-C 9 )heterocyclyl;
R 9 and R 10 are each —(C 1 -C 6 )alkyl and may be taken together with the atoms to which they are attached to form a —(C 2 -C 9 )heterocyclyl; and
R 11 is hydrogen or —(C 1 -C 6 )alkyl.
In a preferred embodiment, the present invention relates to a compound of the formula 1
or a pharmaceutically acceptable salt, solvate, hydrate, or prodrug thereof,
wherein n is an integer from 1 to 3;
each R 1 is a substituent independently selected from the group consisting of hydrogen, hydroxy, —(C 1 -C 6 )alkyl, —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —O(C 1 -C 6 )alkyl, —O(C 3 -C 7 )cycloalkyl, —O(C 2 -C 9 )heterocyclyl, —NR 5 R 6 , —SR 7 , —SOR 7 , —SO 2 R 7 , —CO 2 R 5 , —CONR 5 R 6 , —SO 2 NR 5 R 6 , —NHCOR 5 , —NR 5 CONR 5 R 6 , and —NR 5 SO 2 R 7 ; with the proviso that a heteroatom of the foregoing R 1 substituents may not be bound to an sp 3 carbon atom bound to another heteroatom; and said R 1 substituents, —(C 1 -C 6 )alkyl, —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —O(C 1 -C 6 )alkyl, —O(C 3 -C 7 )cycloalkyl, —O(C 2 -C 9 )heterocyclyl, —NR 5 R 6 , —SR 7 , —SOR 7 , —SO 2 R 7 , —CO 2 R 5 , —CONR 5 R 6 , —SO 2 NR 5 R 6 , —NHCOR 5 , —NR 5 CONR 5 R 6 , and —NR 5 SO 2 R 7 groups are optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —CF 3 , —CN, —(C 1 -C 6 )alkyl, —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 and —CONR 5 R 8 ; with the proviso that a heteroatom of the foregoing optional R 1 moieties may not be bound to an sp 3 carbon atom bound to another heteroatom;
each R 2 is a substituent independently selected from the group consisting of hydrogen, —(C 1 -C 6 )alkyl, —(C 2 -C 6 )alkenyl, —(C 2 -C 6 )alkynyl, —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , and —CONR 5 R 6 ; with the proviso that a heteroatom of any of the foregoing R 2 substituents may not be bound to an sp 3 carbon atom that is bound to another heteroatom; and said R 2 substituents, —(C 1 -C 6 )alkyl, —(C 2 -C 6 )alkenyl, —(C 2 -C 6 )alkynyl, —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , and —CONR 5 R 6 , are optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —CF 3 , —NO 2 , —CN, —(C 1 -C 6 )alkyl, —(C 2 -C 6 )alkenyl, —(C 2 -C 6 )alkynyl, —C═N—OH, —C═N—O((C 1 -C 6 )alkyl), —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 , —CONR 5 R 8 , —SR 7 , —SOR 7 , —SO 2 R 7 , —SO 2 NR 5 R 6 , —NHCOR 5 , —NR 5 CONR 5 R 6 , and —NR 5 SO 2 R 7 , wherein said —(C 2 -C 6 )alkenyl and —(C 2 -C 6 )alkynyl R 2 moieties may be optionally substituted by one to three R 5 groups; and with the proviso that a heteroatom of the foregoing optional R 2 moieties may not be bound to an sp 3 carbon atom bound to another heteroatom;
R 1 and R 2 may be taken together with the atom(s) to which they are attached to form a cyclic group, —(C 3 -C 10 )cycloalkyl or —(C 2 -C 9 )heterocyclyl, wherein said cyclic group is optionally substituted by one to three moieties selected from the group consisting of hydrogen, halogen, hydroxy, —CF 3 , —NO 2 , —CN, —(C 1 -C 6 )alkyl, —(C 2 -C 6 )alkenyl, —(C 2 -C 6 )alkynyl, —C═N—OH, —C═N—O((C 1 -C 6 )alkyl), —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 , —CONR 5 R 8 , —SR 7 , —SOR 7 , —SO 2 R 7 , —SO 2 NR 5 R 6 , —NHCOR 5 , —NHCOR 5 , —NR 5 CONR 5 R 6 , and —NR 5 SO 2 R 7 , wherein said —(C 2 -C 6 )alkenyl and —(C 2 -C 6 )alkynyl moieties of said cyclic group may be optionally substituted by one to three R 5 groups, and said cyclic group is optionally interrupted by one to three elements selected from the group consisting of —(C═O), —SO 2 , —S—, —O—, —N—, —NH— and —NR 5 , with the proviso that any of the foregoing cyclic group moieties or elements may not be bound to an sp 3 carbon atom that is bound to another heteroatom;
R 3 is a substituent selected from the group consisting of:
(a) hydrogen; (c) —(C 6 -C 10 )aryl or —(C 1 -C 9 )heteroaryl, optionally substituted by one to three moieties independently selected from the group consisting of halogen, hydroxy, —(C 1 -C 6 )alkyl, —(C 1 -C 6 )alkyl-P(O)(O(C 1 -C 6 )alkyl) 2 , —(C 3 -C 10 )cycloalkyl, (C 6 -C 10 )aryl, (C 2 -C 9 )heterocyclyl, —(C 1 -C 9 )heteroaryl, —NR 5 R 6 , —N H SO 2 (C 1 -C 6 )alkyl, —NHSO 2 (C 3 -C 6 )cycloalkyl, —N((C 1 -C 6 )alkyl)(SO 2 —C 1 -C 6 )alkyl), —N((C 1 -C 6 )alkyl)(SO 2 (C 3 -C 6 )cycloalkyl), —O(C 1 -C 6 )alkyl, —O—SO 2 (C 1 -C 6 )alkyl, —(CO)(C 1 -C 6 )alkyl, —(CO)CF 3 , —(CO)(C 3 -C 10 )cycloalkyl, —(CO)(C 6 -C 10 )aryl, —(CO)(C 2 -C 9 )heterocyclyl, —(CO)(C 1 -C 9 )heteroaryl, —(CO)O(C 1 -C 6 )alkyl, —(CO)O(C 3 -C 10 )cycloalkyl, —(CO)O(C 6 -C 10 )aryl, —(CO)O(C 2 -C 9 )heterocyclyl, —(CO)O(C 1 -C 9 )heteroaryl, —(CO)(C 1 -C 6 )alkyl-O(C 1 -C 6 )alkyl, —SO 2 (C 1 -C 6 )alkyl, —SO 2 (C 3 -C 6 )cycloalkyl, SO 2 CF 3 , SO 2 NH 2 , SO 2 NH(C 1 -C 6 )alkyl, —SO 2 NH(C 3 -C 6 )cycloalkyl, —SO 2 N((C 1 -C 6 )alkyl) 2 , —SO 2 N((C 3 -C 6 )cycloalkyl) 2 , —SO 2 NR 5 R 6 , and —SO 2 N(C 1 -C 6 )alkyl-(C 6 -C 10 )aryl; wherein said —(C 6 -C 10 )aryl or —(C 1 -C 9 ) heteroaryl are optionally interrupted by one to three elements selected from the group consisting of —(C═O), —SO 2 , —S—, —O—, —N—, —NH— and —NR 5 ; and R 5 and R 6 of said NR 5 R 6 R 3 (b) group may be taken together with the atoms to which they are attached to form a —(C 2 -C 9 )heterocyclyl; (c) —(C 3 -C 10 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, and —(C 1 -C 6 )alkyl-(C 2 -C 9 ) heterocyclyl, optionally substituted by one to three moieties independently selected from the group consisting of halogen, hydroxy, —(C 1 -C 6 )alkyl, —(C 1 -C 6 )alkyl-P(O)(O(C 1 -C 6 )alkyl) 2 , —(C 3 -C 10 )cycloalkyl, (C 6 -C 10 )aryl, (C 2 -C 9 )heterocyclyl, —(C 1 -C 9 )heteroaryl, —NR 5 R 6 , —NSO 2 (C 1 -C 6 )alkyl, —NHSO 2 (C 3 -C 6 )cycloalkyl, —N((C 1 -C 6 )alkyl)(SO 2 —C 1 -C 6 )alkyl), —N((C 1 -C 6 )alkyl)(SO 2 (C 3 -C 6 )cycloalkyl), —O(C 1 -C 6 )alkyl, —O—SO 2 (C 1 -C 6 )alkyl, —O—SO 2 (C 1 -C 6 )alkyl, —(CO)(C 1 -C 6 )alkyl, —(CO)CF 3 , —(CO)(C 3 -C 10 )cycloalkyl, —(CO)(C 6 -C 10 )aryl, —(CO)(C 2 -C 9 )heterocyclyl, —(CO)(C 1 -C 9 )heteroaryl, —(CO)O(C 1 -C 6 )alkyl, —(CO)O(C 3 -C 10 )cycloalkyl, —(CO)O(C 6 -C 10 )aryl, —(CO)O(C 2 -C 9 )heterocyclyl, —(CO)O(C 1 -C 9 )heteroaryl, —(CO)(C 1 -C 6 )alkyl-O(C 1 -C 6 )alkyl, —SO 2 (C 1 -C 6 )alkyl, —SO 2 (C 3 -C 6 )cycloalkyl, SO 2 CF 3 , SO 2 NH 2 , SO 2 NH(C 1 -C 6 )alkyl, —SO 2 NH(C 3 -C 6 )cycloalkyl, —SO 2 N((C 1 -C 6 )alkyl) 2 , —SO 2 N((C 3 -C 6 )cycloalkyl) 2 , —SO 2 NR 5 R 6 , and —SO 2 N(C 1 -C 6 )alkyl-(C 6 -C 10 )aryl; wherein said —(C 3 -C 10 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, and —(C 1 -C 6 )alkyl-(C 2 -C 9 )heterocyclyl are optionally interrupted by one to three elements selected from the group consisting of —(C═O), —SO 2 , —S—, —O—, —N—, —NH— and —NR 5 ; and R 5 and R 6 of said NR 5 R 6 R 3 (b) group may be taken together with the atoms to which they are attached to form a —(C 2 -C 9 )heterocyclyl; (d) —(C 1 -C 6 )alkyl optionally substituted by one to three moieties selected from the group consisting of halogen, hydroxy, —(C 1 -C 6 )alkyl, —(C 1 -C 6 )alkyl-P(O)(O(C 1 -C 6 )alkyl) 2 , —(C 3 -C 10 )cycloalkyl, (C 6 -C 10 )aryl, (C 2 -C 9 )heterocyclyl, —(C 1 -C 9 )heteroaryl, —NR 5 R 6 , —NSO 2 (C 1 -C 6 )alkyl, —NHSO 2 (C 3 -C 6 )cycloalkyl, —N((C 1 -C 6 )alkyl)(SO 2 —C 1 -C 6 )alkyl), —N((C 1 -C 6 )alkyl)(SO 2 (C 3 -C 6 )cycloalkyl), —O(C 1 -C 6 )alkyl, —O—SO 2 (C 1 -C 6 )alkyl, —(CO)(C 1 -C 6 )alkyl, —(CO)CF 3 , —(CO)(C 3 -C 10 )cycloalkyl, —(CO)(C 6 -C 10 )aryl, —(CO)(C 2 -C 9 )heterocyclyl, —(CO)(C 1 -C 9 )heteroaryl, —(CO)O(C 1 -C 6 )alkyl, —(CO)O(C 3 -C 10 )cycloalkyl, —(CO)O(C 6 -C 10 )aryl, —(CO)O(C 2 -C 9 )heterocyclyl, —(CO)O(C 1 -C 9 )heteroaryl, —(CO)(C 1 -C 6 )alkyl-O(C 1 -C 6 )alkyl, —SO 2 (C 1 -C 6 )alkyl, —SO 2 (C 3 -C 6 )cycloalkyl, SO 2 CF 3 , SO 2 NH 2 , SO 2 NH(C 1 -C 6 )alkyl, —SO 2 NH(C 3 -C 6 )cycloalkyl, —SO 2 N((C 1 -C 6 )alkyl) 2 , —SO 2 N((C 3 -C 6 )cycloalkyl) 2 , —SO 2 NR 5 R 6 , and —SO 2 N(C 1 -C 6 )alkyl-(C 6 -C 6 -C 10 )aryl; wherein said —(C 1 -C 6 )alkyl is optionally interrupted by one to three elements selected from the group consisting of —(C═O), —SO 2 , —S—, —O—, —N—, —NH— and —NR 5 ; and R 5 and R 6 of said NR 5 R 6 R 3 (b) group may be taken together with the atoms to which they are attached to form a —(C 2 -C 9 )heterocyclyl;
and wherein each R 3 (b)-(d) substituent, moiety, or element is optionally substituted by one to three radicals independently selected from the group consisting of hydrogen, halogen, hydroxy, —CF 3 , —NO 2 , —CN, —(C 1 -C 6 )alkyl, —(C 2 -C 6 )alkenyl, —(C 2 -C 6 )alkynyl, —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —(C 6 -C 10 )aryl, —(C 1 -C 9 )heteroaryl, —O(C 1 -C 6 )alkyl, —O(C 3 -C 7 )cycloalkyl, —O(C 2 -C 9 )heterocyclyl, —C═N—OH, —C═N—O(C 1 -C 6 alkyl), —NR 5 R 6 , —SR 7 , —SOR 7 , —SO 2 R 7 , —CO 2 R 5 , —CONR 5 R 6 , —SO 2 NR 5 R 6 , —NHCOR 5 , —NR 5 CONR 5 R 6 , and —NR 5 SO 2 R 7 ; with the proviso that a heteroatom of the foregoing R 3 (b)-(d) substituents, moieties, elements or radicals may not be bound to an sp 3 carbon atom bound to another heteroatom; and wherein R 5 and R 6 of said —NR 5 R 6 , —CONR 5 R 6 , —SO 2 NR 5 R 6 , and —NR 5 CONR 5 R 6 groups may be taken together with the atoms to which they are attached to form a —(C 2 -C 9 )heterocyclyl;
R 4 is a substituent selected from the group consisting of hydrogen, (C 1 -C 6 )alkyl, —(C 3 -C 7 )cycloalkyl, and —(C 2 -C 9 )heterocyclyl; wherein said (C 1 -C 6 )alkyl, —(C 3 -C 7 )cycloalkyl, and —(C 2 -C 9 )heterocyclyl R 4 substituents are optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, —(C 1 -C 6 )alkyl, —CN, —NR 5 2 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , and —CONR 5 R 8 ; with the proviso that a heteroatom of the foregoing R 4 substituents may not be bound to an sp 3 carbon atom bound to another heteroatom; and wherein R 5 and R 8 of said —CONR 5 R 8 group may be taken together with the atoms to which they are attached to form a —(C 3 -C 10 )cycloalkyl or —(C 2 -C 9 )heterocyclyl;
R 5 and R 6 are each substituents independently selected from the group consisting of hydrogen, —(C 1 -C 6 )alkyl, —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —(C 6 -C 10 )aryl, and —C 1 -C 9 )heteroaryl; wherein said —(C 1 -C 6 )alkyl, —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —(C 6 -C 10 )aryl, and —(C 1 -C 9 )heteroaryl R 5 or R 6 substituents are optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, —CF 3 , —CN, —(C 1 -C 6 )alkyl, —NH(C 1 -C 6 )alkyl, —NH(C 3 -C 7 )cycloalkyl, —NH(C 2 -C 9 )heterocyclyl, —NH(C 6 -C 10 )aryl, —NH(C 1 -C 9 )heteroaryl, —N((C 1 -C 6 )alkyl) 2 , —N((C 3 -C 7 )cycloalkyl) 2 , —N((C 2 -C 9 )heterocyclyl) 2 , —N((C 6 -C 10 )aryl) 2 , —N((C 1 -C 9 )heteroaryl) 2 , —O(C 1 -C 6 )alkyl, —O(C 3 -C 7 )cycloalkyl, —O(C 2 -C 9 )heterocyclyl, —O(C 6 -C 10 )aryl, —O(C 1 -C 9 )heteroaryl, —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 7 , —CONH 2 , —CONHR 7 , and —CONR 7 R 8 ; with the proviso that a heteroatom of the foregoing R 5 or R 6 substituents or moieties may not be bound to an sp 3 carbon atom bound to another heteroatoms; and wherein R 7 and R 8 of said —CONR 7 R 8 group may be taken together with the atoms to which they are attached to form a —(C 1 -C 9 ) heteroaryl;
R 5 and R 6 may be taken together with the atom(s) to which they are attached to form a cyclic group, —(C 3 -C 10 )cycloalkyl or —(C 2 -C 9 )heterocyclyl, wherein said cyclic group is optionally substituted by one to three moieties selected from the group consisting of hydrogen, halogen, hydroxy, —CF 3 , —NO 2 , —CN, —(C 1 -C 6 )alkyl, —(C 2 -C 6 )alkenyl, —(C 2 -C 6 )alkynyl, —C═N—OH, —C═N—O((C 1 -C 6 )alkyl), —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 , —CONR 5 R 8 , —SR 7 , —SOR 7 , —SO 2 R 7 , —SO 2 NR 5 R 6 , —NHCOR 5 , —NR 5 CONR 5 R 6 , and —NR 5 SO 2 R 7 , wherein said —(C 2 -C 6 )alkenyl and —(C 2 -C 6 )alkynyl moieties of said cyclic group may be optionally substituted by one to three R 7 groups, and said cyclic group is optionally interrupted by one to three elements selected from the group consisting of —(C═O), —SO 2 , —S—, —O—, —N—, —NH— and —NR 5 , with the proviso that any of the foregoing cyclic group moieties or elements may not be bound to an sp 3 carbon atom that is bound to another heteroatom;
R 7 is a substituent selected from the group consisting of —(C 1 -C 6 )alkyl, —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —(C 6 -C 10 )aryl, and —(C 1 -C 9 )heteroaryl; wherein said —(C 1 -C 6 )alkyl, —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —(C 6 -C 10 )aryl, and —(C 1 -C 9 )heteroaryl R 7 substituents are optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —CN, —(C 1 -C 6 )alkyl, —NR 5 2 , and —O(C 1 -C 6 )alkyl, with the proviso that a heteroatom of the foregoing R 7 substituents or moieties may not be bound to an sp 3 carbon atom bound to another heteroatom;
R 8 is a substituent selected from the group consisting of hydrogen, —(C 1 -C 6 )alkyl, —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —(C 6 -C 10 )aryl, and —(C 1 -C 9 )heteroaryl; wherein said —(C 1 -C 6 )alkyl, —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —(C 6 -C 10 )aryl, and —(C 1 -C 9 )heteroaryl R 8 radicals are optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —CN, —(C 1 -C 6 )alkyl, —NH 2 , —NHR 9 , —NR 9 2 , OR 9 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 10 , —CONH 2 , —CONHR 10 , and —CONR 10 R 11 ; with the proviso that a heteroatom of the foregoing R 8 substituents or moieties may not be bound to an sp 3 carbon atom bound to another heteroatom; and wherein R 10 and R 11 of —CONR 10 R 11 may be taken together with the atoms to which they are attached to form a —(C2-C 9 )heterocyclyl;
R 9 and R 10 are each —(C 1 -C 6 )alkyl and may be taken together with the atoms to which they are attached to form a —(C 2 -C 9 )heterocyclyl; and
R 11 is hydrogen or —(C 1 -C 6 )alkyl.
The present invention also includes isotopically-labeled compounds, which are identical to those recited in Formula 1, but for the fact that one or more atoms are replaced by an atom having an atomic mass or mass number different from the atomic mass or mass number usually found in nature. Examples of isotopes that can be incorporated into compounds of the invention include isotopes of hydrogen, carbon, nitrogen, oxygen, phosphorous, fluorine and chlorine, such as 2 H, 3 H, 13 C, 14 C, 15 N, 18 O, 17 O, 31 P, 32 P, 35 S, 18 F, and 36 Cl, respectively. Compounds of the present invention, prodrugs thereof, and pharmaceutically acceptable salts of said compounds or of said prodrugs which contain the aforementioned isotopes and/or other isotopes of other atoms are within the scope of this invention. Certain isotopically-labelled compounds of the present invention, for example those into which radioactive isotopes such as 3 H and 14 C are incorporated, are useful in drug and/or substrate tissue distribution assays. Tritiated, i.e., 3 H, and carbon-14, i.e., 14 C, isotopes are particularly preferred for their ease of preparation and detectability. Further, substitution with heavier isotopes such as deuterium, i.e., 2 H, can afford certain therapeutic advantages resulting from greater metabolic stability, for example increased in vivo half-life or reduced dosage requirements and, hence, may be preferred in some circumstances. Isotopically-labelled compounds of Formula 1 of this invention and prodrugs thereof can generally be prepared by carrying out the procedures disclosed in the Schemes and/or in the Examples and Preparations below, by substituting a readily available isotopically-labelled reagent for a non-isotopically-labelled reagent.
The present invention also relates to the pharmaceutically acceptable acid addition salts of compounds of the formula 1. The acids which are used to prepare the pharmaceutically acceptable acid addition salts of the aforementioned base compounds of this invention are those which form non-toxic acid addition salts, i.e., salts containing pharmacologically acceptable anions, such as the chloride, bromide, iodide, nitrate, sulfate, bisulfate, phosphate, acid phosphate, acetate, lactate, citrate, acid citrate, tartrate, bitartrate, succinate, maleate, fumarate, gluconate, saccharate, benzoate, methanesulfonate, ethanesulfonate, benzenesulfonate, p-toluenesulfonate and pamoate [i.e., 1,1′-methylene-bis-(2-hydroxy-3-naphthoate)]salts.
The invention also relates to base addition salts of formula 1. The chemical bases that may be used as reagents to prepare pharmaceutically acceptable base salts of those compounds of formula 1 that are acidic in nature are those that form non-toxic base salts with such compounds. Such non-toxic base salts include, but are not limited to those derived from such pharmacologically acceptable cations such as alkali metal cations (e.g., potassium and sodium) and alkaline earth metal cations (e.g., calcium and magnesium), ammonium or water-soluble amine addition salts such as N-methylglucamine-(meglumine), and the lower alkanolammonium and other base salts of pharmaceutically acceptable organic amines.
The phrase “pharmaceutically acceptable salt(s)”, as used herein, unless otherwise indicated, includes salts of acidic or basic groups which may be present in the compounds of the present invention. The compounds of the present invention that are basic in nature are capable of forming a wide variety of salts with various inorganic and organic acids. The acids that may be used to prepare pharmaceutically acceptable acid addition salts of such basic compounds of are those that form non-toxic acid addition salts, i.e., salts containing pharmacologically acceptable anions, such as the hydrochloride, hydrobromide, hydroiodide, nitrate, sulfate, bisulfate, phosphate, acid phosphate, isonicotinate, acetate, lactate, salicylate, citrate, acid citrate, tartrate, pantothenate, bitartrate, ascorbate, succinate, maleate, gentisinate, fumarate, gluconate, glucuronate, saccharate, formate, benzoate, glutamate, methanesulfonate, ethanesulfonate, benzenesulfonate, p-toluenesulfonate and pamoate [i.e., 1,1′-methylene-bis-(2-hydroxy-3-naphthoate)] salts. The compounds of the present invention that include a basic moiety, such as an amino group, may form pharmaceutically acceptable salts with various amino acids, in addition to the acids mentioned above.
This invention also encompasses pharmaceutical compositions containing prodrugs of compounds of the formula 1. Compounds of formula 1 having free amino, amido, hydroxy or carboxylic groups can be converted into prodrugs. Prodrugs include compounds wherein an amino acid residue, or a polypeptide chain of two or more (e.g., two, three or four) amino acid residues which are covalently joined through peptide bonds to free amino, hydroxy or carboxylic acid groups of compounds of formula 1. The amino acid residues include the 20 naturally occurring amino acids commonly designated by three letter symbols and also include, 4-hydroxyproline, hydroxylysine, demosine, isodemosine, 3-methylhistidine, norvalin, beta-alanine, gamma-aminobutyric acid, citrulline, homocysteine, homoserine, ornithine and methionine sulfone. Prodrugs also include compounds wherein carbonates, carbamates, amides and alkyl esters that are covalently bonded to the above substituents of formula 1 through the carbonyl carbon prodrug sidechain.
This invention also encompasses compounds of formula 1 containing protective groups. One skilled in the art will also appreciate that compounds of the invention can also be prepared with certain protecting groups that are useful for purification or storage and can be removed before administration to a patient. The protection and deprotection of functional groups is described in “Protective Groups in Organic Chemistry”, edited by J. W. F. McOmie, Plenum Press (1973) and “Protective Groups in Organic Synthesis”, 3rd edition, T. W. Greene and P. G. M. Wuts, Wiley-Interscience (1999).
The compounds of this invention include all stereoisomers (e.g., cis and trans isomers) and all optical isomers of compounds of the formula 1 (e.g., R and S enantiomers), as well as racemic, diastereomeric and other mixtures of such isomers.
The compounds, salts and prodrugs of the present invention can exist in several tautomeric forms, including the enol and imine form, and the keto and enamine form and geometric isomers and mixtures thereof. All such tautomeric forms are included within the scope of the present invention. Tautomers exist as mixtures of a tautomeric set in solution. In solid form, usually one tautomer predominates. Even though one tautomer may be described, the present invention includes all tautomers of the present compounds.
The present invention also includes atropisomers of the present invention. Atropisomers refer to compounds of formula 1 that can be separated into rotationally restricted isomers.
The compounds of this invention may contain olefin-like double bonds. When such bonds are present, the compounds of the invention exist as cis and trans configurations and as mixtures thereof.
A “suitable substituent” is intended to mean a chemically and pharmaceutically acceptable functional group i.e., a moiety that does not negate the biological activity of the inventive compounds. Such suitable substituents may be routinely selected by those skilled in the art. Illustrative examples of suitable substituents include, but are not limited to halo groups, perfluoroalkyl groups, perfluoroalkoxy groups, alkyl groups, alkenyl groups, alkynyl groups, hydroxy groups, oxo groups, mercapto groups, alkylthio groups, alkoxy groups, aryl or heteroaryl groups, aryloxy or heteroaryloxy groups, aralkyl or heteroaralkyl groups, aralkoxy or heteroaralkoxy groups, HO—(C═O)— groups, amino groups, alkyl- and dialkylamino groups, carbamoyl groups, alkylcarbonyl groups, alkoxycarbonyl groups, alkylaminocarbonyl groups dialkylamino carbonyl groups, arylcarbonyl groups, aryloxycarbonyl groups, alkylsulfonyl groups, arylsulfonyl groups and the like. Those skilled in the art will appreciate that many substituents can be substituted by additional substituents. Further examples of suitable substituents include those recited in the definition of compounds of Formula 1, including R 1 through R 11 , as defined hereinabove.
The term “interrupted by” refers to compounds in which a ring carbon atom is replaced by an element selected from the group consisting of —(C═O), —SO 2 , —S—, —O—, —N—, —NH—, and —NR 5 . For example, if R 7 is —(C 6 -C 10 )aryl, such as
the ring may be interrupted or replaced by a nitrogen heteroatom to form the following ring:
such that a ring carbon is replaced by the heteroatom nitrogen. Compounds of the invention can accommodate up to three such replacements or interruptions.
As used herein, the term “alkyl,” as well as the alkyl moieties of other groups referred to herein (e.g., alkoxy), may be linear or branched (such as methyl, ethyl, n-propyl, isopropyl, n-butyl, iso-butyl, secondary-butyl, tertiary-butyl); optionally substituted by 1 to 3 suitable substituents as defined above such as fluoro, chloro, trifluoromethyl, (C 1 -C 6 )alkoxy, (C 6 -C 10 )aryloxy, trifluoromethoxy, difluoromethoxy or (C 1 -C 6 )alkyl. The phrase “each of said alkyl” as used herein refers to any of the preceding alkyl moieties within a group such alkoxy, alkenyl or alkylamino. Preferred alkyls include (C 1 -C 6 )alkyl, more preferred are (C 1 -C 4 )alkyl, and most preferred are methyl and ethyl.
As used herein, the term “cycloalkyl” refers to a mono, bicyclic or tricyclic carbocyclic ring (e.g., cyclopropyl, cyclobutyl, cyclopentyl, cyclohexyl, cycloheptyl, cyclooctyl, cyclononyl, cyclopentenyl, cyclohexenyl, bicyclo[2.2.1]heptanyl, bicyclo[3.2.1]octanyl and bicyclo[5.2.0]nonanyl, etc.); optionally containing 1 or 2 double bonds and optionally substituted by 1 to 3 suitable substituents as defined above such as fluoro, chloro, trifluoromethyl, (C 1 -C 6 )alkoxy, (C 6 -C 10 )aryloxy, trifluoromethoxy, difluoromethoxy or (C 1 -C 6 )alkyl.
As used herein, the term “halogen” includes fluoro, chloro, bromo or iodo or fluoride, chloride, bromide or iodide.
As used herein, the term “alkenyl” means straight or branched chain unsaturated radicals of 2 to 6 carbon atoms, including, but not limited to ethenyl, 1-propenyl, 2-propenyl (allyl), iso-propenyl, 2-methyl-1-propenyl, 1-butenyl, 2-butenyl, and the like; optionally substituted by 1 to 3 suitable substituents as defined above such as fluoro, chloro, trifluoromethyl, (C 1 -C 6 )alkoxy, (C 6 -C 10 )aryloxy, trifluoromethoxy, difluoromethoxy or (C 1 -C 6 )alkyl.
As used herein, the term “alkynyl” is used herein to mean straight or branched hydrocarbon chain radicals having one triple bond including, but not limited to, ethynyl, propynyl, butynyl, and the like; optionally substituted by 1 to 3 suitable substituents as defined above such as fluoro, chloro, trifluoromethyl, (C 1 -C 6 )alkoxy, (C 6 -C 10 )aryloxy, trifluoromethoxy, difluoromethoxy or (C 1 -C 6 )alkyl.
As used herein, the term “carbonyl” or “(C═O)” (as used in phrases such as alkylcarbonyl, alkyl-(C═O)— or alkoxycarbonyl) refers to the joinder of the >C═O moiety to a second moiety such as an alkyl or amino group (i.e. an amido group). Alkoxycarbonylamino (i.e. alkoxy(C═O)—NH—) refers to an alkyl carbamate group. The carbonyl group is also equivalently defined herein as (C═O). Alkylcarbonylamino refers to groups such as acetamide.
As used herein, the term “aryl” means aromatic radicals such as phenyl, naphthyl, tetrahydronaphthyl, indanyl and the like; optionally substituted by 1 to 3 suitable substituents as defined above.
As used herein, the term “heteroaryl” refers to an aromatic heterocyclic group usually with one heteroatom selected from O, S and N in the ring. In addition to said heteroatom, the aromatic group may optionally have up to four N atoms in the ring. For example, heteroaryl group includes pyridyl, pyrazinyl, pyrimidinyl, pyridazinyl, thienyl, furyl, imidazolyl, pyrrolyl, oxazolyl (e.g., 1,3-oxazolyl, 1,2-oxazolyl), thiazolyl (e.g., 1,2-thiazolyl, 1,3-thiazolyl), pyrazolyl, tetrazolyl, triazolyl (e.g., 1,2,3-triazolyl, 1,2,4-triazolyl), oxadiazolyl (e.g., 1,2,3-oxadiazolyl), thiadiazolyl (e.g., 1,3,4-thiadiazolyl), quinolyl, isoquinolyl, benzothienyl, benzofuryl, indolyl, and the like; optionally substituted by 1 to 3 suitable substituents as defined above such as fluoro, chloro, trifluoromethyl, (C 1 -C 6 )alkoxy, (C 6 -C 10 )aryloxy, trifluoromethoxy, difluoromethoxy or (C 1 -C 6 )alkyl.
The term “heterocyclic” as used herein refers to a cyclic group containing 1-9 carbon atoms and 1 to 4 hetero atoms selected from N, O, S(O) n or NR. Examples of such rings include azetidinyl, tetrahydrofuranyl, imidazolidinyl, pyrrolidinyl, piperidinyl, piperazinyl, oxazolidinyl, thiazolidinyl, pyrazolidinyl, thiomorpholinyl, tetrahydrothiazinyl, tetrahydro-thiadiazinyl, morpholinyl, oxetanyl, tetrahydrodiazinyl, oxazinyl, oxathiazinyl, indolinyl, isoindolinyl, quinuclidinyl, chromanyl, isochromanyl, benzoxazinyl, and the like. Examples of said monocyclic saturated or partially saturated ring systems are tetrahydrofuran-2-yl, tetrahydrofuran-3-yl, imidazolidin-1-yl, imidazolidin-2-yl, imidazolidin-4-yl, pyrrolidin-1-yl, pyrrolidin-2-yl, pyrrolidin-3-yl, piperidin-1-yl, piperidin-2-yl, piperidin-3-yl, piperazin-1-yl, piperazin-2-yl, piperazin-3-yl, 1,3-oxazolidin-3-yl, isothiazolidine, 1,3-thiazolidin-3-yl, 1,2-pyrazolidin-2-yl, 1,3-pyrazolidin-1-yl, thiomorpholin-yl, 1,2-tetrahydrothiazin-2-yl, 1,3-tetrahydrothiazin-3-yl, tetrahydrothiadiazin-yl, morpholin-yl, 1,2-tetrahydrodiazin-2-yl, 1,3-tetrahydrodiazin-1-yl, 1,4-oxazin-2-yl, 1,2,5-oxathiazin-4-yl and the like; optionally containing 1 or 2 double bonds and optionally substituted by 1 to 3 suitable substituents as defined above such as fluoro, chloro, trifluoromethyl, (C 1 -C 6 )alkoxy, (C 6 -C 10 )aryloxy, trifluoromethoxy, difluoromethoxy or (C 1 -C 6 )alkyl.
Nitrogen heteroatoms as used herein refers to N═, >N and —NH; wherein —N═ refers to a nitrogen double bond; >N refers to a nitrogen containing two bond connections and —N refers to a nitrogen containing one bond.
“Embodiment” as used herein refers to specific groupings of compounds or uses into discrete subgenera. Such subgenera may be cognizable according to one particular substituent such as a specific R 1 or R 3 group. Other subgenera are cognizable according to combinations of various substituents, such as all compounds wherein R 2 is hydrogen and R 1 is (C 1 -C 6 )alkyl.
Thus, the present invention provides a compound of formula 1, wherein R 1 is selected from hydrogen, hydroxy, and —(C 1 -C 6 )alkyl, optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —CN, —(C 1 -C 6 )alkyl, —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 and —CONR 5 R 8 .
The present invention further provides a compound of formula 1, wherein R 1 is —(C 1 -C 6 )alkyl, optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —CN, —(C 1 -C 6 )alkyl, —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 and —CONR 5 R 8 .
The present invention also provides a compound of formula 1 wherein R 1 is selected from the group consisting of —(C 3 -C 7 )cycloalkyl and —(C 2 -C 9 )heterocyclyl, optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —CN, —(C 1 -C 6 )alkyl, —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 and —CONR 5 R 8 .
The invention also contemplates compounds of formula 1 wherein R 1 is selected from —O(C 1 -C 6 )alkyl, —O(C 3 -C 7 )cycloalkyl, and —O(C 2 -C 9 )heterocyclyl, optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —CN, —(C 1 -C 6 )alkyl, —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 and —CONR 5 R 8 . In a preferred embodiment, R 1 is —O(C 1 -C 6 )alkyl, optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —CN, —(C 1 -C 6 )alkyl, —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 and —CONR 5 R 8 .
One embodiment of the invention is a compound of formula 1 wherein R 1 is —NR 5 R 6 , optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —CN, —(C 1 -C 6 )alkyl, —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 and —CONR 5 R 8 .
A further embodiment of the invention is a compound of formula 1 wherein R 1 is selected from —SR 7 , —SOR 7 , —SO 2 R 7 , and —SO 2 NR 5 R 6 , optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —CN, —(C 1 -C 6 )alkyl, —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 and —CONR 5 R 8 . In a preferred embodiment, R 1 is —SO 2 NR 5 R 6 , optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —CN, —(C 1 -C 6 )alkyl, —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 and —CONR 5 R 8 .
The present invention also provides compounds of formula 1 wherein R 1 is —CO 2 R 5 , —CONR 5 R 6 , —NHCOR 5 , —NR 5 CONR 5 R 6 , or —NR 5 SO 2 R 7 , optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —CN, —(C 1 -C 6 )alkyl, —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 and —CONR 5 R 8 . In a preferred embodiment, R 1 is —NR 5 SO 2 R 7 , optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —CN, —(C 1 -C 6 )alkyl, —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 and —CONR 5 R 8 .
Also provided is a compound of formula 1 wherein R 2 is hydrogen or —(C 1 -C 6 )alkyl, optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —NO 2 , —CN, —(C 1 -C 6 )alkyl, —(C 2 -C 6 )alkenyl, —(C 2 -C 6 )alkynyl, —C═N—OH, —C═N—O((C 1 -C 6 )alkyl), —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 , —CONR 5 R 8 , —SR 7 , —SOR 7 , —SO 2 R 7 , —SO 2 NR 5 R 6 , —NHCOR 5 , —NR 5 CONR 5 R 6 , and —NR 5 SO 2 R 7 , wherein said —(C 2 -C 6 )alkenyl and —(C 2 -C 6 )alkenyl R 2 moieties may be optionally substituted by one to three R 5 groups.
Further provided is a compound of formula 1 wherein R 2 is —(C 3 -C 7 )cycloalkyl, or —(C 2 -C 9 )heterocyclyl, optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —NO 2 , —CN, —(C 1 -C 6 )alkyl, —(C 2 -C 6 )alkenyl, —(C 2 -C 6 )alkynyl, —C═N—OH, —C═N—O((C 1 -C 6 )alkyl), —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 , —CONR 5 R 8 , —SR 7 , —SOR 7 , —S 2 R 7 , —SO 2 NR 5 R 6 , —NHCOR 5 , —NR 5 CONR 5 R 6 , and —NR 5 SO 2 R 7 , wherein said —(C 2 -C 6 )alkenyl and —(C 2 -C 6 )alkynyl R 2 moieties may be optionally substituted by one to three R 5 groups.
Another embodiment of the present invention is a compound of formula 1 wherein R 2 is —CO 2 R 5 and —CONR 5 R 6 optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —NO 2 , —CN, —(C 1 -C 6 )alkyl, —(C 2 -C 6 )alkenyl, —(C 2 -C 6 )alkynyl, —C═N—OH, —C═N—O((C 1 -C 6 )alkyl), —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 , —CONR 5 R 8 , —SR 7 , —SOR 7 , —SO 2 R 7 , —SO 2 NR 5 R 6 , —NHCOR 5 , —NR 5 CONR 5 R 6 , and —NR 5 SO 2 R 7 , wherein said —(C 2 -C 6 )alkenyl and —(C 2 -C 6 )alkynyl R 2 moieties may be optionally substituted by one to three R 5 groups.
Also provided is a compound of formula 1 wherein R 1 is selected from hydrogen, hydroxy, and —(C 1 -C 6 )alkyl, optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —CN, —(C 1 -C 6 )alkyl, —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 and —CONR 5 R 8 ; and R 2 is hydrogen or —(C 1 -C 6 )alkyl, optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —NO 2 , —CN, —(C 1 -C 6 )alkyl, —(C 2 -C 6 )alkenyl, —(C 2 -C 6 )alkynyl, —C═N—OH, —C═N—O((C 1 -C 6 )alkyl), —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 , —CONR 5 R 8 , —SR 7 , —SOR 7 , —SO 2 R 7 , —SO 2 NR 5 R 6 , —NHCOR 5 , —NR 5 CONR 5 R 6 , and —NR 5 SO 2 R 7 , wherein said —(C 2 -C 6 )alkenyl and —(C 2 -C 6 )alkynyl R 2 moieties may be optionally substituted by one to three R 5 groups.
The invention further provides a compound of formula 1 wherein R 1 is selected from hydrogen, hydroxy, and —(C 1 -C 6 )alkyl, optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —CN, —(C 1 -C 6 )alkyl, —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 and —CONR 5 R 8 ; and R 2 is hydrogen.
The present invention further provides a compound of formula 1, wherein R 1 is —(C 1 -C 6 )alkyl, optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —CN, —(C 1 -C 6 )alkyl, —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 and —CONR 5 R 8 ; and R 2 is hydrogen.
The present invention also provides a compound of formula 1 wherein R 1 is selected from the group consisting of —(C 3 -C 7 )cycloalkyl and —(C 2 -C 9 )heterocyclyl, optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —CN, —(C 1 -C 6 )alkyl, —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 and —CONR 5 R 8 ; and R 2 is hydrogen.
The invention also contemplates compounds of formula 1 wherein R 1 is selected from —O(C 1 -C 6 )alkyl, —O(C 3 -C 7 )cycloalkyl, and —O(C 2 -C 9 )heterocyclyl, optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —CN, —(C 1 -C 6 )alkyl, —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CONR 5 R 6 and —CONR 5 R 8 ; and R 2 is hydrogen.
One embodiment of the invention is a compound of formula 1 wherein R 1 is —NR 5 R 6 , optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —CN, —(C 1 -C 6 )alkyl, —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 and —CONR 5 R 8 ; and R 2 is hydrogen.
A further embodiment of the invention is a compound of formula 1 wherein R 1 is selected from —SR 7 , —SOR 7 , —SO 2 R 7 , and —SO 2 NR 5 R 6 , optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —CN, —(C 1 -C 6 )alkyl, —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 and —CONR 5 R 8 ; and R 2 is hydrogen.
The present invention also provides compounds of formula 1 wherein R 1 is —CO 2 R 5 , —CONR 5 R 6 , —NHCOR 5 , —NR 5 CONR 5 R 6 , or —NR 5 SO 2 R 7 , optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —CN, —(C 1 -C 6 )alkyl, —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 and —CONR 5 R 8 ; and R 2 is hydrogen.
Also provided is a compound of formula 1 wherein R 2 is hydrogen or —(C 1 -C 6 )alkyl, optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —NO 2 , —CN, —(C 1 -C 6 )alkyl, —(C 2 -C 6 )alkenyl, —(C 2 -C 6 )alkynyl, —C═N—OH, —C═N—O((C 1 -C 6 )alkyl), —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 , —CONR 5 R 8 , —SR 7 , —SOR 7 , —SO 2 R 7 , —SO 2 NR 5 R 6 , —NHCOR 5 , —NR 5 CONR 5 R 6 , and —NR 5 SO 2 R 7 , wherein said —(C 2 -C 6 )alkenyl and —(C 2 -C 6 )alkynyl R 2 moieties may be optionally substituted by one to three R 5 groups; and R 1 is hydrogen.
Further provided is a compound of formula 1 wherein R 2 is —(C 3 -C 7 )cycloalkyl, or —(C 2 -C 9 )heterocyclyl, optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —NO 2 , —CN, —(C 1 -C 6 )alkyl, —(C 2 -C 6 )alkenyl, —(C 2 -C 6 )alkynyl, —C═N—OH, —C═N—O((C 1 -C 6 )alkyl), —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 , —CONR 5 R 8 , —SR 7 , —SOR 7 , —SO 2 R 7 , —SO 2 NR 5 R 6 , —NHCOR 5 , —NR 5 CONR 5 R 6 , and —NR 5 SO 2 R 7 , wherein said —(C 2 -C 6 )alkenyl and —(C 2 -C 6 )alkynyl R 2 moieties may be optionally substituted by one to three R 5 groups; and R 1 is hydrogen.
Another embodiment of the present invention is a compound of formula 1 wherein R 2 is —CO 2 R 5 and —CONR 5 R 6 optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —NO 2 , —CN, —(C 1 -C 6 )alkyl, —(C 2 -C 6 )alkenyl, —(C 2 -C 6 )alkynyl, —C═N—OH, —C═N—O((C 1 -C 6 )alkyl), —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 , —CONR 5 R 8 , —SR 7 , —SOR 7 , —SO 2 R 7 , —SO 2 NR 5 R 6 , —NHCOR 5 , —NR 5 CONR 5 R 6 , and —NR 5 SO 2 R 7 , wherein said —(C 2 -C 6 )alkenyl and —(C 2 -C 6 )alkynyl R 2 moieties may be optionally substituted by one to three R 5 groups; and R 1 is hydrogen.
The invention further provides a compound of formula 1 wherein R 1 is selected from hydrogen, hydroxy, and —(C 1 -C 6 )alkyl, optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —CN, —(C 1 -C 6 )alkyl, —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 and —CONR 5 R 8 ; and R 2 is —(C 1 -C 6 )alkyl.
The present invention further provides a compound of formula 1, wherein R 1 is —(C 1 -C 6 )alkyl, optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —CN, —(C 1 -C 6 )alkyl, —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 and —CONR 5 R 8 ; and R 2 is —(C 1 -C 6 )alkyl.
The present invention also provides a compound of formula 1 wherein R 1 is selected from the group consisting of —(C 3 -C 7 )cycloalkyl and —(C 2 -C 9 )heterocyclyl, optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —CN, —(C 1 -C 6 )alkyl, —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 and —CONR 5 R 8 ; and R 2 is —(C 1 -C 6 )alkyl.
The invention also contemplates compounds of formula 1 wherein R 1 is selected from —O(C 1 -C 6 )alkyl, —O(C 3 -C 7 )cycloalkyl, and —O(C 2 -C 9 )heterocyclyl, optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —CN, —(C 1 -C 6 )alkyl, —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 and —CONR 5 R 8 ; and R 2 is —(C 1 -C 6 )alkyl.
One embodiment of the invention is a compound of formula 1 wherein R 1 is —NR 5 R 6 , optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —CN, —(C 1 -C 6 )alkyl, —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 and —CONR 5 R 8 ; and R 2 is —(C 1 -C 6 )alkyl.
A further embodiment of the invention is a compound of formula 1 wherein R 1 is selected from —SR 7 , —SOR 7 , —SO 2 R 7 , and —SO 2 NR 5 R 6 , optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —CN, —(C 1 -C 6 )alkyl, —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 and —CONR 5 R 8 ; and R 2 is —(C 1 -C 6 )alkyl.
The present invention also provides compounds of formula 1 wherein R 1 is —CO 2 R 5 , —CONR 5 R 6 , —NHCOR 5 , —NR 5 CONR 5 R 6 , or —NR 5 SO 2 R 7 , optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —CN, —(C 1 -C 6 )alkyl, —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 and —CONR 5 R 8 ; and R 2 is —(C 1 -C 6 )alkyl.
Also provided is a compound of formula 1 wherein R 2 is hydrogen or —(C 1 -C 6 )alkyl, optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —NO 2 , —CN, —(C 1 -C 6 )alkyl, —(C 2 -C 6 )alkenyl, —(C 2 -C 6 )alkynyl, —C═N—OH, —C═N—O((C 1 -C 6 )alkyl), —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 , —CONR 5 R 8 , —SR 7 , —SOR 7 , —SO 2 R 7 , —SO 2 NR 5 R 6 , —NHCOR 5 , —NR 5 CONR 5 R 6 , and —NR 5 SO 2 R 7 , wherein said —(C 2 -C 6 )alkenyl and —(C 2 -C 6 )alkynyl R 2 moieties may be optionally substituted by one to three R 5 groups; and R 1 is —(C 1 -C 6 )alkyl.
Further provided is a compound of formula 1 wherein R 2 is —(C 3 -C 7 )cycloalkyl, or —(C 2 -C 9 )heterocyclyl, optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —NO 2 , —CN, —(C 1 -C 6 )alkyl, —(C 2 -C 6 )alkenyl, —(C 2 -C 6 )alkynyl, —C═N—OH, —C═N—O((C 1 -C 6 )alkyl), —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 , —CONR 5 R 8 , —SR 7 , —SOR 7 , —SO 2 R 7 , —SO 2 NR 5 R 6 , —NHCOR 5 , —NR 5 CONR 5 R 6 , and —NR 5 SO 2 R 7 , wherein said —(C 2 -C 6 )alkenyl and —(C 2 -C 6 )alkynyl R 2 moieties may be optionally substituted by one to three R 5 groups; and R 1 is —(C 1 -C 6 )alkyl.
Another embodiment of the present invention is a compound of formula 1 wherein R 2 is —CO 2 R 5 and —CONR 5 R 6 optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —NO 2 , —CN, —(C 1 -C 6 )alkyl, —(C 2 -C 6 )alkenyl, —(C 2 -C 6 )alkynyl, —C═N—OH, —C═N—O((C 1 -C 6 )alkyl), —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 , —CONR 5 R 8 , —SR 7 , —SOR 7 , —SO 2 R 7 , —SO 2 NR 5 R 6 , —NHCOR 5 , —NR 5 CONR 5 R 6 , and —NR 5 SO 2 R 7 , wherein said —(C 2 -C 6 )alkenyl and —(C 2 -C 6 )alkynyl R 2 moieties may be optionally substituted by one to three R 5 groups; and R 1 is —(C 1 -C 6 )alkyl.
Also provided is a compound of formula 1 wherein R 1 is selected from hydrogen, hydroxy, and —(C 1 -C 6 )alkyl, optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —CN, —(C 1 -C 6 )alkyl, —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 and —CONR 5 R 8 ; R 2 is hydrogen or —(C 1 -C 6 )alkyl, optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —NO 2 , —CN, —(C 1 -C 6 )alkyl, —(C 2 -C 6 )alkenyl, —(C 2 -C 6 )alkynyl, —C═N—OH, —C═N—O((C 1 -C 6 )alkyl), —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 , —CONR 5 R 8 , —SR 7 , —SOR 7 , —SO 2 R 7 , —SO 2 NR 5 R 6 , —NHCOR 5 , —NR 5 CONR 5 R 6 , and —NR 5 SO 2 R 7 , wherein said —(C 2 -C 6 )alkenyl and —(C 2 -C 6 )alkynyl R 2 moieties may be optionally substituted by one to three R 5 groups; and n is 1.
The invention further provides a compound of formula 1 wherein R 1 is selected from hydrogen, hydroxy, and —(C 1 -C 6 )alkyl, optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —CN, —(C 1 -C 6 )alkyl, —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 and —CONR 5 R 8 ; R 2 is —(C 1 -C 6 )alkyl; and n is 1.
The present invention further provides a compound of formula 1, wherein R 1 is —(C 1 -C 6 )alkyl, optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —CN, —(C 1 -C 6 )alkyl, —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 and —CONR 5 R 8 ; R 2 is —C 1 -C 6 )alkyl; and n is 1.
The present invention also provides a compound of formula 1 wherein R 1 is selected from the group consisting of —(C 3 -C 7 )cycloalkyl and —(C 2 -C 9 )heterocyclyl, optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —CN, —(C 1 -C 6 )alkyl, —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 and —CONR 5 R 8 ; R 2 is —(C 1 -C 6 )alkyl; and n is 1.
The invention also contemplates compounds of formula 1 wherein R 1 is selected from —O(C 1 -C 6 )alkyl, —O(C 3 -C 7 )cycloalkyl, and —O(C 2 -C 9 )heterocyclyl, optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —CN, —(C 1 -C 6 )alkyl, —NR 5 R 5 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 and —CONR 5 R 8 ; R 2 is —(C 1 -C 6 )alkyl; and n is 1.
One embodiment of the invention is a compound of formula 1 wherein R 1 is —NR 5 R 6 , optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —CN, —(C 1 -C 6 )alkyl, —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 and —CONR 5 R 8 ; R 2 is —(C 1 -C 6 )alkyl; and n is 1.
A further embodiment of the invention is a compound of formula 1 wherein R 1 is selected from —SR 7 , —SOR 7 , —SO 2 R 7 , and —SO 2 NR 5 R 6 , optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —CN, —(C 1 -C 6 )alkyl, —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 and —CONR 5 R 8 ; R 2 is —(C 1 -C 6 )alkyl; and n is 1.
The present invention also provides compounds of formula 1 wherein R 1 is —CO 2 R 5 , —CONR 5 R 6 , —NHCOR 5 , —NR 5 CONR 5 R 6 , or —NR 5 SO 2 R 7 , optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —CN, —(C 1 -C 6 )alkyl, —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 and —CONR 5 R 8 ; R 2 is —(C 1 -C 6 )alkyl; and n is 1.
Also provided is a compound of formula 1 wherein R 2 is hydrogen or —(C 1 -C 6 )alkyl, optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —NO 2 , —CN, —(C 1 -C 6 )alkyl, —(C 2 -C 6 )alkenyl, —(C 2 -C 6 )alkynyl, —C═N—OH, —C═N—O((C 1 -C 6 )alkyl), —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 , —CONR 5 R 8 , —SR 7 , —SOR 7 , —SO 2 R 7 , —SO 2 NR 5 R 6 , —NHCOR 5 , —NR 5 CONR 5 R 6 , and —NR 5 SO 2 R 7 , wherein said —(C 2 -C 6 )alkenyl and —(C 2 -C 6 )alkynyl R 2 moieties may be optionally substituted by one to three R 5 groups; R 1 is —(C 1 -C 6 )alkyl; and n is 1.
Further provided is a compound of formula 1 wherein R 2 is —(C 3 -C 7 )cycloalkyl, or —(C 2 -C 9 )heterocyclyl, optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —NO 2 , —CN, —(C 1 -C 6 )alkyl, —(C 2 -C 6 )alkenyl, —(C 2 -C 6 )alkynyl, —C═N—OH, —C═N—O((C 1 -C 6 )alkyl), —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 , —CONR 5 R 8 , —SR 7 , —SOR 7 , —SO 2 R 7 , —SO 2 NR 5 R 6 , —NHCOR 5 , —NR 5 CONR 5 R 6 , and —NR 5 SO 2 R 7 , wherein said —(C 2 -C 6 )alkenyl and —(C 2 -C 6 )alkynyl R 2 moieties may be optionally substituted by one to three R 5 groups; R 1 is —(C 1 -C 6 )alkyl; and n is 1.
Another embodiment of the present invention is a compound of formula 1 wherein R 2 is —CO 2 R 5 and —CONR 5 R 6 optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —NO 2 , —CN, —(C 1 -C 6 )alkyl, —(C 2 -C 6 )alkenyl, —(C 2 -C 6 )alkynyl, —C═N—OH, —C═N—O((C 1 -C 6 )alkyl), —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 , —CONR 5 R 8 , —SR 7 , —SOR 7 , —SO 2 R 7 , —SO 2 NR 5 R 6 , —NHCOR 5 , —NR 5 CONR 5 R 6 , and —NR 5 SO 2 R 7 , wherein said —(C 2 -C 6 )alkenyl and —(C 2 -C 6 )alkynyl R 2 moieties may be optionally substituted by one to three R 5 groups; R 1 is —(C 1 -C 6 )alkyl; and n is 1.
The invention further provides a compound of formula 1 wherein R 1 is selected from hydrogen, hydroxy, and —(C 1 -C 6 )alkyl, optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —CN, —(C 1 -C 6 )alkyl, —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 and —CONR 5 R 8 ; R 2 is —(C 1 -C 6 )alkyl; and n is 1.
The present invention further provides a compound of formula 1, wherein R 1 is —(C 1 -C 6 )alkyl, optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —CN, —(C 1 -C 6 )alkyl, —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 and —CONR 5 R 8 ; R 2 is —(C 1 -C 6 )alkyl; and n is 1.
The present invention also provides a compound of formula 1 wherein R 1 is selected from the group consisting of —(C 3 -C 7 )cycloalkyl and —(C 2 -C 9 )heterocyclyl, optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —CN, —(C 1 -C 6 )alkyl, —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 and —CONR 5 R 8 ; R 2 is —(C 1 -C 6 )alkyl; and n is 1.
The invention also contemplates compounds of formula 1 wherein R 1 is selected from —O(C 1 -C 6 )alkyl, —O(C 3 -C 7 )cycloalkyl, and —O(C 2 -C 9 )heterocyclyl, optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —CN, —(C 1 -C 6 )alkyl, —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 and —CONR 5 R 8 ; R 2 is —(C 1 -C 6 )alkyl; and n is 1.
One embodiment of the invention is a compound of formula 1 wherein R 1 is —NR 5 R 6 , optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —CN, —(C 1 -C 6 )alkyl, —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 and —CONR 5 R 8 ; R 2 is n is 1.
A further embodiment of the invention is a compound of formula 1 wherein R 1 is selected from —SR 7 , —SOR 7 , —SO 2 R 7 , and —SO 2 NR 5 R 6 , optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —CN, —(C 1 -C 6 )alkyl, —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 and —CONR 5 R 8 ; R 2 is —(C 1 -C 6 )alkyl; and n is 1.
The present invention also provides compounds of formula 1 wherein R 1 is —CO 2 R 5 , —CONR 5 R 6 , —NHCOR 5 , —NR 5 CONR 5 R 6 , or —NR 5 SO 2 R 7 , optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —CN, —(C 1 -C 6 )alkyl, —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 and —CONR 5 R 8 ; R 2 is —(C 1 -C 6 )alkyl; and n is 1.
Also provided is a compound of formula 1 wherein R 2 is hydrogen or —(C 1 -C 6 )alkyl, optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —NO 2 , —CN, —(C 1 -C 6 )alkyl, —(C 2 -C 6 )alkenyl, —(C 2 -C 6 )alkynyl, —C═N—OH, —C═N—O((C 1 -C 6 )alkyl), —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 , —CONR 5 R 8 , —SR 7 , —SOR 7 , —SO 2 R 7 , —SO 2 NR 5 R 6 , —NHCOR 5 , —NR 5 CONR 5 R 6 , and —NR 5 SO 2 R 7 , wherein said —(C 2 -C 6 )alkenyl and —(C 2 -C 6 )alkynyl R 2 moieties may be optionally substituted by one to three R 5 groups; R 1 is —(C 1 -C 6 )alkyl; and n is 1.
Further provided is a compound of formula 1 wherein R 2 is —(C 3 -C 7 )cycloalkyl, or —(C 2 -C 9 )heterocyclyl, optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —NO 2 , —CN, —(C 1 -C 6 )alkyl, —(C 2 -C 6 )alkenyl, —(C 2 -C 6 )alkynyl, —C═N—OH, —C═N—O((C 1 -C 6 )alkyl), —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 , —CONR 5 R 8 , —SR 7 , —SOR 7 , —SO 2 R 7 , —SO 2 NR 5 R 6 , —NHCOR 5 , —NR 5 CONR 5 R 6 , and —NR 5 SO 2 R 7 , wherein said —(C 2 -C 6 )alkenyl and —(C 2 -C 6 )alkynyl R 2 moieties may be optionally substituted by one to three R 5 groups; R 1 is —(C 1 -C 6 )alkyl; and n is 1.
Another embodiment of the present invention is a compound of formula 1 wherein R 2 is —CO 2 R 5 and —CONR 5 R 6 optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —NO 2 , —CN, —(C 1 -C 6 )alkyl, —(C 2 -C 6 )alkenyl, —(C 2 -C 6 )alkynyl, —C═N—OH, —C═N—O((C 1 -C 6 )alkyl), —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 , —CONR 5 R 8 , —SR 7 , —SOR 7 , —SO 2 R 7 , —SO 2 NR 5 R 6 , —NHCOR 5 , —NR 5 CONR 5 R 6 , and —NR 5 SO 2 R 7 , wherein said —(C 2 -C 6 )alkenyl and —(C 2 -C 6 )alkynyl R 2 moieties may be optionally substituted by one to three R 5 groups; R 1 is —(C 1 -C 6 )alkyl; and n is 1.
Also provided is a compound of formula 1 wherein R 1 is selected from hydrogen, hydroxy, and —(C 1 -C 6 )alkyl, optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —CN, —(C 1 -C 6 )alkyl, —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 and —CONR 5 R 8 ; R 2 is hydrogen or —(C 1 -C 6 )alkyl, optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —NO 2 , —CN, —(C 1 -C 6 )alkyl, —(C 2 -C 6 )alkenyl, —(C 2 -C 6 )alkynyl, —C═N—OH, —C═N—O((C 1 -C 6 )alkyl), —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 , —CONR 5 R 8 , —SR 7 , —SOR 7 , —SO 2 R 7 , —SO 2 NR 5 R 6 , —NHCOR 5 , —NR 5 CONR 5 R 6 , and —NR 5 SO 2 R 7 , wherein said —(C 2 -C 6 )alkenyl and —(C 2 -C 6 )alkynyl R 2 moieties may be optionally substituted by one to three R 5 groups; and n is 1.
The invention further provides a compound of formula 1 wherein R 1 is selected from hydrogen, hydroxy, and —(C 1 -C 6 )alkyl, optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —CN, —(C 1 -C 6 )alkyl, —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 and —CONR 5 R 8 ; R 2 is hydrogen; and n is 1.
The present invention further provides a compound of formula 1, wherein R 1 is —(C 1 -C 6 )alkyl, optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —CN, —(C 1 -C 6 )alkyl, —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 and —CONR 5 R 8 ; R 2 is hydrogen; and n is 1.
The present invention also provides a compound of formula 1 wherein R 1 is selected from the group consisting of —(C 3 -C 7 )cycloalkyl and —(C 2 -C 9 )heterocyclyl, optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —CN, —(C 1 -C 6 )alkyl, —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 and —CONR 5 R 8 ; R 2 is hydrogen; and n is 1.
The invention also contemplates compounds of formula 1 wherein R 1 is selected from —O(C 1 -C 6 )alkyl, —O(C 3 -C 7 )cycloalkyl, and —O(C 2 -C 9 )heterocyclyl, optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —CN, —(C 1 -C 6 )alkyl, —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 and —CONR 5 R 8 ; R 2 is hydrogen; and n is 1.
One embodiment of the invention is a compound of formula 1 wherein R 1 is —NR 5 R 6 , optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —CN, —(C 1 -C 6 )alkyl, —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 and —CONR 5 R 8 ; R 2 is hydrogen; and n is 1.
A further embodiment of the invention is a compound of formula 1 wherein R 1 is selected from —SR 7 , —SOR 7 , —SO 2 R 7 , and —SO 2 NR 5 R 6 , optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —CN, —(C 1 -C 6 )alkyl, —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 and —CONR 5 R 8 ; R 2 is hydrogen; and n is 1.
The present invention also provides compounds of formula 1 wherein R 1 is —CO 2 R 5 , —CONR 5 R 6 , —NHCOR 5 , —NR 5 CONR 5 R 6 , or —NR 5 SO 2 R 7 , optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —CN, —(C 1 -C 6 )alkyl, —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 and —CONR 5 R 8 ; R 2 is hydrogen; and n is 1.
Also provided is a compound of formula 1 wherein R 2 is hydrogen or —(C 1 -C 6 )alkyl, optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —NO 2 , —CN, —(C 1 -C 6 )alkyl, —(C 2 -C 6 )alkenyl, —(C 2 -C 6 )alkynyl, —C═N—OH, —C═N—O((C 1 -C 6 )alkyl), —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 , —CONR 5 R 8 , —SR 7 , —SOR 7 , —SO 2 R 7 , —SO 2 NR 5 R 6 , —NHCOR 5 , —NR 5 CONR 5 R 6 , and —NR 5 SO 2 R 7 , wherein said —(C 2 -C 6 )alkenyl and —(C 2 -C 6 )alkynyl R 2 moieties may be optionally substituted by one to three R 5 groups; R 1 is hydrogen; and n is 1.
Further provided is a compound of formula 1 wherein R 2 is —(C 3 -C 7 )cycloalkyl, or —(C 2 -C 9 )heterocyclyl, optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —NO 2 , —CN, —(C 1 -C 6 )alkyl, —(C 2 -C 6 )alkenyl, —(C 2 -C 6 )alkynyl, —C═N—OH, —C═N—O((C 1 -C 6 )alkyl), —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 , —CONR 5 R 8 , —SR 7 , —SOR 7 , —SO 2 R 7 , —SO 2 NR 5 R 6 , —NHCOR 5 , —NR 5 CONR 5 R 6 , and —NR 5 SO 2 R 7 , wherein said —(C 2 -C 6 )alkenyl and —(C 2 -C 6 )alkynyl R 2 moieties may be optionally substituted by one to three R 5 groups; R 1 is hydrogen; and n is 1.
Another embodiment of the present invention is a compound of formula 1 wherein R 2 is —CO 2 R 5 and —CONR 5 R 6 optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —NO 2 , —CN, —(C 1 -C 6 )alkyl, —(C 2 -C 6 )alkenyl, —(C 2 -C 6 )alkynyl, —C═N—OH, —C═N—O((C 1 -C 6 )alkyl), —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 , —CONR 5 R 8 , —SR 7 , —SOR 7 , —SO 2 R 7 , —SO 2 NR 5 R 6 , —NHCOR 5 , —NR 5 CONR 5 R 6 , and —NR 5 SO 2 R 7 , wherein said —(C 2 -C 6 )alkenyl and —(C 2 -C 6 )alkynyl R 2 moieties may be optionally substituted by one to three R 5 groups; R 1 is hydrogen; and n is 1.
Also provided is a compound of formula 1 wherein R 1 is selected from hydrogen, hydroxy, and —(C 1 -C 6 )alkyl, optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —CN, —(C 1 -C 6 )alkyl, —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 and —CONR 5 R 8 ; R 2 is hydrogen or —(C 1 -C 6 )alkyl, optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —NO 2 , —CN, —(C 1 -C 6 )alkyl, —(C 2 -C 6 )alkenyl, —(C 2 -C 6 )alkynyl, —C═N—OH, —C═N—O((C 1 -C 6 )alkyl), —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 , —CONR 5 R 8 , —SR 7 , —SOR 7 , —SO 2 R 7 , —SO 2 NR 5 R 6 , —NHCOR 5 , —NR 5 CONR 5 R 6 , and —NR 5 SO 2 R 7 , wherein said —(C 2 -C 6 )alkenyl and —(C 2 -C 6 )alkynyl R 2 moieties may be optionally substituted by one to three R 5 groups; and n is 2.
The invention further provides a compound of formula 1 wherein R 1 is selected from hydrogen, hydroxy, and —(C 1 -C 6 )alkyl, optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —CN, —(C 1 -C 6 )alkyl, —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 and —CONR 5 R 8 ; R 2 is —(C 1 -C 6 )alkyl; and n is 2.
The present invention further provides a compound of formula 1, wherein R 1 is —(C 1 -C 6 )alkyl, optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —CN, —(C 1 -C 6 )alkyl, —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 and —CONR 5 R 8 ; R 2 is —(C 1 -C 6 )alkyl; and n is 2.
The present invention also provides a compound of formula 1 wherein R 1 is selected from the group consisting of —(C 3 -C 7 )cycloalkyl and —(C 2 -C 9 )heterocyclyl, optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —CN, —(C 1 -C 6 )alkyl, —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 and —CONR 5 R 8 ; R 2 is —(C 1 -C 6 )alkyl; and n is 2.
The invention also contemplates compounds of formula 1 wherein R 1 is selected from —O(C 1 -C 6 )alkyl, —O(C 3 -C 7 )cycloalkyl, and —O(C 2 -C 9 )heterocyclyl, optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —CN, —(C 1 -C 6 )alkyl, —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 and —CONR 5 R 8 ; R 2 is —(C 1 -C 6 )alkyl; and n is 2.
One embodiment of the invention is a compound of formula 1 wherein R 1 is —NR 5 R 6 , optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —CN, —(C 1 -C 6 )alkyl, —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 and —CONR 5 R 8 ; R 2 is —(C 1 -C 6 )alkyl; and n is 2.
A further embodiment of the invention is a compound of formula 1 wherein R 1 is selected from —SR 7 , —SOR 7 , —SO 2 R 7 , and —SO 2 NR 5 R 6 , optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —CN, —(C 1 -C 6 )alkyl, —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 and —CONR 5 R 8 ; R 2 is —(C 1 -C 6 )alkyl; and n is 2.
The present invention also provides compounds of formula 1 wherein R 1 is —CO 2 R 5 , —CONR 5 R 6 , —NHCOR 5 , —NR 5 CONR 5 R 6 , or —NR 5 SO 2 R 7 , optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —CN, —(C 1 -C 6 )alkyl, —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 and —CONR 5 R 8 ; R 2 is —(C 1 -C 6 )alkyl; and n is 2.
Also provided is a compound of formula 1 wherein R 2 is hydrogen or —(C 1 -C 6 )alkyl, optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —NO 2 , —CN, —(C 1 -C 6 )alkyl, —(C 2 -C 6 )alkenyl, —(C 2 -C 6 )alkynyl, —C═N—OH, —C═N—O((C 1 -C 6 )alkyl), —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 , —CONR 5 R 8 , —SR 7 , —SOR 7 , —SO 2 R 7 , —SO 2 NR 5 R 6 , —NHCOR 5 , —NR 5 CONR 5 R 6 , and —NR 5 SO 2 R 7 , wherein said —(C 2 -C 6 )alkenyl and —(C 2 -C 6 )alkynyl R 2 moieties may be optionally substituted by one to three R 5 groups; R 1 is —(C 1 -C 6 )alkyl; and n is 2.
Further provided is a compound of formula 1 wherein R 2 is —(C 3 -C 7 )cycloalkyl, or —(C 2 -C 9 )heterocyclyl, optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —NO 2 , —CN, —(C 1 -C 6 )alkyl, —(C 2 -C 6 )alkenyl, —(C 2 -C 6 )alkynyl, —C═N—OH, —C═N—O((C 1 -C 6 )alkyl), —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 , —CONR 5 R 8 , —SR 7 , —SOR 7 , —SO 2 R 7 , —SO 2 NR 5 R 6 , —NHCOR 5 , —NR 5 CONR 5 R 6 , and —NR 5 SO 2 R 7 , wherein said —(C 2 -C 6 )alkenyl and —(C 2 -C 6 )alkynyl R 2 moieties may be optionally substituted by one to three R 5 groups; R 1 is —(C 1 -C 6 )alkyl; and n is 2.
Another embodiment of the present invention is a compound of formula 1 wherein R 2 is —CO 2 R 5 and —CONR 5 R 6 optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —NO 2 , —CN, —(C 1 -C 6 )alkyl, —(C 2 -C 6 )alkenyl, —(C 2 -C 6 )alkynyl, —C═N—OH, —C═N—O((C 1 -C 6 )alkyl), —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 , —CONR 5 R 8 , —SR 7 , —SOR 7 , —SO 2 R 7 , —SO 2 NR 5 R 6 , —NHCOR 5 , —NR 5 CONR 5 R 6 , and —NR 5 SO 2 R 7 , wherein said —(C 2 -C 6 )alkenyl and —(C 2 -C 6 )alkynyl R 2 moieties may be optionally substituted by one to three R 5 groups; R 1 is —(C 1 -C 6 )alkyl; and n is 2.
The invention further provides a compound of formula 1 wherein R 1 is selected from hydrogen, hydroxy, and —(C 1 -C 6 )alkyl, optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —CN, —(C 1 -C 6 )alkyl, —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 and —CONR 5 R 8 ; R 2 is —(C 1 -C 6 )alkyl; and n is 2.
The present invention further provides a compound of formula 1, wherein R 1 is —(C 1 -C 6 )alkyl, optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —CN, —(C 1 -C 6 )alkyl, —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 and —CONR 5 R 8 ; R 2 is —(C 1 -C 6 )alkyl; and n is 2.
The present invention also provides a compound of formula 1 wherein R 1 is selected from the group consisting of —(C 3 -C 7 )cycloalkyl and —(C 2 -C 9 )heterocyclyl, optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —CN, —(C 1 -C 6 )alkyl, —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 and —CONR 5 R 8 ; R 2 is —(C 1 -C 6 )alkyl; and n is 2.
The invention also contemplates compounds of formula 1 wherein R 1 is selected from —O(C 1 -C 6 )alkyl, —O(C 3 -C 7 )cycloalkyl, and —O(C 2 -C 9 )heterocyclyl, optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —CN, —(C 1 -C 6 )alkyl, —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 and —CONR 5 R 8 ; R 2 is —(C 1 -C 6 )alkyl; and n is 2.
One embodiment of the invention is a compound of formula 1 wherein R 1 is —NR 5 R 6 , optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —CN, —(C 1 -C 6 )alkyl, —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 and —CONR 5 R 8 ; R 2 is —(C 1 -C 6 )alkyl; and n is 2.
A further embodiment of the invention is a compound of formula 1 wherein R 1 is selected from —SR 7 , —SOR 7 , —SO 2 R 7 , and —SO 2 NR 5 R 6 , optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —CN, —(C 1 -C 6 )alkyl, —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 and —CONR 5 R 8 ; R 2 is —(C 1 -C 6 )alkyl; and n is 2.
The present invention also provides compounds of formula 1 wherein R 1 is —CO 2 R 5 , —CONR 5 R 6 , —NHCOR 5 , —NR 5 CONR 5 R 6 , or —NR 5 SO 2 R 7 , optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —CN, —(C 1 -C 6 )alkyl, —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 and —CONR 5 R 8 ; R 2 is —(C 1 -C 6 )alkyl; and n is 2.
Also provided is a compound of formula 1 wherein R 2 is hydrogen or —(C 1 -C 6 )alkyl, optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —NO 2 , —CN, —(C 1 -C 6 )alkyl, —(C 2 -C 6 )alkenyl, —(C 2 -C 6 )alkynyl, —C═N—OH, —C═N—O((C 1 -C 6 )alkyl), —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 , —CONR 5 R 8 , —SR 7 , —SOR 7 , —SO 2 R 7 , —SO 2 NR 5 R 6 , —NHCOR 5 , —NR 5 CONR 5 R 6 , and —NR 5 SO 2 R 7 , wherein said —(C 2 -C 6 )alkenyl and —(C 2 -C 6 )alkynyl R 2 moieties may be optionally substituted by one to three R 5 groups; R 1 is —(C 1 -C 6 )alkyl; and n is 2.
Further provided is a compound of formula 1 wherein R 2 is —(C 3 -C 7 )cycloalkyl, or —(C 2 -C 9 )heterocyclyl, optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —NO 2 , —CN, —(C 1 -C 6 )alkyl, —(C 2 -C 6 )alkenyl, —(C 2 -C 6 )alkynyl, —C═N—OH, —C═N—O((C 1 -C 6 )alkyl), —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 , —CONR 5 R 8 , —SR 7 , —SOR 7 , —SO 2 R 7 , —SO 2 NR 5 R 6 , —NHCOR 5 , —NR 5 CONR 5 R 6 , and —NR 5 SO 2 R 7 , wherein said —(C 2 -C 6 )alkenyl and —(C 2 -C 6 )alkynyl R 2 moieties may be optionally substituted by one to three R 5 groups; R 1 is —(C 1 -C 6 )alkyl; and n is 2.
Another embodiment of the present invention is a compound of formula 1 wherein R 2 is —CO 2 R 5 and —CONR 5 R 6 optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —NO 2 , —CN, —(C 1 -C 6 )alkyl, —(C 2 -C 6 )alkenyl, —(C 2 -C 6 )alkynyl, —C═N—OH, —C═N—O((C 1 -C 6 )alkyl), —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 , —CONR 5 R 8 , —SR 7 , —SOR 7 , —SO 2 R 7 , —SO 2 NR 5 R 6 , —NHCOR 5 , —NR 5 CONR 5 R 6 , and —NR 5 SO 2 R 7 , wherein said —(C 2 -C 6 )alkenyl and —(C 2 -C 6 )alkynyl R 2 moieties may be optionally substituted by one to three R 5 groups; R 1 is —(C 1 -C 6 )alkyl; and n is 2.
Also provided is a compound of formula 1 wherein R 1 is selected from hydrogen, hydroxy, and —(C 1 -C 6 )alkyl, optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —CN, —(C 1 -C 6 )alkyl, —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 and —CONR 5 R 8 ; R 2 is hydrogen or —(C 1 -C 6 )alkyl, optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —NO 2 , —CN, —(C 1 -C 6 )alkyl, —(C 2 -C 6 )alkenyl, —(C 2 -C 6 )alkynyl, —C═N—OH, —C═N—O((C 1 -C 6 )alkyl), —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 , —CONR 5 R 8 , —SR 7 , —SOR 7 , —SO 2 R 7 , —SO 2 NR 5 R 6 , —NHCOR 5 , —NR 5 CONR 5 R 6 , and —NR 5 SO 2 R 7 , wherein said —(C 2 -C 6 )alkenyl and —(C 2 -C 6 )alkynyl R 2 moieties may be optionally substituted by one to three R 5 groups; and n is 2.
The invention further provides a compound of formula 1 wherein R 1 is selected from hydrogen, hydroxy, and —(C 1 -C 6 )alkyl, optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —CN, —(C 1 -C 6 )alkyl, —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 and —CONR 5 R 8 ; R 2 is hydrogen; and n is 2.
The present invention further provides a compound of formula 1, wherein R 1 is —(C 1 -C 6 )alkyl, optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —CN, —(C 1 -C 6 )alkyl, —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 and —CONR 5 R 8 ; R 2 is hydrogen; and n is 2.
The present invention also provides a compound of formula 1 wherein R 1 is selected from the group consisting of —(C 3 -C 7 )cycloalkyl and —(C 2 -C 9 )heterocyclyl, optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —CN, —(C 1 -C 6 )alkyl, —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 and —CONR 5 R 8 ; R 2 is hydrogen; and n is 2.
The invention also contemplates compounds of formula 1 wherein R 1 is selected from —O(C 1 -C 6 )alkyl, —O(C 3 -C 7 )cycloalkyl, and —O(C 2 -C 9 )heterocyclyl, optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —CN, —(C 1 -C 6 )alkyl, —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 and —CONR 5 R 8 ; R 2 is hydrogen; and n is 2.
One embodiment of the invention is a compound of formula 1 wherein R 1 is —NR 5 R 6 , optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —CN, —(C 1 -C 6 )alkyl, —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 and —CONR 5 R 8 ; R 2 is hydrogen; and n is 2.
A further embodiment of the invention is a compound of formula 1 wherein R 1 is selected from —SR 7 , —SOR 7 , —SO 2 R 7 , and —SO 2 NR 5 R 6 , optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —CN, —(C 1 -C 6 )alkyl, —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 and —CONR 5 R 8 ; R 2 is hydrogen; and n is 2.
The present invention also provides compounds of formula 1 wherein R 1 is —CO 2 R 5 , —CONR 5 R 6 , —NHCOR 5 , —NR 5 CONR 5 R 6 , or —NR 5 SO 2 R 7 , optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —CN, —(C 1 -C 6 )alkyl, —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 and —CONR 5 R 8 ; R 2 is hydrogen; and n is 2.
Also provided is a compound of formula 1 wherein R 2 is hydrogen or —(C 1 -C 6 )alkyl, optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —NO 2 , —CN, —(C 1 -C 6 )alkyl, —(C 2 -C 6 )alkenyl, —(C 2 -C 6 )alkynyl, —C═N—OH, —C═N—O((C 1 -C 6 )alkyl), —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 , —CONR 5 R 8 , —SR 7 , —SOR 7 , —SO 2 R 7 , —SO 2 NR 5 R 6 , —NHCOR 5 , —NR 5 CONR 5 R 6 , and —NR 5 SO 2 R 7 , wherein said —(C 2 -C 6 )alkenyl and —(C 2 -C 6 )alkynyl R 2 moieties may be optionally substituted by one to three R 5 groups; R 1 is hydrogen; and n is 2.
Further provided is a compound of formula 1 wherein R 2 is —(C 3 -C 7 )cycloalkyl, or —(C 2 -C 9 )heterocyclyl, optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —NO 2 , —CN, —(C 1 -C 6 )alkyl, —(C 2 -C 6 )alkenyl, —(C 2 -C 6 )alkynyl, —C═N—OH, —C═N—O((C 1 -C 6 )alkyl), —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 , —CONR 5 R 8 , —SR 7 , —SOR 7 , —SO 2 R 7 , —SO 2 NR 5 R 6 , —NHCOR 5 , —NR 5 CONR 5 R 6 , and —NR 5 SO 2 R 7 , wherein said —(C 2 -C 6 )alkenyl and —(C 2 -C 6 )alkynyl R 2 moieties may be optionally substituted by one to three R 5 groups; R 1 is hydrogen; and n is 2.
Another embodiment of the present invention is a compound of formula 1 wherein R 2 is —CO 2 R 5 and —CONR 5 R 6 optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, hydroxy, —NO 2 , —CN, —(C 1 -C 6 )alkyl, —(C 2 -C 6 )alkenyl, —(C 2 -C 6 )alkynyl, —C═N—OH, —C═N—O((C 1 -C 6 )alkyl), —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 , —CONR 5 R 8 , —SR 7 , —SOR 7 , —SO 2 R 7 , —SO 2 NR 5 R 6 , —NHCOR 5 , —NR 5 CONR 5 R 6 , and —NR 5 SO 2 R 7 , wherein said —(C 2 -C 6 )alkenyl and —(C 2 -C 6 )alkynyl R 2 moieties may be optionally substituted by one to three R 5 groups; R 1 is hydrogen; and n is 2.
The present invention also provides a compound of formula 1 in which R 1 and R 2 are taken together with the atom(s) to which they are attached to form a —(C 3 -C 10 )cycloalkyl optionally substituted by one to three moieties selected from the group consisting of a hydrogen, halogen, hydroxy, —NO 2 , —CN, —(C 1 -C 6 )alkyl, —(C 2 -C 6 )alkenyl, —(C 2 -C 6 )alkynyl, —C═N—OH, —C═N—O(C 1 -C 6 alkyl), —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 , —CONR 5 R 8 , —SR 7 , —SOR 7 , —SO 2 R 7 , —SO 2 NR 5 R 6 , —NHCOR 5 , —NR 5 CONR 5 R 6 , and —NR 5 SO 2 R 7 , wherein said —(C 2 -C 6 )alkenyl and —(C 2 -C 6 )alkynyl moieties of said cyclic group may be optionally substituted by one to three R 5 groups.
The present invention further provides a compound of formula 1 in which R 1 and R 2 are taken together with the atom(s) to which they are attached to form a —(C 2 -C 9 )heterocyclyl optionally substituted by one to three moieties selected from the group consisting of a hydrogen, halogen, hydroxy, —NO 2 , —CN, —(C 1 -C 6 )alkyl, —(C 2 -C 6 )alkenyl, —(C 2 -C 6 )alkynyl, —C═N—OH, —C═N—O(C 1 -C 6 alkyl), —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 , —CONR 5 R 8 , —SR 7 , —SOR 7 , —SO 2 R 7 , —SO 2 NR 5 R 6 , —NHCOR 5 , —NR 5 CONR 5 R 6 , and —NR 5 SO 2 R 7 , wherein said —(C 2 -C 6 )alkenyl and —(C 2 -C 6 )alkynyl moieties of said cyclic group may be optionally substituted by one to three R 5 groups.
The present invention also provides a compound of formula 1 in which R 1 and R 2 are taken together with the atom(s) to which they are attached to form a —(C 3 -C 10 )cycloalkyl optionally substituted by one to three moieties selected from the group consisting of a hydrogen, halogen, hydroxy, —NO 2 , —CN, —(C 1 -C 6 )alkyl, —(C 2 -C 6 )alkenyl, —(C 2 -C 6 )alkynyl, —C═N—OH, —C═N—O(C 1 -C 6 alkyl), —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 , —CONR 5 R 8 , —SR 7 , —SOR 7 , —SO 2 R 7 , —SO 2 NR 5 R 6 , —NHCOR 5 , —NR 5 CONR 5 R 6 , and —NR 5 SO 2 R 7 , wherein said —(C 2 -C 6 )alkenyl and —(C 2 -C 6 )alkynyl moieties of said cyclic group may be optionally substituted by one to three R 5 groups; and n is 1.
The present invention further provides a compound of formula 1 in which R 1 and R 2 are taken together with the atom(s) to which they are attached to form a —(C 2 -C 9 )heterocyclyl optionally substituted by one to three moieties selected from the group consisting of a hydrogen, halogen, hydroxy, —NO 2 , —CN, —(C 1 -C 6 )alkyl, —(C 2 -C 6 )alkenyl, —(C 2 -C 6 )alkynyl, —C═N—OH, —C═N—O(C 1 -C 6 alkyl), —NR 5 R 6 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , —CONR 5 R 6 , —CONR 5 R 8 , —SR 7 , —SOR 7 , —SO 2 R 7 , —SO 2 NR 5 R 6 , —NHCOR 5 , —NR 5 CONR 5 R 6 , and —NR 5 SO 2 R 7 , wherein said —(C 2 -C 6 )alkenyl and —(C 2 -C 6 )alkynyl moieties of said cyclic group may be optionally substituted by one to three R 5 groups; and n is 1.
The present invention also provides a compound of formula 1 wherein R 3 is hydrogen.
Preferably, R 3 is —(C 6 -C 10 )aryl or —(C 1 -C 9 )heteroaryl, optionally substituted by one to three moieties independently selected from the group consisting of halogen, hydroxy, —(C 1 -C 6 )alkyl, —(C 1 -C 6 )alkyl-P(O)(O(C 1 -C 6 )alkyl) 2 , —(C 3 -C 10 )cycloalkyl, (C 6 -C 10 )aryl, (C 2 -C 9 )heterocyclyl, —(C 1 -C 9 )heteroaryl, —NR 5 R 6 , —NHSO 2 (C 1 -C 6 )alkyl, —NHSO 2 (C 3 -C 6 )cycloalkyl, —N((C 1 -C 6 )alkyl)(SO 2 —C 1 -C 6 )alkyl), —N((C 1 -C 6 )alkyl)(SO 2 (C 3 -C 6 )cycloalkyl), —O(C 1 -C 6 )alkyl, —O—SO 2 (C 1 -C 6 )alkyl, —(CO)(C 1 -C 6 )alkyl, —(CO)CF 3 , —(CO)(C 3 -C 10 )cycloalkyl, —(CO)(C 6 -C 10 )aryl, —(CO)(C 2 -C 9 )heterocyclyl, —(CO)(C 1 -C 9 )heteroaryl, —(CO)O(C 1 -C 6 )alkyl, —(CO)O(C 3 -C 10 )cycloalkyl, —(CO)O(C 6 -C 10 )aryl, —(CO)O(C 2 -C 9 )heterocyclyl, —(CO)O(C 1 -C 9 )heteroaryl, —(CO)(C 1 -C 6 )alkyl-O(C 1 -C 6 )alkyl, —SO 2 (C 1 -C 6 )alkyl, —SO 2 (C 3 -C 6 )cycloalkyl, SO 2 CF 3 , SO 2 NH 2 , SO 2 NH(C 1 -C 6 )alkyl, —SO 2 NH(C 3 -C 6 )cycloalkyl, —SO 2 N((C 1 -C 6 )alkyl) 2 , —SO 2 N((C 3 -C 6 )cycloalkyl) 2 , —SO 2 NR 5 R 6 , and —SO 2 N(C 1 -C 6 )alkyl-(C 6 -C 10 )aryl; wherein said —(C 6 -C 10 )aryl or —(C 1 -C 9 )heteroaryl are optionally interrupted by one to three elements selected from the group consisting of —(C═O), —SO 2 , —S—, —O—, —N—, —NH— and —NR 5 ; and R 5 and R 6 of said NR 5 R 6 R 3 (b) group may be taken together with the atoms to which they are attached to form a —(C 2 -C 9 )heterocyclyl.
Alternatively, the invention provides a compound of formula 1 wherein R 3 is —(C 6 -C 10 )aryl, optionally substituted by one to three moieties independently selected from the group consisting of halogen, hydroxy, —(C 1 -C 6 )alkyl, —(C 3 -C 10 )cycloalkyl, —NHSO 2 (C 1 -C 6 )alkyl, —NHSO 2 (C 3 -C 6 )cycloalkyl, —N((C 1 -C 6 )alkyl)(SO 2 —C 1 -C 6 )alkyl), —N((C 1 -C 6 )alkyl)SO 2 (C 3 -C 6 )cycloalkyl), —O(C 1 -C 6 )alkyl, —O—SO 2 (C 1 -C 6 )alkyl, —SO 2 (C 1 -C 6 )alkyl, —SO 2 NH 2 , —SO 2 NH(C 1 -C 6 )alkyl, —SO 2 NH(C 3 -C 6 )cycloalkyl, —SO 2 N((C 1 -C 6 )alkyl) 2 , —SO 2 N((C 3 -C 6 )cycloalkyl) 2 , and —SO 2 NR 5 R 6 .
The invention also provides a compound of formula 1 wherein R 3 is —(C 1 -C 9 )heteroaryl, optionally substituted by one to three moieties independently selected from the group consisting of halogen, hydroxy, —(C 1 -C 6 )alkyl, —(C 3 -C 10 )cycloalkyl, —NHSO 2 (C 1 -C 6 )alkyl, —NHSO 2 (C 3 -C 6 )cycloalkyl, —N((C 1 -C 6 )alkyl)(SO 2 —C 1 -C 6 )alkyl), —N((C 1 -C 6 )alkyl)(SO 2 (C 3 -C 6 )cycloalkyl), —O(C 1 -C 6 )alkyl, —O—SO 2 (C 1 -C 6 )alkyl, —SO 2 (C 1 -C 6 )alkyl, —SO 2 (C 3 -C 6 )cycloalkyl, —SO 2 NH 2 , —SO 2 NH(C 1 -C 6 )alkyl, —SO 2 NH(C 3 -C 6 )cycloalkyl, —SO 2 N((C 1 -C 6 )alkyl) 2 , —SO 2 N((C 3 -C 6 )cycloalkyl) 2 , and —SO 2 NR 5 R 6 .
Further, the invention provides a compound in which R 3 is selected from —(C 3 -C 10 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, and —(C 1 -C 6 )alkyl-(C 2 -C 9 )heterocyclyl, optionally substituted by one to three moieties independently selected from the group consisting of halogen, hydroxy, —(C 1 -C 6 )alkyl, —(C 1 -C 6 )alkyl-P(O)(O(C 1 -C 6 )alkyl) 2 , —(C 3 -C 10 )cycloalkyl, (C 6 -C 10 )aryl, (C 2 -C 9 )heterocyclyl, —(C 1 -C 9 )heteroaryl, —NR 5 R 6 , —NSO 2 (C 1 -C 6 )alkyl, —NHSO 2 (C 3 -C 6 )cycloalkyl, —N((C 1 -C 6 )alkyl)(SO 2 —C 1 -C 6 )alkyl), —N((C 1 -C 6 )alkyl)(SO 2 (C 3 -C 6 )cycloalkyl), —O(C 1 -C 6 )alkyl, —O—SO 2 (C 1 -C 6 )alkyl, —O—SO 2 (C 1 -C 6 )alkyl, —(CO)(C 1 -C 6 )alkyl, —(CO)CF 3 , —(CO)(C 3 -C 10 )cycloalkyl, —(CO)(C 6 -C 10 )aryl, —(CO)(C 2 -C 9 )heterocyclyl, —(CO)(C 1 -C 9 )heteroaryl, —(CO)O(C 1 -C 6 )alkyl, —(CO)O(C 3 -C 10 )cycloalkyl, —(CO)O(C 6 -C 10 )aryl, —(CO)O(C 2 -C 9 )heterocyclyl, —(CO)O(C 1 -C 9 )heteroaryl, —(CO)(C 1 -C 6 )alkyl-O(C 1 -C 6 )alkyl, —SO 2 (C 1 -C 6 )alkyl, —SO 2 (C 1 -C 6 )alkyl, —SO 2 (C 3 -C 6 )cycloalkyl, SO 2 CF 3 , SO 2 NH 2 , SO 2 NH(C 1 -C 6 )alkyl, —SO 2 NH(C 3 -C 6 )cycloalkyl, —SO 2 N((C 1 -C 6 )alkyl) 2 , —SO 2 N((C 3 -C 6 )cycloalkyl) 2 , —SO 2 NR 5 R 6 , and —SO 2 N(C 1 -C 6 )alkyl-(C 6 -C 10 )aryl; wherein said —(C 3 -C 10 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, and —(C 1 -C 6 )alkyl-(C 2 -C 9 )heterocyclyl are optionally interrupted by one to three elements selected from the group consisting of —(C═O), —SO 2 , —S—, —O—, —N—, —NH— and —NR 5 ; and R 5 and R 6 of said NR 5 R 6 R 3 (b) group taken together with the atoms to which they are attached to form a —(C 2 -C 9 )heterocyclyl.
Also provided is a compound in which R 3 is —(C 3 -C 10 )cycloalkyl, optionally substituted by one to three moieties independently selected from the group consisting of halogen, hydroxy, —(C 1 -C 6 )alkyl, —(C 3 -C 10 )cycloalkyl, —NSO 2 (C 1 -C 6 )alkyl, —NHSO 2 (C 3 -C 6 )cyccloalkyl, —N((C 1 -C 6 )alkyl)(SO 2 —C 1 -C 6 )alkyl), —N((C 1 -C 6 )alkyl)(SO 2 (C 3 -C 6 )cycloalkyl), —O(C 1 -C 6 )alkyl, —O—SO 2 (C 1 -C 6 )alkyl, —SO 2 (C 1 -C 6 )alkyl, —SO 2 (C 3 -C 6 )cycloalkyl, SO 2 NH 2 , SO 2 NH(C 1 -C 6 )alkyl, —SO 2 NH(C 3 -C 6 )cycloalkyl, —SO 2 N((C 1 -C 6 )alkyl) 2 , —SO 2 N((C 3 -C 6 )cycloalkyl) 2 , —SO 2 NR 5 R 6 .
The invention further provides a compound in which R 3 is —(C 2 -C 9 )heterocyclyl, optionally substituted by one to three moieties independently selected from the group consisting of halogen, hydroxy, —(C 1 -C 6 )alkyl, —(C 3 -C 10 )cycloalkyl, —NSO 2 (C 1 -C 6 )alkyl, —NHSO 2 (C 3 -C 6 )cycloalkyl, —N((C 1 -C 6 )alkyl)(SO 2 —C 1 -C 6 )alkyl), —N((C 1 -C 6 )alkyl)(SO 2 (C 3 -C 6 )cycloalkyl), —O(C 1 -C 6 )alkyl, —O—SO 2 (C 1 -C 6 )alkyl, —SO 2 (C 1 -C 6 )alkyl, —SO 2 (C 3 -C 6 )cycloalkyl, SO 2 NH 2 , SO 2 NH(C 1 -C 6 )alkyl, —SO 2 NH(C 3 -C 6 )cycloalkyl, —SO 2 N((C 1 -C 6 )alkyl) 2 , —SO 2 N((C 3 -C 6 )cycloalkyl) 2 , and —SO 2 NR 5 R 6 .
The invention further provides a compound in which R 3 is —(C 1 -C 6 )alkyl-(C 2 -C 9 ) heterocyclyl, optionally substituted by one to three moieties independently selected from the group consisting of halogen, hydroxy, —(C 1 -C 6 )alkyl, —(C 3 -C 10 )cycloalkyl, —NSO 2 (C 1 -C 6 )alkyl, —NHSO 2 (C 3 -C 6 )cycloalkyl, —N((C 1 -C 6 )alkyl)(SO 2 —C 1 -C 6 )alkyl), —N((C 1 -C 6 )alkyl)(SO 2 (C 3 -C 6 )cycloalkyl), —O(C 1 -C 6 )alkyl, —O—SO 2 (C 1 -C 6 )alkyl, —SO 2 (C 1 -C 6 )cycloalkyl, SO 2 NH 2 , SO 2 NH(C 1 -C 6 )alkyl, —SO 2 NH(C 3 -C 6 )cycloalkyl, —SO 2 N((C 1 -C 6 )alkyl) 2 , —SO 2 N((C 3 -C 6 )cycloalkyl) 2 , and —SO 2 NR 5 R 6 .
Moreover, the invention provides a compound of formula 1 wherein R 3 is —(C 1 -C 6 )alkyl optionally substituted by one to three moieties selected from the group consisting of halogen, hydroxy, —(C 1 -C 6 )alkyl, —(C 1 -C 6 )alkyl-P(O)(O(C 1 -C 6 )alkyl) 2 , —(C 3 -C 10 )cycloalkyl, (C 6 -C 10 )aryl, (C 2 -C 9 )heterocyclyl, —(C 1 -C 9 )heteroaryl, —NR 5 R 6 , —NSO 2 (C 1 -C 6 )alkyl, —NHSO 2 (C 3 -C 6 )cycloalkyl, —N((C 1 -C 6 )alkyl)(SO 2 —C 1 -C 6 )alkyl), —N((C 1 -C 6 )alkyl)(SO 2 (C 3 -C 6 )cycloalkyl), —O(C 1 -C 6 )alkyl, —O—SO 2 (C 1 -C 6 )alkyl, —(CO)(C 1 -C 6 )alkyl, —(CO)CF 3 , —(CO)(C 3 -C 10 )cycloalkyl, —(CO)(C 6 -C 10 )aryl, —(CO)(C 2 -C 9 )heterocyclyl, —(CO)(C 1 -C 9 )heteroaryl, —(CO)O(C 1 -C 6 )alkyl, —(CO)O(C 3 -C 10 )cycloalkyl, —(CO)O(C 6 -C 10 )aryl, —(CO)O(C 2 -C 9 )heterocyclyl, —(CO)O(C 1 -C 9 )heteroaryl, —(CO)(C 1 -C 6 )alkyl-O(C 1 -C 6 )alkyl, —SO 2 (C 1 -C 6 )alkyl, —SO 2 (C 3 -C 6 )cycloalkyl, SO 2 CF 3 , SO 2 NH 2 , SO 2 NH(C 1 -C 6 )alkyl, —SO 2 NH(C 3 -C 6 )cycloalkyl, —SO 2 N((C 1 -C 6 )alkyl) 2 , —SO 2 N((C 3 -C 6 )cycloalkyl) 2 , —SO 2 NR 5 R 6 , and —SO 2 N(C 1 -C 6 )alkyl-(C 6 -C 10 )aryl; wherein said —(C 1 -C 6 )alkyl is optionally interrupted by one to three elements selected from the group consisting of —(C═O), —SO 2 , —S—, —O—, —N—, —NH— and —NR 5 ; and R 5 and R 6 of said NR 5 R 6 R 3 (b) group may be taken together with the atoms to which they are attached to form a —(C 2 -C 9 )heterocyclyl.
Further provided is a compound of formula 1 wherein R 3 is —(C 1 -C 6 )alkyl optionally substituted by one to three moieties selected from the group consisting of halogen, hydroxy, —(C 1 -C 6 )alkyl, —(C 3 -C 10 )cycloalkyl, —NSO 2 (C 1 -C 6 )alkyl, —NHSO 2 (C 3 -C 6 )cycloalkyl, —N((C 1 -C 6 )alkyl)(SO 2 —C 1 -C 6 )alkyl), —N((C 1 -C 6 )alkyl)(SO 2 (C 3 -C 6 )cycloalkyl), —O(C 1 -C 6 )alkyl, —SO 2 NH(C 1 -C 6 )alkyl, —SO 2 (C 1 -C 6 )alkyl, —SO 2 (C 3 -C 6 )cycloalkyl, —SO 2 NH 2 , SO 2 NH(C 1 -C 6 )alkyl, —SO 2 NH(C 3 -C 6 )cycloalkyl, —SO 2 N((C 1 -C 6 )alkyl) 2 , —SO 2 N((C 3 -C 6 )cycloalkyl) 2 , and —SO 2 NR 5 R 6 .
In a preferred embodiment, R 4 is a substituent selected from the group consisting of hydrogen, (C 1 -C 6 )alkyl, and —(C 3 -C 7 )cycloalkyl; wherein said —(C 1 -C 6 )alkyl and —(C 3 -C 7 )cycloalkyl is optionally substituted by one to three moieties independently selected from the group consisting of hydrogen, halogen, —(C 1 -C 6 )alkyl, —CN, —NR 5 2 , —OR 5 , —(C 3 -C 7 )cycloalkyl, —(C 2 -C 9 )heterocyclyl, —CO 2 R 5 , and —CONR 5 R 8 ; with the proviso that a heteroatom of the foregoing R 4 substituents may not be bound to an sp 3 carbon atom bound to another heteroatom; and wherein R 5 and R 8 of said —CONR 5 R 8 group may be taken together with the atoms to which they are attached to form a —(C 2 -C 9 )heterocyclyl.
In a further preferred embodiment, R 4 is hydrogen.
Further, the invention provides a compound of formula 1 wherein R 5 and R 6 are each substituents independently selected from the group consisting of hydrogen and —(C 1 -C 6 )alkyl, optionally substituted as described above.
In a preferred embodiment, the present invention provides a compound of the formula 2
wherein A is selected from the group consisting of:
wherein m is an integer from 0-3 and R 13 is a substituent selected from the group consisting of hydrogen, halogen, hydroxy, (C 1 -C 6 )-alkyl, (C 3 -C 7 )-cycloalkyl, (C 6 -C 10 )-aryl, (C 1 -C 9 )heteroaryl, (C 2 -C 9 )-heterocyclyl, O—(C 1 -C 6 )-alkyl, O—(C 3 -C 7 )-cycloalkyl, SO 2 -(C 1 -C 6 )alkyl, SO 2 (C 3 -C 7 )-cycloalkyl, NHSO 2 (C 1 -C 6 )alkyl, N((C 1 -C 6 )alkyl)(SO 2 (C 1 -C 6 -alkyl)), N((C 3 -C 7 )cycloalkyl)(SO 2 (C 1 -C 6 -alkyl)), N(C 1 -C 6 -alkyl)(SO 2 (C 3 -C 7 )cycloalkyl), N((C 3 -C 7 )cycloalkyl)(SO 2 (C 3 -C 7 )cycloalkyl), OSO 2 (C 1 -C 6 )alkyl, SO 2 CF 3 , SO 2 NH 2 , SO 2 NH(C 1 -C 6 )alkyl, SO 2 NH(C 3 -C 7 )cycloalkyl, SO 2 NR 5 R 6 , SO 2 N((C 1 -C 6 )alkyl) 2 , CF 3 , CO—(C 1 -C 6 )alkyl, CO—(C 3 -C 7 )cycloalkyl, COCF 3 , CO 2 (C 1 -C 6 )alkyl,
Also provided is a compound of the formula 3
wherein B is selected from the group consisting of:
The present invention also provides a compound of formula 4
wherein D is selected from the group consisting of:
wherein q is an integer from 1-2.
Moreover, the present invention provides a compound of formula 5:
wherein E is selected from the group consisting of:
wherein R 14 is selected from the group consisting of (C 1 -C 6 )-alkyl, (C 3 -C 7 )-cycloalkyl, and (C 2 -C 9 )-heterocyclyl, and R 15 is selected from the group consisting of hydrogen, (C 1 -C 6 )-alkyl, (C 3 -C 7 )-cycloalkyl, and (C 2 -C 9 )-heterocyclyl.
Specific embodiments of the present invention are compounds selected from
N-(1-Methyl-1-phenyl-ethyl)-3-{[2-(2-oxo-2,3-dihydro-1H-indol-5-ylamino)-5-trifluoromethyl-pyrimidin-4-ylamino]-methyl}-benzenesulfonamide; 3-{[2-(2-Oxo-2,3-dihydro-1H-indol-5-ylamino)-5-trifluoromethyl-pyrimidin-4-ylamino]-methyl}-benzenesulfonamide; 5-{4-[3-(Trifluoro-methanesulfonyl)-benzylamino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; 5-{4-[(Piperidin-3-ylmethyl)-amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; 5-{4-[(1-Methanesulfonyl-piperidin-3-ylmethyl)-amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; N-(3-{[2-(2-Oxo-2,3-dihydro-1H-indol-5-ylamino)-5-trifluoromethyl-pyrimidin-4-ylamino]-methyl}-phenyl)-methanesulfonamide; 3-Oxo-3-(3-{[2-(2-oxo-2,3-dihydro-1H-indol-5-ylamino)-5-trifluoromethyl-pyrimidin-4-ylamino]-methyl}-piperidin-1-yl)-propionitrile; 5-{4-[3-(1,1-Dioxo-1N 6 -isothiazolidin-2-yl)-propylamino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; 5-[4-(2-Methyl-butylamino)-5-trifluoromethyl-pyrimidin-2-ylamino]-1,3-dihydro-indol-2-one; 5-{4-[(1-Methanesulfonyl-piperidin-2-ylmethyl)-amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; N-{2-[2-(2-Oxo-2,3-dihydro-1H-indol-5-ylamino)-5-trifluoromethyl-pyrimidin-4-ylamino]-ethyl}-methanesulfonamide; N-{4-[2-(2-Oxo-2,3-dihydro-1H-indol-5-ylamino)-5-trifluoromethyl-pyrimidin-4-ylamino]-butyl}-methanesulfonamide; 5-{4-[(1-Methanesulfonyl-piperidin-4-ylmethyl)-amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; N-Methyl-N-{2-[2-(2-oxo-2,3-dihydro-1H-indol-5-ylamino)-5-trifluoromethyl-pyrimidin-4-ylamino]-ethyl}-methanesulfonamide; Methanesulfonic acid 3-{[2-(2-oxo-2,3-dihydro-1H-indol-5-ylamino)-5-trifluoromethyl-pyrimidin-4-ylamino]-methyl}-phenyl ester; N-{3-[2-(2-Oxo-2,3-dihydro-1H-indol-5-ylamino)-5-trifluoromethyl-pyrimidin-4-ylamino]-propyl}-methanesulfonamide; 5-{4-[(4-Methanesulfonyl-morpholin-2-ylmethyl)-amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; N-(4-Fluoro-3-{[2-(2-oxo-2,3-dihydro-1H-indol-5-ylamino)-5-trifluoromethyl-pyrimidin-4-ylamino]-methyl}-phenyl)-methanesulfonamide; 5-{4-[(5-Oxo-morpholin-2-ylmethyl)-amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one N-(4-Methoxy-3-{[2-(2-oxo-2,3-dihydro-1H-indol-5-ylamino)-5-trifluoromethyl-pyrimidin-4-ylamino]-methyl}-phenyl)-methanesulfonamide; N-(4-Methyl-3-{[2-(2-oxo-2,3-dihydro-1H-indol-5-ylamino)-5-trifluoromethyl-pyrimidin-4-ylamino]-methyl}-phenyl)-methanesulfonamide; 5-[4-(3-Methanesulfonylmethyl-benzylamino)-5-trifluoromethyl-pyrimidin-2-ylamino]-1,3-dihydro-indol-2-one; 5-{4-[(4-Trifluoroacetyl-morpholin-2-ylmethyl)-amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; 5-{4-[(1-Methanesulfonyl-azetidin-3-ylmethyl)-amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; N-Methyl-N-(4-methyl-3-{[2-(2-oxo-2,3-dihydro-1H-indol-5-ylamino)-5-trifluoromethyl-pyrimidin-4-ylamino]-methyl}-phenyl)-methanesulfonamide; 5-{4-[(1-Methanesulfonyl-pyrrolidin-3-ylmethyl)-amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; N-Methyl-N-{3-[2-(2-oxo-2,3-dihydro-1H-indol-5-ylamino)-5-trifluoromethyl-pyrimidin-4-ylamino]-propyl}-methanesulfonamide; 5-{4-[2-(1-Methanesulfonyl-piperidin-2-yl)-ethylamino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; 5-{4-[(4-Methanesulfonyl-pyridin-2-ylmethyl)-amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; {2,2-Dimethyl-3-[2-(2-oxo-2,3-dihydro-1H-indol-5-ylamino)-5-trifluoromethyl-pyrimidin-4-ylamino]-propyl}-carbamic acid tert-butyl ester; 5-[4-(3-Isopropoxy-propylamino)-5-trifluoromethyl-pyrimidin-2-ylamino]-1,3-dihydro-indol-2-one; 5-{4-[(1-Methyl-piperidin-3-ylmethyl)-amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; 5-{4-[(Tetrahydro-pyran-4-ylmethyl)-amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; 5-[4-(2-Ethyl-butylamino)-5-trifluoromethyl-pyrimidin-2-ylamino]-1,3-dihydro-indol-2-one; 5-{4-[(Tetrahydro-furan-2R-ylmethyl)-amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; 5-{4-[(Tetrahydro-furan-2S-ylmethyl)-amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; 5-{4-[(5-Methyl-furan-2-ylmethyl)-amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; 5-{4-[(1-Methanesulfonyl-pyrrolidin-2-ylmethyl)-amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; 5-{4-[(Adamantan-2-ylmethyl)-amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; 5-{4-[(Adamantan-2-ylmethyl)-amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; 5-[4-(2-Methoxy-2-methyl-propylamino)-5-trifluoromethyl-pyrimidin-2-ylamino]-1,3-dihydro-indol-2-one; 5-{4-[(endo-Bicyclo[2.2.1]hept-5-en-2-ylmethyl)-amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; (3-{[2-(2-Oxo-2,3-dihydro-1H-indol-5-ylamino)-5-trifluoromethyl-pyrimidin-4-ylamino]-methyl}-benzyl)-phosphonic acid dimethyl ester; 5-[4-(3-Methyl-butylamino)-5-trifluoromethyl-pyrimidin-2-ylamino]-1,3-dihydro-indol-2-one; 5-{4-[(2-Hydroxy-cyclohexylmethyl)-amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; N-(4-Methoxy-3-{[2-(2-oxo-2,3-dihydro-1H-indol-5-ylamino)-5-trifluoromethyl-pyrimidin-4-ylamino]-methyl}-phenyl)-N-methyl-methanesulfonamide; 5-{4-[(4-Ethanesulfonyl-morpholin-2-ylmethyl)-amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; 5-(4-{[4-(Propane-2-sulfonyl)-morpholin-2-ylmethyl]-amino}-5-trifluoromethyl-pyrimidin-2-ylamino)-1,3-dihydro-indol-2-one; 5-{4-[(4-Acetyl-morpholin-2-ylmethyl)-amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; 5-{4-[(4-Propionyl-morpholin-2-ylmethyl)-amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; 5-(4-{[4-(2,2-Dimethyl-propionyl)-morpholin-2-ylmethyl]-amino}-5-trifluoromethyl-pyrimidin-2-ylamino)-1,3-dihydro-indol-2-one; 2-{[2-(2-Oxo-2,3-dihydro-1H-indol-5-ylamino)-5-trifluoromethyl-pyrimidin-4-ylamino]-methyl}-morpholine-4-carboxylic acid methyl ester; 5-{4-[(4-Methoxyacetyl-morpholin-2-ylmethyl)-amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; 5-[4-(3-Ethanesulfonyl-benzylamino)-5-trifluoromethyl-pyrimidin-2-ylamino]-1,3-dihydro-indol-2-one; 5-{4-[(4-Methanesulfonyl-morpholin-2R-ylmethyl)-amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; 5-{4-[(4-Methanesulfonyl-morpholin-2S-ylmethyl)-amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; 5-{4-[(Pyrimidin-2-ylmethyl)-amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; 5-{4-[(Pyrazin-2-ylmethyl)-amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; N-(4-Fluoro-3-{[2-(2-oxo-2,3-dihydro-1H-indol-5-ylamino)-5-trifluoromethyl-pyrimidin-4-ylamino]-methyl}-phenyl)-N-methyl-methanesulfonamide; 5-{4-[(1-Methanesulfonyl-piperidin-3-ylmethyl)-amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; 5-{4-[(4-Isobutyryl-morpholin-2-ylmethyl)-amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; 5-[4-(3,3-Dimethyl-2-oxo-butylamino)-5-trifluoromethyl-pyrimidin-2-ylamino]-1,3-dihydro-indol-2-one; 5-[4-(1,2-Dimethyl-propylamino)-5-trifluoromethyl-pyrimidin-2-ylamino]-1,3-dihydro-indol-2-one; 5-[4-(2-Methoxy-1-methyl-ethylamino)-5-trifluoromethyl-pyrimidin-2-ylamino]-1,3-dihydro-indol-2-one; 5-{4-[2-(1,1-Dioxo-1D 6 -isothiazolidin-2-yl)-ethylamino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; 5-[4-(3-Methylamino-propylamino)-5-trifluoromethyl-pyrimidin-2-ylamino]-1,3-dihydro-indol-2-one; 5-{4-[(Pyridin-3-ylmethyl)-amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; 5-{4-[(6-Methanesulfonyl-pyridin-2-ylmethyl)-amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; 5-{4-[3-(1,1-Dioxo-1,I,6-isothiazolidin-2-yl)-benzylamino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; 5-[4-(1R-Phenyl-ethylamino)-5-trifluoromethyl-pyrimidin-2-ylamino]-1,3-dihydro-indol-2-one; 5-(4-Isopropylamino-5-trifluoromethyl-pyrimidin-2-ylamino)-1,3-dihydro-indol-2-one; 5-(4R -sec-Butylamino-5-trifluoromethyl-pyrimidin-2-ylamino)-1,3-dihydro-indol-2-one; 5-(4S-sec-Butylamino-5-trifluoromethyl-pyrimidin-2-ylamino)-1,3-dihydro-indol-2-one; 5-[4-(2-Methylamino-ethylamino)-5-trifluoromethyl-pyrimidin-2-ylamino]-1,3-dihydro-indol-2-one; 5-[4-(1S-Phenyl-ethylamino)-5-trifluoromethyl-pyrimidin-2-ylamino]-1,3-dihydro-indol-2-one; 5-{4-[(2-Methanesulfonylmethyl-thiazol-4-ylmethyl)-amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; 5-(4-Propylamino-5-trifluoromethyl-pyrimidin-2-ylamino)-1,3-dihydro-indol-2-one; 5-[4-(2-Hydroxy-1-methyl-ethylamino)-5-trifluoromethyl-pyrimidin-2-ylamino]-1,3-dihydro-indol-2-one; 5-[4-(1-Hydroxymethyl-propylamino)-5-trifluoromethyl-pyrimidin-2-ylamino]-1,3-dihydro-indol-2-one; 5-{4-[(5-Methanesulfonyl-pyridin-3-ylmethyl)-amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; 5-{4-[(Pyridin-4-ylmethyl)-amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; 5-[4-(1,3-Dimethyl-butylamino)-5-trifluoromethyl-pyrimidin-2-ylamino]-1,3-dihydro-indol-2-one; N-Isopropyl-N-{3-[2-(2-oxo-2,3-dihydro-1H-indol-5-ylamino)-5-trifluoromethyl-pyrimidin-4-ylamino]-propyl}-methanesulfonamide; 5-[4-(1S-Hydroxymethyl-2-methyl-propylamino)-5-trifluoromethyl-pyrimidin-2-ylamino]-1,3-dihydro-indol-2-one; N-Cyclohexyl-N-{3-[2-(2-oxo-2,3-dihydro-1H-indol-5-ylamino)-5-trifluoromethyl-pyrimidin-4-ylamino]-propyl}-methanesulfonamide; 5-[4-(1,2,3,4-Tetrahydro-naphthalen-1-ylamino)-5-trifluoromethyl-pyrimidin-2-ylamino]-1,3-dihydro-indol-2-one; 5-{4-[(1-Methanesulfonyl-pyrrolidin-2S-ylmethyl)-amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; 5-{4-[(3-Methyl-thiophen-2-ylmethyl)-amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; 5-{4-[(1-Methanesulfonyl-pyrrolidin-3R-ylmethyl)-amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; 5-[4-(2-Hydroxy-1S-phenyl-ethylamino)-5-trifluoromethyl-pyrimidin-2-ylamino]-1,3-dihydro-indol-2-one; 5-[4-(2-Hydroxy-1S-methyl-ethylamino)-5-trifluoromethyl-pyrimidin-2-ylamino]-1,3-dihydro-indol-2-one; 5-[4-(1R-Hydroxymethyl-propylamino)-5-trifluoromethyl-pyrimidin-2-ylamino]-1,3-dihydro-indol-2-one; 5-[4-(1-Pyrimidin-4-yl-ethylamino)-5-trifluoromethyl-pyrimidin-2-ylamino]-1,3-dihydro-indol-2-one; 5-[4-(1,1-Dioxo-tetrahydro-1-thiophen-3-ylamino)-5-trifluoromethyl-pyrimidin-2-ylamino]-1,3-dihydro-indol-2-one; 5-{4-[(1H-Imidazol-2-ylmethyl)-amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; 5-[4-(2-Piperidin-2-yl-ethylamino)-5-trifluoromethyl-pyrimidin-2-ylamino]-1,3-dihydro-indol-2-one; 5-[4-(Isobutyl-methyl-amino)-5-trifluoromethyl-pyrimidin-2-ylamino]-1,3-dihydro-indol-2-one; N-Methyl-N-(3-{[2-(2-oxo-2,3-dihydro-1H-indol-5-ylamino)-5-trifluoromethyl-pyrimidin-4-ylamino]-methyl}-phenyl)-methanesulfonamide; N-Ethyl-N-(3-{[2-(2-oxo-2,3-dihydro-1H-indol-5-ylamino)-5-trifluoromethyl-pyrimidin-4-ylamino]-methyl}-phenyl)-methanesulfonamide; 5-[4-(2-Methanesulfonyl-benzylamino)-5-trifluoromethyl-pyrimidin-2-ylamino]-1,3-dihydro-indol-2-one; N-Isopropyl-N-(3-{[2-(2-oxo-2,3-dihydro-1H-indol-5-ylamino)-5-trifluoromethyl-pyrimidin-4-ylamino]-methyl}-phenyl)-methanesulfonamide; 5-{4-[(3,4,5,6-Tetrahydro-2H-[1,2′]bipyridinyl-3-ylmethyl)-amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; 5-{4-[(1-Pyrimidin-2-yl-piperidin-3-ylmethyl)-amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; 5-{4-[2R-(1-Methanesulfonyl-piperidin-2-yl)-ethylamino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; 5-{4-[2S-(1-Methanesulfonyl-piperidin-2-yl)-ethylamino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; 5-[4-(3-Methylsufanyl-propylamino)-5-trifluoromethyl-pyrimidin-2-ylamino]-1,3-dihydro-indol-2-one; 5-[4-(1S-Hydroxymethyl-3-methylsulfanyl-propylamino)-5-trifluoromethyl-pyrimidin-2-ylamino]-1,3-dihydro-indol-2-one; 5-[4-(2-Hydroxy-1R-methyl-ethylamino)-5-trifluoromethyl-pyrimidin-2-ylamino]-1,3-dihydro-indol-2-one; 5-[4-(1R-Hydroxymethyl-2-methyl-propylamino)-5-trifluoromethyl-pyrimidin-2-ylamino]-1,3-dihydro-indol-2-one; N-Ethyl-N-{3-[2-(2-oxo-2,3-dihydro-1H-indol-5-ylamino)-5-trifluoromethyl-pyrimidin-4-ylamino]-propyl}-methanesulfonamide; 5-{4-[(1-Methanesulfonyl-pyrrolidin-3R-ylmethyl)-amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; 5-[4-(1S-Hydroxymethyl-propylamino)-5-trifluoromethyl-pyrimidin-2-ylamino]-1,3-dihydro-indol-2-one; 5-[4-(3,5-Dinitro-benzylamino)-5-trifluoromethyl-pyrimidin-2-ylamino]-1,3-dihydro-indol-2-one; N-(2-{[2-(2-Oxo-2,3-dihydro-1H-indol-5-ylamino)-5-trifluoromethyl-pyrimidin-4-ylamino]-methyl}-phenyl)-methanesulfonamide; N-Isopropyl-N-{2-[2-(2-oxo-2,3-dihydro-1H-indol-5-ylamino)-5-trifluoromethyl-pyrimidin-4-ylamino]-ethyl}-methanesulfonamide; 5-[4-(2-Hydroxy-1-phenyl-ethylamino)-5-trifluoromethyl-pyrimidin-2-ylamino]-1,3-dihydro-indol-2-one; 5-[4-(1R-Hydroxymethyl-3-methyl-butylamino)-5-trifluoromethyl-pyrimidin-2-ylamino]-1,3-dihydro-indol-2-one; 5-[4-(1S-Hydroxymethyl-3-methyl-butylamino)-5-trifluoromethyl-pyrimidin-2-ylamino]-1,3-dihydro-indol-2-one; 5-{4-[(1-Methanesulfonyl-piperidin-2S-ylmethyl)-amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; 5-{4-[(1-Methanesulfonyl-pyrrolidin-2R-ylmethyl)-amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; 5-[4-(Methyl-pyridin-2-ylmethyl-amino)-5-trifluoromethyl-pyrimidin-2-ylamino]-1,3-dihydro-indol-2-one; 5-{4-[(3-Methanesulfonyl-benzyl)-methyl-amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; N-Methyl-N-(2-{[2-(2-oxo-2,3-dihydro-1H-indol-5-ylamino)-5-trifluoromethyl-pyrimidin-4-ylamino]-methyl}-phenyl)-methanesulfonamide; 5-[4-(Methyl-pyridin-3-ylmethyl-amino)-5-trifluoromethyl-pyrimidin-2-ylamino]-1,3-dihydro-indol-2-one; 5-{4-[(1-Methanesulfonyl-piperidin-3-ylmethyl)-methyl-amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; 5-[4-(Methyl-pyridin-4-ylmethyl-amino)-5-trifluoromethyl-pyrimidin-2-ylamino]-1,3-dihydro-indol-2-one; 5-(4-Cyclopentylamino-5-trifluoromethyl-pyrimidin-2-ylamino)-1,3-dihydro-indol-2-one; 5-[4-(2,6-Dimethoxy-benzylamino)-5-trifluoromethyl-pyrimidin-2-ylamino]-1,3-dihydro-indol-2-one; 5-{4-[(1,5-Dimethyl-1H-pyrazol-3-ylmethyl)-amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one and 5-[4-(2-Imidazol-1-yl-ethylamino)-5-trifluoromethyl-pyrimidin-2-ylamino]-1,3-dihydro-indol-2-one.
Certain preferred embodiments of the invention are compounds selected from:
5-{4-[(1-Methanesulfonyl-piperidin-3-ylmethyl)-amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; N-Methyl-N-{2-[2-(2-oxo-2,3-dihydro-1H-indol-5-ylamino)-5-trifluoromethyl-pyrimidin-4-ylamino]-ethyl}-methanesulfonamide; N-Methyl-N-{3-[2-(2-oxo-2,3-dihydro-1H-indol-5-ylamino)-5-trifluoromethyl-pyrimidin-4-ylamino]-propyl}-methanesulfonamide; 5-{4-[2-(1-Methanesulfonyl-piperidin-2-yl)-ethylamino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; 5-{4-[(Bicyclo[2.2.1]hept-5-en-2-ylmethyl)-amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; 5-[4-(3-Methyl-butylamino)-5-trifluoromethyl-pyrimidin-2-ylamino]-1,3-dihydro-indol-2-one; 5-{4-[(1-Methanesulfonyl-piperidin-3-ylmethyl)-amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; N-Isopropyl-N-{3-[2-(2-oxo-2,3-dihydro-1H-indol-5-ylamino)-5-trifluoromethyl-pyrimidin-4-ylamino]-propyl}-methanesulfonamide; N-Cyclohexyl-N-{3-[2-(2-oxo-2,3-dihydro-1H-indol-5-ylamino)-5-trifluoromethyl-pyrimidin-4-ylamino]-propyl}-methanesulfonamide; 5-{4-[2-(1-Methanesulfonyl-piperidin-2-yl)-ethylamino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; N-Isopropyl-N-{2-[2-(2-oxo-2,3-dihydro-1H-indol-5-ylamino)-5-trifluoromethyl-pyrimidin-4-ylamino]-ethyl}-methanesulfonamide; 5-{4-[(1-Methanesulfonyl-pyrrolidin-2-ylmethyl)-amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; 5-(4-Cyclopentylamino-5-trifluoromethyl-pyrimidin-2-ylamino)-1,3-dihydro-indol-2-one; Ethanesulfonic acid methyl-{3-[2-(2-oxo-2,3-dihydro-1H-indol-5-ylamino)-5-trifluoromethyl-pyrimidin-4-ylamino]-propyl}-amide; 2,2,2-Trifluoro-N-methyl-N-{3-[2-(2-oxo-2,3-dihydro-1H-indol-5-ylamino)-5-trifluoromethyl-pyrimidin-4-ylamino]-propyl}-acetamide; N-Methyl-N-{2-[2-(2-oxo-2,3-dihydro-1H-indol-5-ylamino)-5-trifluoromethyl-pyrimidin-4-ylamino]-ethyl}-methanesulfonamide; 5-(4-Cyclobutylamino-5-trifluoromethyl-pyrimidin-2-ylamino)-1,3-dihydro-indol-2-one; 5-{4-[2-Hydroxy-2-(1-methanesulfonyl-piperidin-2-yl)-ethylamino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; 3-Oxo-3-(3-{[2-(2-oxo-2,3-dihydro-1H-indol-5-ylamino)-5-trifluoromethyl-pyrimidin-4-ylamino]-methyl}-piperidin-1-yl)-propionitrile; 5-{4-[(1-Methanesulfonyl-piperidin-4-ylmethyl)-amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; 5-{4-[(4-Methanesulfonyl-morpholin-2-ylmethyl)-amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; 5-{4-[(5-Oxo-morpholin-2-ylmethyl)-amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; 5-{4-[(1-Methanesulfonyl-pyrrolidin-3-ylmethyl)-amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; 5-[4-(3-Isopropoxy-propylamino)-5-trifluoromethyl-pyrimidin-2-ylamino]-1,3-dihydro-indol-2-one; 5-{4-[(Adamantan-2-ylmethyl)-amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; N-{2,2-Dimethyl-3-[2-(2-oxo-2,3-dihydro-1H-indol-5-ylamino)-5-trifluoromethyl-pyrimidin-4-ylamino]-propyl}-methanesulfonamide; 5-{4-[(1-Hydroxy-cyclopentylmethyl)-amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; 5-{4-[(4-Hydroxy-tetrahydro-pyran-4-ylmethyl)-amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; 5-{4-[(2-Hydroxy-cyclohexylmethyl)-amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; 5-[4-(3-Methanesulfonyl-propylamino)-5-trifluoromethyl-pyrimidin-2-ylamino]-1,3-dihydro-indol-2-one; 5-{4-[(1-Pyrimidin-2-yl-piperidin-3-ylmethyl)-amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; 3-[2-(2-Oxo-2,3-dihydro-1H-indol-5-ylamino)-5-trifluoromethyl-pyrimidin-4-ylamino]-propionic acid ethyl ester; 5-{4-[(1-Ethyl-5-oxo-pyrrolidin-3-ylmethyl)-amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; 2,N-Dimethyl-N-{2-[2-(2-oxo-2,3-dihydro-1H-indol-5-ylamino)-5-trifluoromethyl-pyrimidin-4-ylamino]-ethyl}-butyramide; 2-Methoxy-N-methyl-N-{3-[2-(2-oxo-2,3-dihydro-1H-indol-5-ylamino)-5-trifluoromethyl-pyrimidin-4-ylamino]-propyl}-acetamide; 5-{4-[2-(1-Acetyl-piperidin-2-yl)-ethylamino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; 5-{4-[(1-Methanesulfonyl-piperidin-2-ylmethyl)-amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; 5-{4-[(1-Methanesulfonyl-pyrrolidin-3-ylmethyl)-amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; 5-{4-[(1-Pyrimidin-2-yl-piperidin-3-ylmethyl)-amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; 3-{[2-(2-Oxo-2,3-dihydro-1H-indol-5-ylamino)-5-trifluoromethyl-pyrimidin-4-ylamino]-methyl}-benzenesulfonamide; N-(3-{[2-(2-Oxo-2,3-dihydro-1H-indol-5-ylamino)-5-trifluoromethyl-pyrimidin-4-ylamino]-methyl}-phenyl)-methanesulfonamide; N-(4-Methoxy-3-{[2-(2-oxo-2,3-dihydro-1H-indol-5-ylamino)-5-trifluoromethyl-pyrimidin-4-ylamino]-methyl}-phenyl)-methanesulfonamide; 5-[4-(3-Methanesulfonylmethyl-benzylamino)-5-trifluoromethyl-pyrimidin-2-ylamino]-1,3-dihydro-indol-2-one; N-Methyl-N-(4-methyl-3-{[2-(2-oxo-2,3-dihydro-1H-indol-5-ylamino)-5-trifluoromethyl-pyrimidin-4-ylamino]-methyl}-phenyl)-methanesulfonamide; 5-{4-[(4-Methanesulfonyl-pyridin-2-ylmethyl)-amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; 5-{4-[(5-Methyl-furan-2-ylmethyl)-amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; (3-{[2-(2-Oxo-2,3-dihydro-1H-indol-5-ylamino)-5-trifluoromethyl-pyrimidin-4-ylamino]-methyl}-benzyl)-phosphonic acid dimethyl ester; 5-{4-[(Pyridin-2-ylmethyl)-amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; 5-[5-Trifluoromethyl-4-(2-trifluoromethyl-benzylamino)-pyrimidin-2-ylamino]-1,3-dihydro-indol-2-one; 5-[4-(3-Ethanesulfonyl-benzylamino)-5-trifluoromethyl-pyrimidin-2-ylamino]-1,3-dihydro-indol-2-one; 5-{4-[(Pyrimidin-2-ylmethyl)-amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; 5-{4-[(Pyrazin-2-ylmethyl)-amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; N-(4-Fluoro-3-{[2-(2-oxo-2,3-dihydro-1H-indol-5-ylamino)-5-trifluoromethyl-pyrimidin-4-ylamino]-methyl}-phenyl)-N-methyl-methanesulfonamide; 5-{4-[(Pyridin-3-ylmethyl)-amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; 5-{4-[(6-Methanesulfonyl-pyridin-2-ylmethyl)-amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; 5-{4-[(2-Methanesulfonylmethyl-thiazol-4-ylmethyl)-amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; 5-{4-[(5-Methanesulfonyl-pyridin-3-ylmethyl)-amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; 5-{4-[(3-Methyl-thiophen-2-ylmethyl)-amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; 5-{4-[(1H-Imidazol-2-ylmethyl)-amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; N-Methyl-N-(3-{[2-(2-oxo-2,3-dihydro-1H-indol-5-ylamino)-5-trifluoromethyl-pyrimidin-4-ylamino]-methyl}-phenyl)-methanesulfonamide; 5-[4-(2-Methanesulfonyl-benzylamino)-5-trifluoromethyl-pyrimidin-2-ylamino]-1,3-dihydro-indol-2-one; N-(2-{[2-(2-Oxo-2,3-dihydro-1H-indol-5-ylamino)-5-trifluoromethyl-pyrimidin-4-ylamino]-methyl}-phenyl)-methanesulfonamide; N-Methyl-N-(2-{[2-(2-oxo-2,3-dihydro-1H-indol-5-ylamino)-5-trifluoromethyl-pyrimidin-4-ylamino]-methyl}-phenyl)-methanesulfonamide; 5-{4-[(1,5-Dimethyl-1H-pyrazol-3-ylmethyl)-amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; 5-[4-(2-Imidazol-1-yl-ethylamino)-5-trifluoromethyl-pyrimidin-2-ylamino]-1,3-dihydro-indol-2-one; N-(5-Methyl-2-{[2-(2-oxo-2,3-dihydro-1H-indol-5-ylamino)-5-trifluoromethyl-pyrimidin-4-ylamino]-methyl}-phenyl)-methanesulfonamide; 5-{4-[(3-Methyl-pyridin-2-ylmethyl)-amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; 5-[4-(3-Methanesulfonyl-benzylamino)-5-trifluoromethyl-pyrimidin-2-ylamino]-1,3-dihydro-indol-2-one; 5-{4-[(Isochroman-1-ylmethyl)-amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; 5-{4-[2-(Pyridin-3-yloxy)-propylamino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; 5-{4-[2-(6-Methyl-pyridin-2-yl)-ethylamino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; 5-{4-[(2,3-Dihydro-benzo[1,4]dioxin-2-ylmethyl)-amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; 5-{4-[2-(4-Methyl-1H-imidazol-2-yl)-ethylamino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; 5-{4-[2-(1H-Benzoimidazol-2-yl)-ethylamino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; 5-{4-[(5-Phenyl-4 H-[1,2,4]triazol-3-ylmethyl)-amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; 5-{4-[(3-Methyl-imidazo[2,1-b]thiazol-6-ylmethyl)-amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; N-Methyl-N-(2-methyl-6-{[2-(2-oxo-2,3-dihydro-1H-indol-5-ylamino)-5-trifluoromethyl-pyrimidin-4-ylamino]-methyl}-phenyl)-methanesulfonamide; N-(2-Methyl-6-{[2-(2-oxo-2,3-dihydro-1H-indol-5-ylamino)-5-trifluoromethyl-pyrimidin-4-ylamino]-methyl}-phenyl)-methanesulfonamide; N-(3-Methanesulfonylamino-5-{[2-(2-oxo-2,3-dihydro-1H-indol-5-ylamino)-5-trifluoromethyl-pyrimidin-4-ylamino]-methyl}-phenyl)-methanesulfonamide; and N-Methyl-N-(3-{[2-(2-oxo-2,3-dihydro-1H-indol-5-ylamino)-5-trifluoromethyl-pyrimidin-4-ylamino]-methyl}-pyridin-2-yl)-methanesulfonamide.
Preferred embodiment of the present invention are selected from
5-[4-(3-Methanesulfonyl-benzylamino)-5-trifluoromethyl-pyrimidin-2-ylamino]-1,3-dihydro-indol-2-one; Ethanesulfonic acid methyl-{3-[2-(2-oxo-2,3-dihydro-1H-indol-5-ylamino)-5-trifluoromethyl-pyrimidin-4-ylamino]-propyl}-amide; 5-{4-[(Isochroman-1-ylmethyl)-amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; 5-{4-[2-(Pyridin-3-yloxy)-propylamino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; 3-{[2-(2-Oxo-2,3-dihydro-1H-indol-5-ylamino)-5-trifluoromethyl-pyrimidin-4-ylamino]-methyl}-benzenesulfonamide; 5-{4-[(1-Methanesulfonyl-piperidin-3-ylmethyl)-amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; N-(3-{[2-(2-Oxo-2,3-dihydro-1H-indol-5-ylamino)-5-trifluoromethyl-pyrimidin-4-ylamino]-methyl}-phenyl)-methanesulfonamide; N-Methyl-N-{2-[2-(2-oxo-2,3-dihydro-1H-indol-5-ylamino)-5-trifluoromethyl-pyrimidin-4-ylamino]-ethyl}-methanesulfonamide; 5-{4-[(4-Methanesulfonyl-morpholin-2-ylmethyl)-amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; 5-[4-(3-Methanesulfonylmethyl-benzylamino)-5-trifluoromethyl-pyrimidin-2-ylamino]-1,3-dihydro-indol-2-one; 5-{4-[(1-Methanesulfonyl-pyrrolidin-3-ylmethyl)-amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; N-Methyl-N-{3-[2-(2-oxo-2,3-dihydro-1H-indol-5-ylamino)-5-trifluoromethyl-pyrimidin-4-ylamino]-propyl}-methanesulfonamide; 5-{4-[2-(1-Methanesulfonyl-piperidin-2-yl)-ethylamino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; 5-{4-[(4-Methanesulfonyl-pyridin-2-ylmethyl)-amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; 5-[4-(3-Isopropoxy-propylamino)-5-trifluoromethyl-pyrimidin-2-ylamino]-1,3-dihydro-indol-2-one; 5-{4-[(5-Methyl-furan-2-ylmethyl)-amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; 5-{4-[(Bicyclo[2.2.1]hept-5-en-2-ylmethyl)-amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; N-(4-Fluoro-3-{[2-(2-oxo-2,3-dihydro-1H-indol-5-ylamino)-5-trifluoromethyl-pyrimidin-4-ylamino]-methyl}-phenyl)-N-methyl-methanesulfonamide; 5-{4-[(1-Methanesulfonyl-piperidin-3-ylmethyl)-amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; 5-{4-[(6-Methanesulfonyl-pyridin-2-ylmethyl)-amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; 5-{4-[(5-Methanesulfonyl-pyridin-3-ylmethyl)-amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; 5-[4-(2-Methanesulfonyl-benzylamino)-5-trifluoromethyl-pyrimidin-2-ylamino]-1,3-dihydro-indol-2-one; 5-{4-[(1-Pyrimidin-2-yl-piperidin-3-ylmethyl)-amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; 5-{4-[2-(1-Methanesulfonyl-piperidin-2-yl)-ethylamino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; 5-{4-[2-(1-Methanesulfonyl-piperidin-2-yl)-ethylamino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; N-(2-{[2-(2-Oxo-2,3-dihydro-1H-indol-5-ylamino)-5-trifluoromethyl-pyrimidin-4-ylamino]-methyl}-phenyl)-methanesulfonamide; 5-{4-[(1-Methanesulfonyl-pyrrolidin-2-ylmethyl)-amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; N-Methyl-N-(2-{[2-(2-oxo-2,3-dihydro-1H-indol-5-ylamino)-5-trifluoromethyl-pyrimidin-4-ylamino]-methyl}-phenyl)-methanesulfonamide; N-Methyl-N-(2-methyl-6-{[2-(2-oxo-2,3-dihydro-1H-indol-5-ylamino)-5-trifluoromethyl-pyrimidin-4-ylamino]-methyl}-phenyl)-methanesulfonamide; 5-[4-(2-Hydroxy-indan-1-ylamino)-5-trifluoromethyl-pyrimidin-2-ylamino]-1,3-dihydro-indol-2-one; 5-{4-[(1-Hydroxy-cyclopentylmethyl)-amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; 5-{4-[2-Hydroxy-2-(1-methanesulfonyl-piperidin-2-yl)-ethylamino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-one; and N-Methyl-N-(3-{[2-(2-oxo-2,3-dihydro-1H-indol-5-ylamino)-5-trifluoromethyl-pyrimidin-4-ylamino]-methyl}-pyridin-2-yl)-methanesulfonamide.
This invention also relates to a method for the treatment of abnormal cell growth in a mammal, including a human, comprising administering to said mammal an amount of a compound of the formula 1, as defined above, or a pharmaceutically acceptable salt, solvate or prodrug thereof, that is effective in treating abnormal cell growth. In one embodiment of this method, the abnormal cell growth is cancer, including, but not limited to, lung cancer, bone cancer, pancreatic cancer, skin cancer, cancer of the head or neck, cutaneous or intraocular melanoma, uterine cancer, ovarian cancer, rectal cancer, cancer of the anal region, stomach cancer, colon cancer, breast cancer, uterine cancer, carcinoma of the fallopian tubes, carcinoma of the endometrium, carcinoma of the cervix, carcinoma of the vagina, carcinoma of the vulva, Hodgkin's Disease, cancer of the esophagus, cancer of the small intestine, cancer of the endocrine system, cancer of the thyroid gland, cancer of the parathyroid gland, cancer of the adrenal gland, sarcoma of soft tissue, cancer of the urethra, cancer of the penis, prostate cancer, chronic or acute leukemia, lymphocytic lymphomas, cancer of the bladder, cancer of the kidney or ureter, renal cell carcinoma, carcinoma of the renal pelvis, neoplasms of the central nervous system (CNS), primary CNS lymphoma, spinal axis tumors, brain stem glioma, pituitary adenoma, or a combination of one or more of the foregoing cancers. In one embodiment the method comprises comprising administering to a mammal an amount of a compound of formula 1 that is effective in treating said cancer solid tumor. In one preferred embodiment the solid tumor is breast, lung, colon, brain, prostate, stomach, pancreatic, ovarian, skin (melanoma), endocrine, uterine, testicular, and bladder cancer.
In another embodiment of said method, said abnormal cell growth is a benign proliferative disease, including, but not limited to, psoriasis, benign prostatic hypertrophy or restinosis.
This invention also relates to a method for the treatment of abnormal cell growth in a mammal which comprises administering to said mammal an amount of a compound of formula 1, or a pharmaceutically acceptable salt, solvate or prodrug thereof, that is effective in treating abnormal cell growth in combination with an anti-tumor agent selected from the group consisting of mitotic inhibitors, alkylating agents, anti-metabolites, intercalating antibiotics, growth factor inhibitors, cell cycle inhibitors, enzymes, topoisomerase inhibitors, biological response modifiers, antibodies, cytotoxics, anti-hormones, and anti-androgens.
This invention also relates to a pharmaceutical composition for the treatment of abnormal cell growth in a mammal, including a human, comprising an amount of a compound of the formula 1, as defined above, or a pharmaceutically acceptable salt, solvate or prodrug thereof, that is effective in treating abnormal cell growth, and a pharmaceutically acceptable carrier. In one embodiment of said composition, said abnormal cell growth is cancer, including, but not limited to, lung cancer, bone cancer, pancreatic cancer, skin cancer, cancer of the head or neck, cutaneous or intraocular melanoma, uterine cancer, ovarian cancer, rectal cancer, cancer of the anal region, stomach cancer, colon cancer, breast cancer, uterine cancer, carcinoma of the fallopian tubes, carcinoma of the endometrium, carcinoma of the cervix, carcinoma of the vagina, carcinoma of the vulva, Hodgkin's Disease, cancer of the esophagus, cancer of the small intestine, cancer of the endocrine system, cancer of the thyroid gland, cancer of the parathyroid gland, cancer of the adrenal gland, sarcoma of soft tissue, cancer of the urethra, cancer of the penis, prostate cancer, chronic or acute leukemia, lymphocytic lymphomas, cancer of the bladder, cancer of the kidney or ureter, renal cell carcinoma, carcinoma of the renal pelvis, neoplasms of the central nervous system (CNS), primary CNS lymphoma, spinal axis tumors, brain stem glioma, pituitary adenoma, or a combination of one or more of the foregoing cancers. In another embodiment of said pharmaceutical composition, said abnormal cell growth is a benign proliferative disease, including, but not limited to, psoriasis, benign prostatic hypertrophy or restinosis.
The invention also relates to a pharmaceutical composition for the treatment of abnormal cell growth in a mammal, including a human, which comprises an amount of a compound of formula 1, as defined above, or a pharmaceutically acceptable salt, solvate or prodrug thereof, that is effective in treating abnormal cell growth in combination with a pharmaceutically acceptable carrier and an anti-tumor agent selected from the group consisting of mitotic inhibitors, alkylating agents, anti-metabolites, intercalating antibiotics, growth factor inhibitors, cell cycle inhibitors, enzymes, topoisomerase inhibitors, biological response modifiers, anti-hormones, and anti-androgens.
This invention also relates to a method for the treatment of a disorder associated with angiogenesis in a mammal, including a human, comprising administering to said mammal an amount of a compound of the formula 1, as defined above, or a pharmaceutically acceptable salt, solvate or prodrug thereof, that is effective in treating said disorder. Such disorders include cancerous tumors such as melanoma; ocular disorders such as age-related macular degeneration, presumed ocular histoplasmosis syndrome, and retinal neovascularization from proliferative diabetic retinopathy; rheumatoid arthritis; bone loss disorders such as osteoporosis, particularly, post-menopausal osteoporosis, Paget's disease, humoral hypercalcemia of malignancy, hypercalcemia from tumors metastatic to bone, and osteoporosis induced by glucocorticoid treatment; coronary restenosis; and certain microbial infections including those associated with microbial pathogens selected from adenovirus, hantaviruses, Borrelia burgdorferi, Yersinia spp., Bordetella pertussis , and group A Streptococcus.
This invention also relates to a method of (and to a pharmaceutical composition for) treating abnormal cell growth in a mammal which comprise an amount of a compound of formula 1, or a pharmaceutically acceptable salt, solvate or prodrug thereof, and an amount of one or more substances selected from anti-angiogenesis agents, signal transduction inhibitors, and antiproliferative agents, which amounts are together effective in treating said abnormal cell growth.
Anti-angiogenesis agents, such as MMP-2 (matrix-metalloprotienase 2) inhibitors, MMP-9 (matrix-metalloprotienase 9) inhibitors, and COX-II (cyclooxygenase II) inhibitors, can be used in conjunction with a compound of formula 1 in the methods and pharmaceutical compositions described herein. Examples of useful COX-II inhibitors include CELEBREX™ (alecoxib), valdecoxib, and rofecoxib. Examples of useful matrix metalloproteinase inhibitors are described in WO 96/33172 (published Oct. 24, 1996), WO 96/27583 (published Mar. 7, 1996), European Patent Application No. 97304971.1 (filed Jul. 8, 1997), European Patent Application No. 99308617.2 (filed Oct. 29, 1999), WO 98/07697 (published Feb. 26, 1998), WO 98/03516 (published Jan. 29, 1998), WO 98/34918 (published Aug. 13, 1998), WO 98/34915 (published Aug. 13, 1998), WO 98/33768 (published Aug. 6, 1998), WO 98/30566 (published Jul. 16, 1998), European Patent Publication 606,046 (published Jul. 13, 1994), European Patent Publication 931,788 (published Jul. 28, 1999), WO 90/05719 (published May 331, 1990), WO 99/52910 (published Oct. 21, 1999), WO 99/52889 (published Oct. 21, 1999), WO 99/29667 (published Jun. 17, 1999), PCT International Application No. PCT/IB98/01113 (filed Jul. 21, 1998), European Patent Application No. 99302232.1 (filed Mar. 25, 1999), Great Britain patent application number 9912961.1 (filed Jun. 3, 1999), U.S. Provisional Application No. 60/148,464 (filed Aug. 12, 1999), U.S. Pat. No. 5,863,949 (issued Jan. 26, 1999), U.S. Pat. No. 5,861,510 (issued Jan. 19, 1999), and European Patent Publication 780,386 (published Jun. 25, 1997), all of which are herein incorporated by reference in their entirety. Preferred MMP-2 and MMP-9 inhibitors are those that have little or no activity inhibiting MMP-1. More preferred, are those that selectively inhibit MMP-2 and/or MMP-9 relative to the other matrix-metalloproteinases (i.e. MMP-1, MMP-3, MMP-4, MMP-5, MMP-6, MMP-7, MMP-8, MMP-10, MMP-11, MMP-12, and MMP-13).
Some specific examples of MMP inhibitors useful in combination with the compounds of the present invention are AG-3340, RO 32-3555, RS 13-0830, and the compounds recited in the following list:
3-[[4-(4-fluoro-phenoxy)-benzenesulfonyl]-(1-hydroxycarbamoyl-cyclopentyl)-amino]-propionic acid; 3-exo-3-[4-(4-fluoro-phenoxy)-benzenesulfonylamino]-8-oxa-bicyclo[3.2.1]octane-3-carboxylic acid hydroxyamide; (2R,3R)1-[4-(2-chloro-4-fluoro-benzyloxy)-benzenesulfonyl]-3-hydroxy-3-methyl-piperidine-2-carboxylic acid hydroxyamide; 4-[4-(4-fluoro-phenoxy)-benzenesulfonylamino]-tetrahydro-pyran-4-carboxylic acid hydroxyamide; 3-[[4-(4-fluoro-phenoxy)-benzenesulfonyl]-(1-hydroxycarbamoyl-cyclobutyl)-amino]-propionic acid; 4-[4-(4-chloro-phenoxy)-benzenesulfonylamino]-tetrahydro-pyran-4-carboxylic acid hydroxyamide; 3-[4-(4-chloro-phenoxy)-benzenesulfonylamino]-tetrahydro-pyran-3-carboxylic acid hydroxyamide; (2R,3R)1-[4-(4-fluoro-2-methyl-benzyloxy)-benzenesulfonyl]-3-hydroxy-3-methyl-piperidine-2-carboxylic acid hydroxyamide; 3-[[4-(4-fluoro-phenoxy)-benzenesulfonyl]-(1-hydroxycarbamoyl-1-methyl-ethyl)-amino]-propionic acid; 3-[[4-(4-fluoro-phenoxy)-benzenesulfonyl]-(4-hydroxycarbamoyl-tetrahydro-pyran-4-yl)-amino]-propionic acid; 3-exo-3-[4-(4-chloro-phenoxy)-benzenesulfonylamino]-8-oxa-bicyclo[3.2.1]octane-3-carboxylic acid hydroxyamide; 3-endo-3-[4-(4-fluoro-phenoxy)-benzenesulfonylamino]-8-oxa-bicyclo[3.2.1]octane-3-carboxylic acid hydroxyamide; and 3-[4-(4-fluoro-phenoxy)-benzenesulfonylamino]-tetrahydro-furan-3-carboxylic acid hydroxyamide;
and pharmaceutically acceptable salts, solvates and prodrugs of said compounds.
The compounds of formula 1, and the pharmaceutically acceptable salts, solvates and prodrugs thereof, can also be used in combination with signal transduction inhibitors, such as agents that can inhibit EGFR (epidermal growth factor receptor) responses, such as EGFR antibodies, EGF antibodies, and molecules that are EGFR inhibitors; VEGF (vascular endothelial growth factor) inhibitors; and erbB2 receptor inhibitors, such as organic molecules or antibodies that bind to the erbB2 receptor, for example, HERCEPTIN™ (Genentech, Inc. of South San Francisco, Calif., USA).
EGFR inhibitors are described in, for example in WO 95/19970 (published Jul. 27, 1995), WO 98/14451 (published Apr. 9, 1998), WO 98/02434 (published Jan. 22, 1998), and U.S. Pat. No. 5,747,498 (issued May 5, 1998). EGFR-inhibiting agents include, but are not limited to, CI-1033 (Pfizer Inc.), the monoclonal antibodies C225 and anti-EGFR 22Mab (ImClone Systems Incorporated of New York, N.Y., USA), the compounds ZD-1839 (AstraZeneca), BIBX-1382 (Boehringer Ingelheim), MDX-447 (Medarex Inc. of Annandale, N.J., USA), and OLX-103 (Merck & Co. of Whitehouse Station, N.J., USA), VRCTC-310 (Ventech Research) and EGF fusion toxin (Seragen Inc. of Hopkinton, Mass.).
VEGF inhibitors, for example CP-547,632 and AG-13736 (Pfizer, Inc.), SU-5416 and SU-6668 (Sugen Inc. of South San Francisco, Calif., USA), can also be combined with a compound of formula 1. VEGF inhibitors are described in, for example in WO 99/24440 (published May 20, 1999), PCT International Application PCT/IB99/00797 (filed May 3, 1999), in WO 95/21613 (published Aug. 17, 1995), WO 99/61422 (published Dec. 2, 1999), U.S. Pat. No. 5,834,504 (issued Nov. 10, 1998), WO 98/50356 (published Nov. 12, 1998), U.S. Pat. No. 5,883,113 (issued Mar. 16, 1999), U.S. Pat. No. 5,886,020 (issued Mar. 23, 1999), U.S. Pat. No. 5,792,783 (issued Aug. 11, 1998), WO 99/10349 (published Mar. 4, 1999), WO 97/32856 (published Sep. 12, 1997), WO 97/22596 (published Jun. 26, 1997), WO 98/54093 (published Dec. 3, 1998), WO 98/02438 (published Jan. 22, 1998), WO 99/16755 (published Apr. 8, 1999), and WO 98/02437 (published Jan. 22, 1998), all of which are herein incorporated by reference in their entirety. Other examples of some specific VEGF inhibitors are IM862 (Cytran Inc. of Kirkland, Wash., USA); anti-VEGF monoclonal antibody of Genentech, Inc. of South San Francisco, Calif.; and angiozyme, a synthetic ribozyme from Ribozyme (Boulder, Colo.) and Chiron (Emeryville, Calif.).
ErbB2 receptor inhibitors, such as CP-724,714 (Pfizer, Inc.), GW-282974 (Glaxo Wellcome plc), and the monoclonal antibodies AR-209 (Aronex Pharmaceuticals Inc. of The Woodlands, Tex., USA) and 2B-1 (Chiron), may be administered in combination with a compound of formula 1. Such erbB2 inhibitors include those described in WO 98/02434 (published Jan. 22, 1998), WO 99/35146 (published Jul. 15, 1999), WO 99/35132 (published Jul. 15, 1999), WO 98/02437 (published Jan. 22, 1998), WO 97/13760 (published Apr. 17, 1997), WO 95/19970 (published Jul. 27, 1995), U.S. Pat. No. 5,587,458 (issued Dec. 24, 1996), and U.S. Pat. No. 5,877,305 (issued Mar. 2, 1999), each of which is herein incorporated by reference in its entirety. ErbB2 receptor inhibitors useful in the present invention are also described in U.S. Provisional Application No. 60/117,341, filed Jan. 27, 1999, and in U.S. Provisional Application No. 60/117,346, filed Jan. 27, 1999, both of which are herein incorporated by reference in their entirety.
Other antiproliferative agents that may be used with the compounds of the present invention include inhibitors of HDI (CI-994, Pfizer Inc.), MEK (CI-1040, Pfizer Inc.), the enzyme farnesyl protein transferase and the receptor tyrosine kinase PDGFr, including the compounds disclosed and claimed in the following U.S. patent application Ser. Nos. 09/221,946 (filed Dec. 28, 1998); Ser. No. 09/454,058 (filed Dec. 2, 1999); Ser. No. 09/501,163 (filed Feb. 9, 2000); Ser. No. 09/539,930 (filed Mar. 31, 2000); Ser. No. 09/202,796 (filed May 22, 1997); Ser. No. 09/384,339 (filed Aug. 26, 1999); and Ser. No. 09/383,755 (filed Aug. 26, 1999); and the compounds disclosed and claimed in the following U.S. provisional patent applications 60/168,207 (filed Nov. 30, 1999); 60/170,119 (filed Dec. 10, 1999); 60/177,718 (filed Jan. 21, 2000); 60/168,217 (filed Nov. 30, 1999), and 60/200,834 (filed May 1, 2000). The compounds of the invention may also be used in combination with inhibitors of topoisomerase I, e.g., irinotecan (Camptosar®) and edotecarin. Each of the foregoing patent applications and provisional patent applications is herein incorporated by reference in their entirety.
A compound of formula 1 may also be used with other agents useful in treating abnormal cell growth or cancer, including, but not limited to, agents capable of enhancing antitumor immune responses, such as CTLA4 (cytotoxic lymphocite antigen 4) antibodies, and other agents capable of blocking CTLA4; and anti-proliferative agents such as other farnesyl protein transferase inhibitors, for example the farnesyl protein transferase inhibitors described in the references cited in the “Background” section, supra. Specific CTLA4 antibodies that can be used in the present invention include those described in U.S. Provisional Application 60/113,647 (filed Dec. 23, 1998) which is herein incorporated by reference in its entirety.
“Abnormal cell growth”, as used herein, unless otherwise indicated, refers to cell growth that is independent of normal regulatory mechanisms (e.g., loss of contact inhibition). This includes the abnormal growth of: (1) tumor cells (tumors) that proliferate by expressing a mutated tyrosine kinase or overexpression of a receptor tyrosine kinase; (2) benign and malignant cells of other proliferative diseases in which aberrant tyrosine kinase activation occurs; (4) any tumors that proliferate by receptor tyrosine kinases; (5) any tumors that proliferate by aberrant serine/threonine kinase activation; and (6) benign and malignant cells of other proliferative diseases in which aberrant serine/threonine kinase activation occurs.
The compounds of the present invention are potent inhibitors of the FAK protein tyrosine kinases, and thus are all adapted to therapeutic use as antiproliferative agents (e.g., anticancer), antitumor (e.g., effective against solid tumors), antiangiogenesis (e.g., stop or prevent proliferationation of blood vessels) in mammals, particularly in humans. In particular, the compounds of the present invention are useful in the prevention and treatment of a variety of human hyperproliferative disorders such as malignant and benign tumors of the liver, kidney, bladder, breast, gastric, ovarian, colorectal, prostate, pancreatic, lung, vulval, thyroid, hepatic carcinomas, sarcomas, glioblastomas, head and neck, and other hyperplastic conditions such as benign hyperplasia of the skin (e.g., psoriasis) and benign hyperplasia of the prostate (e.g., BPH). It is, in addition, expected that a compound of the present invention may possess activity against a range of leukemias and lymphoid malignancies.
In one preferred embodiment of the present invention cancer is selected from lung cancer, bone cancer, pancreatic cancer, gastric, skin cancer, cancer of the head or neck, cutaneous or intraocular melanoma, uterine cancer, ovarian cancer, gynecological, rectal cancer, cancer of the anal region, stomach cancer, colon cancer, breast cancer, uterine cancer, carcinoma of the fallopian tubes, carcinoma of the endometrium, carcinoma of the cervix, carcinoma of the vagina, carcinoma of the vulva, Hodgkin's Disease, cancer of the esophagus, cancer of the small intestine, cancer of the endocrine system, cancer of the thyroid gland, cancer of the parathyroid gland, cancer of the adrenal gland, sarcoma of soft tissue, cancer of the urethra, cancer of the penis, squamous cell, prostate cancer, chronic or acute leukemia, lymphocytic lymphomas, cancer of the bladder, cancer of the kidney or ureter, renal cell carcinoma, carcinoma of the renal pelvis, neoplasms of the central nervous system (CNS), primary CNS lymphoma, spinal axis tumors, brain, pituitary adenoma, or a combination of one or more of the foregoing cancers.
In a more preferred embodiment cancer is selected a solid tumor, such as, but not limited to, breast, lung, colon, brain, prostate, stomach, pancreatic, ovarian, skin (melanoma), endocrine, uterine, testicular, and bladder.
The compounds of the present invention may also be useful in the treatment of additional disorders in which aberrant expression ligand/receptor interactions or activation or signalling events related to various protein tyrosine kinases, are involved. Such disorders may include those of neuronal, glial, astrocytal, hypothalamic, and other glandular, macrophagal, epithelial, stromal, and blastocoelic nature in which aberrant function, expression, activation or signalling of the erbB tyrosine kinases are involved. In addition, the compounds of the present invention may have therapeutic utility in inflammatory, angiogenic and immunologic disorders involving both identified and as yet unidentified tyrosine kinases that are inhibited by the compounds of the present invention.
The term “treating”, as used herein, unless otherwise indicated, means reversing, alleviating, inhibiting the progress of, or preventing the disorder or condition to which such term applies, or one or more symptoms of such disorder or condition. The term “treatment”, as used herein, unless otherwise indicated, refers to the act of treating as “treating” is defined immediately above.
The present invention also provides a pharmaceutical composition comprising a compound of formula (I), or a pharmaceutically acceptable salt or solvate thereof, as hereinbefore defined in association with a pharmaceutically acceptable adjuvant, diluent or carrier.
The invention further provides a process for the preparation of a pharmaceutical composition of the invention which comprises mixing a compound of formula (I), or a pharmaceutically acceptable salt or solvate thereof, as hereinbefore defined with a pharmaceutically acceptable adjuvant, diluent or carrier.
For the above-mentioned therapeutic uses the dosage administered will, of course, vary with the compound employed, the mode of administration, the treatment desired and the disorder indicated. The daily dosage of the compound of formula (I)/salt/solvate (active ingredient) may be in the range from 1 mg to 1 gram, preferably 1 mg to 250 mg, more preferably 10 mg to 100 mg.
The present invention also encompasses sustained release compositions.
DETAILED DESCRIPTION OF THE INVENTION
The compounds of formula 1 can be prepared using the synthetic route outlined in Scheme 1. The substituents in Scheme 1 have the same meaning as the substituents defined for formula 1.
Compounds of formula 1 can be prepared starting from the 5-amino-oxindole (2) and pyrimidine (3). Combining 3 with an equimolar amount of a Lewis Acid at temperatures ranging from −15 to 45° C. for a time period of 10-60 minutes in an inert solvent (or solvent mixture) followed by addition of 2 and a suitable base provides after the period of 1-24 h the intermediate 4-chloropyrimidine (4) in high yields. Examples of inert solvents include but are not limited to THF, 1,4-dioxane, n-BuOH, i-PrOH, dichloromethane and 1,2-dichloroethane. Examples of suitable bases employed may include but are not limited to (i) non-nucleophilic organic bases for example triethylamine or diisopropylethylamine (ii) inorganic bases such as potassium carbonate or cesium carbonate or (iii) resin bound bases such as MP-carbonate.
Examples of Lewis Acids include but are not limited to halide salts of magnesium, copper, zinc, tin or titanium. In the next reaction, intermediate 4 is reacted with an amine of the formula 5 either neat or in the presence of an inert solvent (or solvent mixture) at temperatures ranging from 0 to 150° C. to provide the compounds of formula 1. Optionally this reaction can be run in the presence of a suitable base. Examples of suitable solvents for this reaction include but are not limited to THF, 1,4-dioxane, DMF, N-methyl-pyrrolidinone, EtOH, n-BuOH, i-PrOH, dichloromethane, 1,2-dichloroethane, DMSO or acetonitrile. Suitable bases are as outlined above.
Compounds of the present invention may be synthetically transformed into other compounds of the invention by techniques known to those skilled in the art. Simply for illustrative purposes and without limitation, such methods include:
a) removal of a protecting group by methods outlined in T. W. Greene and P. G. M. Wuts, “Protective Groups in Organic Synthesis”, Second Edition, John Wiley and Sons, New York, 1991; e.g., emoval of a BOC protecting group with an acid source such as HCl or trifluoroacetic acid.
b) displacement of a leaving group (halide, mesylate, tosylate, etc) with functional groups such as but not limited to a primary or secondary amine, thiol or alcohol to form a secondary or tertiary amine, thioether or ether, respectively.
c) treatment of phenyl (or substituted phenyl) carbamates with primary of secondary amines to form the corresponding ureas as in Thavonekham, B et. al. Synthesis (1997), 10, p 1189;
d) reduction of propargyl or homopropargyl alcohols or N-BOC protected primary amines to the corresponding E-allylic or E-homoallylic derivatives by treatment with sodium bis(2-methoxyethoxy)aluminum hydride (Red-Al) as in Denmark, S. E.; Jones, T. K. J. Org. Chem. (1982) 47, 4595-4597 or van Benthem, R. A. T. M.; Michels, J. J.; Speckamp, W. N. Synlett (1994), 368-370;
e) reduction of alkynes to the corresponding Z-alkene derivatives by treatment hydrogen gas and a Pd catalyst as in Tomassy, B. et. al. Synth. Commun. (1998), 28, p 1201
f) treatment of primary and secondary amines with an isocyanate, acid chloride (or other activated carboxylic acid derivative), alkyl/aryl chloroformate or sulfonyl chloride to provide the corresponding urea, amide, carbamate or sulfonamide;
g) reductive amination of a primary or secondary amine using an aldehyde or ketone and an appropriate reducing reagent.
h) treatment of alcohols with an isocyanate, acid chloride (or other activated carboxylic acid derivative), alkyl/aryl chloroformate or sulfonyl chloride to provide the corresponding carbamate, ester, carbonate or sulfonic acid ester.
Amines of the formula 5 may be purchased and used directly or alternatively be prepared by one skilled in the art using ordinary chemical transformations. For example; arylalkylamines or heteroarylalkylamines may be prepared from the corresponding nitrile by catalytic hydrogenation using catalysts such as Pd/C or Raney Nickel or by lithium aluminum hydride reduction, (see Rylander, Catalytic Hydrogenation in Organic Synthesis, Academic Press, 1979).
The nitrile starting materials can be either purchased or prepared from the corresponding aryl/heteroaryl bromide, iodide or triflate and Zn(CN)2 using Pd coupling conditions found in Tschaen, D. M., et. al Synthetic Communications (1994), 24, 6, pp 887-890.
Alternatively, benzylamines or heteroarylmethylamines can be prepared by reacting the appropriate arylalkyl or heteroarylalkyl halide and the potassium salt of (BOC) 2 NH (reference) and subsequent removal of the BOC groups with acid.
Amines, protected forms of amines, precursors to amines and precursors to the protected forms of amines of formula 5 can be prepared by combining the appropriate alkyne, or alkenyl stannane, alkenyl borane, alkenyl boronic acid, boronic ester with the appropriate aryl or heteroaryl bromide, iodide or triflate using Pd coupling conditions as found in Tsuji, J.; Palladium Reagents and Catalysis, John Wiley and Sons 1999 and references cited therein.
Appropriately protected amines of formula 5 may be converted to different amines of formula 5 according to methods familiar to those skilled in the art for example as but limited to:
(a) oxidation of a thioether to a sulfoxide or sulfone.
(b) N-alkylation of a sulfanilide can be achieved under phase transfer using conditions described by Brehme, R. “Synthesis”, (1976), pp 113-114.
As understood by those skilled in the art, the chemical transformation to convert an aryl halide or triflate or heteroaryl halide or triflate to an aromatic or heteroaromatic amine may be carried out using conditions currently outlined in the literature, see Hartwig, J. F.: “Angew. Chem. Int. Ed.” (1998), 37, pp. 2046-2067, Wolfe, J. P.; Wagaw, S.; Marcoux, J. F.; Buchwald, S. L.; “Acc. Chem. Res.”, (1998), 31, pp 805-818, Wolfe, J. P.; Buchwald, S. L.; “J. Org. Chem.”, (2000), 65, pp 1144-1157, Muci, A. R.; Buchwald, S. L.; “Topics in Current Chemistry” (2002), pp 131-209 and references cited therein. Further, as understood by those skilled in the art, these same aryl or heteroaryl amination chemical transformations may alternatively be carried out on nitrile (or primary amide) precursors which provide amines of the formula 5 after nitrile (or amide) reduction. Protected amines of formula 5 may be further converted to different amines of formula 5 according to methods familiar to those skilled in the art.
The in vitro activity of the compounds of formula 1 may be determined by the following procedure. More particularly, the following assay provides a method to determine whether compounds of the formula 1 inhibit the tyrosine kinase activity of the catalytic construct FAK(410-689). The assay is an ELISA-based format, measuring the inhibition of poly-glu-tyr phosphorylation by FAK(410-689).
The assay protocol has three parts:
I. Purification and cleavage of His-FAK(410-689)
II. FAK410-689 (a.k.a. FAKcd) Activation
III. FAKcd Kinase ELISA
Materials:
Ni-NTA agarose (Qiagen)
XK-16 column (Amersham-Pharmacia)
300 mM Imidizole
Superdex 200 HiLoad 16/60 prep grade column (Amersham Biotech.)
Antibody: Anti-Phosphotyrosine HRP-Conjugated Py20 (Transduction labs).
FAKcd: Purified and activated in house
TMB Microwell Peroxidase Substrate (Oncogene Research Products #CL07)
BSA: Sigma #A3294
Tween-20: Sigma #P1379
DMSO: Sigma #D-5879
D-PBS: Gibco #14190-037.
Reagents for Purification:
Buffer A: 50mM HEPES pH 7.0,
500 mM NaCl,
0.1 mM TCEP
CompleteTM protease inhibitor cocktail tablets (Roche)
Buffer B: 25 mM HEPES pH 7.0,
400mM NaCl
0.1 mM TCEP.
Buffer C: 10 mM HEPES pH 7.5,
200 mM Ammonium Sulfate
0.1 mM TCEP.
Reagents for Activation
FAK(410-689): 3 tubes of frozen aliquots at 150 ul/tube for a total of 450 ul at 1.48 mg/ml (660 ug)
His-Src(249-524): ˜0.74 mg/ml stock in 10 mM HEPES, 200 mM (NH4)2SO4
Src reaction buffer (Upstate Biotech):
100 mM Tris-HCl pH7.2, 125 mM MgCl2, 25 mM MnCl2, 2 mM EDTA, 250 uM Na3VO4, 2 mM DTT
Mn2+/ATP cocktail (Upstate Biotech)
75 mM MnCl2 500 uM ATP 20 mM MOPS pH 7.2 1 mM Na3VO4 25 mM □-glycerol phosphate 5 mM EGTA 1 mM DTT
ATP: 150 mM stock
MgCl 2 : 1 M Stock
DTT: 1M stock
Reagents for FAKcd Kinase ELISA
Phosphorylation Buffer:
50 mM HEPES, pH 7.5, 125 mM NaCl, 48 mM MgCl2
Wash Buffer: TBS+0.1% Tween-20.
Blocking Buffer:
Tris Buffer Saline, 3% BSA, 0.05% Tween-20, filtered.
Plate Coating Buffer:
50 mg/ml Poly-Glu-Tyr (Sigma #P0275) in Phosphate buffer Saline (DPBS).
ATP: 0.1M ATP in H2O or HEPES, pH7.
Note: ATP Assay Buffer: Make up as 75 uM ATP in PBS, so that 80 ul in 120 ul reaction volume=50 uM final ATP concentration.
I. Purification of His-FAKcd(410-689)
1. Resuspend 130 g baculovirus cell paste containing the over expressed His-FAKcd410-689 recombinant protein in 3 volumes (400 ml) of Buffer A,
2. Lyse cells with one pass on a microfluidizer
3. Remove cell debris by centrifugation at 40 C for 35 minutes at 14,000 rpm in a Sorval SLA-1500 rotor.
4. Transfer the supernatant to a clean tube and add 6.0 ml of Ni-NTA agarose (Qiagen)
5. Incubate the suspension with gentle rocking at 40 C for 1 hour
6. Centrifuge suspension at 700×g in a swinging bucket rotor.
7. Discard the supernatant and resuspend the agarose beads in 20.0 ml of Buffer A
8. Transfer the beads to an XK-16 column (Amersham-Pharmacia) connected to a FPLCTM.
9. Wash the agarose-beads with 5 column volumes of Buffer A and elute off the column with a step gradient of Buffer A containing 300 mM Imidizole.
10. Perform a buffer exchange of the eluted fractions into Buffer B
11. Following buffer exchange, pool the fractions and add thrombin at a 1:300 (w/w) ratio and incubated overnight at 13° C. to remove the N-terminal His-tag (His-FAK410-698 →FAK410-689 (a.k.a. FAKcd)).
12. Add the reaction mixture back onto the Ni-NTA column equilibrated with Buffer A and collect the flow-through.
13. Concentrate the flow-through down to 1.7 ml and load directly onto a Superdex 200 HiLoad 16/60 prep grade column equilibrated with Buffer C. The desired protein elutes between 85-95 ml.
14. Aliquot the FAKcd protein and store frozen at −80° C.
II. FAK Activation
1. To 450 ul of FAK(410-689) at 1.48 mg/ml (660 ug) add the following:
30 ul of 0.037 mg/ml (1 uM) His-Src(249-524) 30 ul of 7.5 mM ATP 12 ul of 20 mM MgCl2 10 ul Mn2+/ATP cocktail (UpState Biotech.) 4 ul of 6.7 mM DTT 60 ul Src Reaction Buffer (UpState Biotech.)
2. Incubate Reaction for at least 3 hours at room temperature
At time t 0 , almost all of the FAK(410-689) is singly phosphorylated. The second phosphorylation is slow. At t 120 (t=120 minutes), add 10 ul of 150 mM ATP.
T 0 =(Start) 90% singly phosphorylated FAK(410-689) (1 PO4)
T 43 =(43 min) 65% singly phosphorylated (1 PO4), 35% doubly phosphorylated (2 PO4)
T 90 =(90 min) 45% 1 PO4, 55% 2 PO4
T 150 =15% 1 PO4, 85% 2 PO4
T 210 =<10% 1 PO4, >90% 2 PO4 desalted sample
3. Add 180 ul aliquots of the desalted material to NiNTA spin column and incubate on spin column
4. Spin at 10k rpm (microfuge), for 5 min to isolate and collect flow through (Activated FAK(410-689)) and remove His-Src (captured on column)
III. FAKcd Kinase ELISA
1. Coat 96-well Nunc MaxiSorp plates with poly-glu-tyr (pGT) at 10 ug/well: Prepare 10 ug/ml of pGT in PBS and aliquot 100 ul/well. Incubate the plates at 37° C. overnight, aspirate the supernatant, wash the plates 3 times with Wash Buffer, and flick to dry before storing at 4° C.
2. Prepare compound stock solutions of 2.5 mM in 100% DMSO. The stocks are subsequently diluted to 60× of the final concentration in 100% DMSO, and diluted 1:5 in Kinase Phosphorylation Buffer.
3. Prepare a 75 uM working ATP solution in Kinase phosphorylation buffer. Add 80 ul to each well for a final ATP concentration of 50 uM.
4. Transfer 10 ul of the diluted compounds (0.5 log serial dilutions) to each well of the pGT assay plate, running each compound in triplicates on the same plate.
5. Dilute on ice, FAKcd protein to 1:1000 in Kinase Phosphorylation Buffer. Dispense 30 ul per well.
6. Note: Linearity and the appropriate dilution must be pre-determined for each batch of protein. The enzyme concentration selected should be such that quantitation of the assay signal will be approximately 0.8-1.0 at OD450, and in the linear range of the reaction rate.
7. Prepare both a No ATP control (noise) and a No Compound Control (Signal):
8. (Noise) One blank row of wells receives 10 ul of 1:5 diluted compounds in DMSO, 80 ul of Phosphorylation buffer (minus ATP), and 30 ul FAKcd solution.
9. (Signal) Control wells receive 10 ul of 1:5 diluted DMSO (minus Compound) in Kinase phosphorylation buffer, 80 ul of 75 uM ATP, and 30 ul of 1:1000 FAKcd enzyme.
10. Incubate reaction at room temperature for 15 minutes with gentle shaking on a plate shaker.
11. Terminate the reaction by aspirating off the reaction mixture and washing 3 times with wash buffer.
12. Dilute phospho-tyrosine HRP-conjugated (pY20HRP) antibody to 0.250 ug/ml (1:1000 of Stock) in blocking buffer. Dispense 100 ul per well, and incubate with shaking for 30 min. at R. T.
13. Aspirate the supernatant and wash the plate 3 times with wash buffer.
14. Add 100 ul per well of room temperature TMB solution to initiate color development. Color development is terminated after approximately 15-30 sec. by the addition of 100 ul of 0.09M H2SO4 per well.
15. The signal is quantitated by measurement of absorbance at 450 nm on the BioRad microplate reader or a microplate reader capable of reading at OD450.
16. Inhibition of tyrosine kinase activity would result in a reduced absorbance signal. The signal is typically 0.8-1.0 OD units. The values are reported as IC 50s , uM concentration.
FAK Inducible Cell-Based ELISA: Final Protocol
Materials:
Reacti-Bind Goat Anti-Rabbit Plates 96-well (Pierce Product#15135ZZ @115.00 USD)
FAKpY397 rabbit polyclonal antibody (Biosource #44624 @315.00 USD)
ChromePure Rabbit IgG, whole molecule (Jackson Laboratories #001-000-003 @60/25 mg USD)
UBI αFAK clone 2A7 mouse monoclonal antibody (Upstate#05-182 @289.00 USD)
Peroxidase-conjugated AffiniPure Goat Anti-Mouse IgG (Jackson Labs #115-035-146 @95/1.5 ml USD)
SuperBlock TBS (Pierce Product#37535ZZ @99 USD)
Bovine Serum Albumin (Sigma #A-9647 @117.95/100 g USD)
TMB Peroxidase substrate (Oncogene Research Products #CL07-100 ml @40.00 USD)
Na3VO4 Sodium Orthovanadate (Sigma #S6508 @43.95/50 g USD)
MTT substrate (Sigma #M-2128 @25.95/500 mg USD)
Growth Media: DMEM+10% FBS, P/S, Glu, 750 ug/ml Zeocin and 50 ug/ml Hygromycin (Zeocin InVitrogen #R250-05 @725 USD and Hygromycon InVitrogen #R220-05 @150 USD)
Mifepristone InVitrogen #H110-01 @125 USD
CompleteTM EDTA-free Protease Inhibitor pellet Boehringer Mannheim #1873580
FAK Cell-Based Protocol for Selectivity of Kinase-Dependent PhosphoFAKY397
Procedure:
An inducible FAK cell-based assay in ELISA format for the screening of chemical matter to identify tyrosine kinase specific inhibitors was developed. The cell-based assay exploits the mechanism of the GeneSwitchTM system (InVitrogen) to exogenously control the expression and phosphorylation of FAK and the kinase-dependent autophosphorylation site at residue Y397.
Inhibition of the kinase-dependent autophosphorylation at Y397 results in a reduced absorbance signal at OD450. The signal is typically 0.9 to 1.5 OD450 units with the noise falling in the range of 0.08 to 0.1 OD450 units. The values are reported as IC50s, uM concentration.
On day 1, grow A431·FAKwt in T175 flasks. On the day prior to running the FAK cell-assay, seed A431·FAKwt cells in growth media on 96-well U-bottom plates. Allow cells to sit at 37° C., 5% CO2 for 6 to 8 hours prior to FAK induction. Prepare Mifepristone stock solution of 10 uM in 100% Ethanol. The stock solution is subsequently diluted to 10× of the final concentration in Growth Media. Transfer 10 ul of this dilution (final concentration of 0.1 nM Mifepristone) into each well. Allow cells to sit at 37° C., 5% CO2 overnight (12 to 16 hours). Also, prepare control wells without Mifepristone induction of FAK expression and phosphorylation.
On day 2, coat Goat Anti-Rabbit plate(s) with 3.5 ug/ml of phosphospecific FAKpY397 polyclonal antibody prepared in SuperBlock TBS buffer, and allow plate(s) to shake on a plate shaker at room temperature for 2 hours. Optionally, control wells may be coated with 3.5 ug/ml of control Capture antibody (Whole Rabbit IgG molecules) prepared in SuperBlock TBS. Wash off excess FAKpY397 antibody 3 times using buffer. Block Anti-FAKpY397 coated plate(s) with 200 ul per well of 3% BSA/0.5% Tween Blocking buffer for 1 hour at room temperature on the plate shaker. While the plate(s) are blocking, prepare compound stock solutions of 5 mM in 100% DMSO. The stock solutions are subsequently serially diluted to 100× of the final concentration in 100% DMSO. Make a 1:10 dilution using the 100× solution into growth media and transfer 10 ul of the appropriate compound dilutions to each well containing either the FAK induced or uninduced control A431 cells for 30 minutes at 37° C., 5% CO2. Prepare RIPA lysis buffer (50 mM Tris-HCl, pH7.4, 1% NP-40, 0.25% Na-deoxycholate, 150 mM NaCl, 1 mM EDTA, 1 mM Na3VO4, 1 mM NaF, and one CompleteTM EDTA-free protease inhibitor pellet per 50 ml solution). At the end of 30 minutes compound treatment, wash off compound 3 times using TBS-T wash buffer. Lyse cells with 100 ul/well of RIPA buffer.
To the coated plate, remove blocking buffer and wash 3 times using TBS-T wash buffer. Using a 96-well automated microdispenser, transfer 100 ul of whole cell-lysate (from step 6) to the Goat Anti-Rabbit FAKpY397 coated plate(s) to capture phosphoFAKY397 proteins. Shake at room temperature for 2 hours. Wash off unbound proteins 3 times using TBS-T wash buffer. Prepare 0.5 ug/ml (1:2000 dilution) of UBI αFAK detection antibody in 3% BSA/0.5% Tween blocking buffer. Dispense 100 ul of UBI αFAK solution per well and shake for 30 minutes at room temperature. Wash off excess UBI αFAK antibody 3 times using TBS-T wash buffer. Prepare 0.08 ug/ml (1:5000 dilution) of secondary Anti-Mouse Peroxidase (Anti-2MHRP) conjugated antibody. Dispense 100 ul per well of the Anti-2MHRP solution and shake for 30 minutes at room temperature. Wash off excess Anti-2MHRP antibody 3 times using TBS-T wash buffer. Add 100 ul per well of room temperature TMB substrate solution to allow for color development. Terminate the TMB reaction with 100 ul per well of TMB stop solution (0.09M H2SO4) and quantitate the signal by measurement of absorbance at 450 nm on the BioRad microplate reader.
Additional FAK cell assays are hereby incorporated by reference from Pfizer Appl. No. 60/412,078 entitled “INDUCIBLE FOCAL ADHESION KINASE CELL ASSAY”.
In a preferred embodiment, the compounds of the present invention have an in vivo activity as determined by a kinase assay, e.g., such as that described herein, of less than 100 nM. Preferably, the compounds have an IC 50 of less than 25 nM in the kinase assay, and more preferably less than 10 nM. In a further preferred embodiment, the compounds exhibit an IC 50 in a FAK cell based assay, e.g., such as that described herein, of less than 1 □M, more preferably less than 100 nM, and most preferably less than 25 nM.
Administration of the compounds of the present invention (hereinafter the “active compound(s)”) can be effected by any method that enables delivery of the compounds to the site of action. These methods include oral routes, intraduodenal routes, parenteral injection (including intravenous, subcutaneous, intramuscular, intravascular or infusion), topical, and rectal administration.
The amount of the active compound administered will be dependent on the subject being treated, the severity of the disorder or condition, the rate of administration, the disposition of the compound and the discretion of the prescribing physician. However, an effective dosage is in the range of about 0.001 to about 100 mg per kg body weight per day, preferably about 1 to about 35 mg/kg/day, in single or divided doses. For a 70 kg human, this would amount to about 0.05 to about 7 g/day, preferably about 0.2 to about 2.5 g/day. In some instances, dosage levels below the lower limit of the aforesaid range may be more than adequate, while in other cases still larger doses may be employed without causing any harmful side effect, provided that such larger doses are first divided into several small doses for administration throughout the day.
The active compound may be applied as a sole therapy or may involve one or more other anti-tumour substances, for example those selected from, for example, mitotic inhibitors, for example vinblastine; alkylating agents, for example cis-platin, carboplatin and cyclophosphamide; anti-metabolites, for example 5-fluorouracil, cytosine arabinoside and hydroxyurea, or, for example, one of the preferred anti-metabolites disclosed in European Patent Application No. 239362 such as N -(5-[ N -(3,4-dihydro-2-methyl-4-oxoquinazolin-6-ylmethyl)- N -methylamino]-2-thenoyl)-L-glutamic acid; growth factor inhibitors; cell cycle inhibitors; intercalating antibiotics, for example adriamycin and bleomycin; enzymes, for example interferon; and anti-hormones, for example anti-estrogens such as Nolvadex□ (tamoxifen) or, for example anti-androgens such as Casodex□ (4′-cyano-3-(4-fluorophenylsulphonyl)-2-hydroxy-2-methyl-3′-(trifluoromethyl)propionanilide). Such conjoint treatment may be achieved by way of the simultaneous, sequential or separate dosing of the individual components of the treatment.
The pharmaceutical composition may, for example, be in a form suitable for oral administration as a tablet, capsule, pill, powder, sustained release formulations, solution, suspension, for parenteral injection as a sterile solution, suspension or emulsion, for topical administration as an ointment or cream or for rectal administration as a suppository. The pharmaceutical composition may be in unit dosage forms suitable for single administration of precise dosages. The pharmaceutical composition will include a conventional pharmaceutical carrier or excipient and a compound according to the invention as an active ingredient. In addition, it may include other medicinal or pharmaceutical agents, carriers, adjuvants, etc.
Exemplary parenteral administration forms include solutions or suspensions of active compounds in sterile aqueous solutions, for example, aqueous propylene glycol or dextrose solutions. Such dosage forms can be suitably buffered, if desired.
Suitable pharmaceutical carriers include inert diluents or fillers, water and various organic solvents. The pharmaceutical compositions may, if desired, contain additional ingredients such as flavorings, binders, excipients and the like. Thus for oral administration, tablets containing various excipients, such as citric acid may be employed together with various disintegrants such as starch, alginic acid and certain complex silicates and with binding agents such as sucrose, gelatin and acacia. Additionally, lubricating agents such as magnesium stearate, sodium lauryl sulfate and talc are often useful for tableting purposes. Solid compositions of a similar type may also be employed in soft and hard filled gelatin capsules. Preferred materials, therefor, include lactose or milk sugar and high molecular weight polyethylene glycols. When aqueous suspensions or elixirs are desired for oral administration the active compound therein may be combined with various sweetening or flavoring agents, coloring matters or dyes and, if desired, emulsifying agents or suspending agents, together with diluents such as water, ethanol, propylene glycol, glycerin, or combinations thereof.
Methods of preparing various pharmaceutical compositions with a specific amount of active compound are known, or will be apparent, to those skilled in this art. For examples, see Remington's Pharmaceutical Sciences , Mack Publishing Company, Easter, Pa., 15th Edition (1975).
The examples and preparations provided below further illustrate and exemplify the compounds of the present invention and methods of preparing such compounds. It is to be understood that the scope of the present invention is not limited in any way by the scope of the following examples and preparations. In the following examples molecules with a single chiral center, unless otherwise noted, exist as a racemic mixture. Those molecules with two or more chiral centers, unless otherwise noted, exist as a racemic mixture of diastereomers. Single enantiomers/diastereomers may be obtained by methods known to those skilled in the art.
Where HPLC chromatography is referred to in the preparations and examples below, the general conditions used, unless otherwise indicated, are as follows. The column used is a ZORBAX□ RXC18 column (manufactured by Hewlett Packard) of 150 mm distance and 4.6 mm interior diameter. The samples are run on a Hewlett Packard-1100 system. A gradient solvent method is used running 100 percent ammonium acetate/acetic acid buffer (0.2 M) to 100 percent acetonitrile over 10 minutes. The system then proceeds on a wash cycle with 100 percent acetonitrile for 1.5 minutes and then 100 percent buffer solution for 3 minutes. The flow rate over this period is a constant 3 ml/minute.
In the following examples and preparations, “Et” means ethyl, “Ac” means acetyl, “Me” means methyl, and “Bu” means butyl.
EXAMPLES
General Methods
Preparation of 5-nitro-oxindole
To a solution of oxindole (26 g) in 100 mL of concentrated sulfuric acid at −15° C. was added fuming nitric acid (8.4 mL) dropwise. Careful attention was paid to maintain the reaction temperature at −15° C. After the addition was complete, the reaction was stirred for 30 minutes and then poured into ice water. A yellow precipitate was formed which was isolated by filtration to provide 34 grams (98%) of 5-nitro oxindole.
Preparation of 5-amino-oxindole (2)
To a solution of 5-nitro-oxindole (25 g) in 120 mL of dimethylacetamide in a Parr bottle was added 10% Pd/C (0.5 g). The mixture was hydrogenated (40 psi H2) for 16 h. The catalyst was removed by filtration and the filtrate was diluted with ether (2 L) to provide 5-amino-oxindole (10.5 g; 50%).
Preparation of 2,4-dichloro-5-trifluoromethylpyrimidine (3)
5-Trifluoromethyluracil (250 g, 1.39 mol) and phosphorous oxychloride (655 mL, 6.94 mol, 5 equiv) were charged to a 3 L 4-neck flask equipped with overhead stirrer, a reflux condenser, an addition funnel and an internal theromocouple. The contents were maintained under a nitrogen atmosphere as concentrated phosphoric acid (85 wt %, 9.5 mL, 0.1 equiv) was added in one portion to the slurry, resulting in a moderate exotherm. Diisopropylethylamine (245 mL, 1.39 mol, 1 equiv) was then added dropwise over 15 min at such a rate that the internal temperature of the reaction reached 85-90° C. by the end of the addition. By the end of the amine addition the reaction mixture was a homogenous light-orange solution. Heating was initiated and the orange solution was maintained at 100° C. for 20 h, at which time HPLC analysis of the reaction mixture indicated that the starting material was consumed. External heating was removed and the contents of the flask were cooled to 40° C. and then added dropwise to a cooled mixture of 3N HCl (5 L, 10 equiv) and diethyl ether (2 L) keeping the temperature of the quench pot between 10 and 15° C. The layers were separated, and the aqueous layer was extracted once with ether (1 L). The combined organic layers were combined, washed with water until the washes were neutral (5×1.5 L washes), dried with MgSO 4 and concentrated to provide 288 g (95% yield) of a light yellow-orange oil of 96% purity (HPLC). This material can be further purified by distillation (bp 109° C. at 79 mmHg).
Preparation of 5-(4-Chloro-5-trifluoromethyl-pyrimidin-2-ylamino)-1,3-dihydro-indol-2-one (4)
To a solution of 5-trifluoromethyl-2,4-dichloropyrimidine (214.8 g; 0.921 mol) in 1:1 DCE/tBuOH (1.240 L) was added Zinc chloride 1M solution in ether (1 eq; 0.921 L). After 0.5 hour, 5-amino-oxindole (124 g; 0.837 mol) was added followed by triethylamine (129.4 ml; 0.921 mol) keeping temperature at 25° C. The reaction was allowed to stir at room temperature overnight, then was concentrated and the product triturated from methanol as a yellow solid (224.3 g; 82%). 1 H NMR (DMSO-d 6 , 400 MHz) □ 3.29 (s, 2H), 6.76 (d, J=7.9 Hz, 2H), 7.39 (d, J=8.3 Hz), 7.51 (br s, 1H), 8.71 (s, 1H), 10.33 (s, 1H), 10.49 (s, 1H). 13 C NMR (DMSO-d 6 , 100 MHz) □ 177.0, 161.3, 158.7 (br), 140.7, 132.8, 126.9, 123.7 (q, J=268 Hz), 121.0, 118.7, 111.2 (q, J=32 Hz), 109.6, 36.7; HPLC ret. time: 5.759 min. LRMS (M+) 329.1, 331.1.
Example 1
5-[4-(R-1-Phenyl-ethylamino)-5-trifluoromethyl-pyrimidin-2-ylamino]-1,3-dihydro-indol-2-one
To a solution of 1:1 DCE/t-BuOH alcohol (1:1 ratio, 4 mL) and 5-(4-Chloro-5-trifluoromethyl-pyrimdin-2-ylamino)-1,3-dihydro-indol-2-one (0.15 g; 0.456 mmole) was added (R)(+) alpha phenethyl amine (0.071 mL; 0.547 mmole) and diisopropyl ethyl amine (0.081 mL, 0.456 mmole). The resultant solution was stirred under nitrogen and heated to 80° C. for 16 hours. The reaction was cooled to room temperature, diluted with ˜10 mL of a 1:1 mixture of dichloromethane and methanol followed by the addition of 0.5 g of MP-carbonate. The resultant mixture was stirred, filtered, concentrated and purified by silica gel chromatography (97:2.8:0.3 ratio of chloroform/methanol/concentrated ammonium hydroxide). The desired title compounds was obtained as a white solid (0.021 g; 11%). HPLC ret. time: 6.46 min. LRMS (M+) 413.4
The following compounds of the invention were prepared by heating chloropyrimidine (4) with an appropriate amine as in Example 1. Amines used in these reactions were either obtained commercially and used as received or alternatively they were prepared by common synthetic methods for amines known to those skilled in the art. Unless otherwise noted, compounds having chiral centers were prepared as racemic mixtures.
TABLE 1
Compounds Prepared by the Method of Example 1:
HPLC
Retention
Time
MS
Compound Name
(min.)
Data (M + H)
N-(1-Methyl-1-phenyl-ethyl)-3-{[2-(2-oxo-2,3-
6.46
597.5
dihydro-1H-indol-5-ylamino)-5-trifluoromethyl-pyrimidin-
4-ylamino]-methyl}-benzenesulfonamide
3-{[2-(2-Oxo-2,3-dihydro-1H-indol-5-ylamino)-5-
4.87
479.1
trifluoromethyl-pyrimidin-4-ylamino]-methyl}-
benzenesulfonamide
5-{4-[3-(Trifluoro-methanesulfonyl)-
6.35
532.1
benzylamino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-
dihydro-indol-2-one
5-{4-[(Piperidin-3-ylmethyl)-amino]-5-
3.74
407.3
trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-
one
5-{4-[(1-Methanesulfonyl-piperidin-3-ylmethyl)-
5.21
485.2
amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-
dihydro-indol-2-one
N-(3-{[2-(2-Oxo-2,3-dihydro-1H-indol-5-
5.22
493.3
ylamino)-5-trifluoromethyl-pyrimidin-4-ylamino]-methyl}-
phenyl)-methanesulfonamide
3-Oxo-3-(3-{[2-(2-oxo-2,3-dihydro-1H-indol-5-
4.92
474.3
ylamino)-5-trifluoromethyl-pyrimidin-4-ylamino]-methyl}-
piperidin-1-yl)-propionitrile
5-{4-[3-(1,1-Dioxo-1N 6 -isothiazolidin-2-yl)-
4.89
471.1
propylamino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-
dihydro-indol-2-one
5-[4-(2-Methyl-butylamino)-5-trifluoromethyl-
6.53
380.3
pyrimidin-2-ylamino]-1,3-dihydro-indol-2-one
5-{4-[(1-Methanesulfonyl-piperidin-2-ylmethyl)-
5.17
485.3
amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-
dihydro-indol-2-one
N-{2-[2-(2-Oxo-2,3-dihydro-1H-indol-5-ylamino)-
4.38
431.2
5-trifluoromethyl-pyrimidin-4-ylamino]-ethyl}-
methanesulfonamide
N-{4-[2-(2-Oxo-2,3-dihydro-1H-indol-5-ylamino)-
4.78
459.3
5-trifluoromethyl-pyrimidin-4-ylamino]-butyl}-
methanesulfonamide
5-{4-[(1-Methanesulfonyl-piperidin-4-ylmethyl)-
5.22
485.3
amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-
dihydro-indol-2-one
N-Methyl-N-{2-[2-(2-oxo-2,3-dihydro-1H-indol-5-
4.81
445.1
ylamino)-5-trifluoromethyl-pyrimidin-4-ylamino]-ethyl}-
methanesulfonamide
Methanesulfonic acid 3-{[2-(2-oxo-2,3-dihydro-
5.67
494.1
1H-indol-5-ylamino)-5-trifluoromethyl-pyrimidin-4-
ylamino]-methyl}-phenyl ester
N-{3-[2-(2-Oxo-2,3-dihydro-1H-indol-5-ylamino)-
4.58
445.1
5-trifluoromethyl-pyrimidin-4-ylamino]-propyl}-
methanesulfonamide
5-{4-[(4-Methanesulfonyl-morpholin-2-ylmethyl)-
4.87
487.2
amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-
dihydro-indol-2-one
N-(4-Fluoro-3-{[2-(2-oxo-2,3-dihydro-1H-indol-5-
5.29
511.1
ylamino)-5-trifluoromethyl-pyrimidin-4-ylamino]-methyl}-
phenyl)-methanesulfonamide
5-{4-[(5-Oxo-morpholin-2-ylmethyl)-amino]-5-
4.12
423.3
trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-
one
N-(4-Methoxy-3-{[2-(2-oxo-2,3-dihydro-1H-indol-
5.38
523.2
5-ylamino)-5-trifluoromethyl-pyrimidin-4-ylamino]-
methyl}-phenyl)-methanesulfonamide
N-(4-Methyl-3-{[2-(2-oxo-2,3-dihydro-1H-indol-5-
5.30
507.2
ylamino)-5-trifluoromethyl-pyrimidin-4-ylamino]-methyl}-
phenyl)-methanesulfonamide
5-[4-(3-Methanesulfonylmethyl-benzylamino)-5-
5.14
492.2
trifluoromethyl-pyrimidin-2-ylamino]-1,3-dihydro-indol-2-
one
5-{4-[(4-Trifluoroacetyl-morpholin-2-ylmethyl)-
5.64
505.1
amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-
dihydro-indol-2-one
5-{4-[(1-Methanesulfonyl-azetidin-3-ylmethyl)-
4.76
457.2
amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-
dihydro-indol-2-one
N-Methyl-N-(4-methyl-3-{[2-(2-oxo-2,3-dihydro-
6.66
521.3
1H-indol-5-ylamino)-5-trifluoromethyl-pyrimidin-4-
ylamino]-methyl}-phenyl)-methanesulfonamide
5-{4-[(1-Methanesulfonyl-pyrrolidin-3-ylmethyl)-
4.97
471.2
amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-
dihydro-indol-2-one
N-Methyl-N-{3-[2-(2-oxo-2,3-dihydro-1H-indol-5-
5.02
459.2
ylamino)-5-trifluoromethyl-pyrimidin-4-ylamino]-propyl}-
methanesulfonamide
5-{4-[2-(1-Methanesulfonyl-piperidin-2-yl)-
5.71
499.4
ethylamino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-
dihydro-indol-2-one
5-{4-[(4-Methanesulfonyl-pyridin-2-ylmethyl)-
4.68
479.1
amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-
dihydro-indol-2-one
{2,2-Dimethyl-3-[2-(2-oxo-2,3-dihydro-1H-indol-
7.01
495.0
5-ylamino)-5-trifluoromethyl-pyrimidin-4-ylamino]-
propyl}-carbamic acid tert-butyl ester
5-[4-(3-Isopropoxy-propylamino)-5-
6.27
410.4
trifluoromethyl-pyrimidin-2-ylamino]-1,3-dihydro-indol-2-
one
5-{4-[(1-Methyl-piperidin-3-ylmethyl)-amino]-5-
3.71
421.0
trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-
one
5-{4-[(Tetrahydro-pyran-4-ylmethyl)-amino]-5-
5.16
408.3
trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-
one
5-[4-(2-Ethyl-butylamino)-5-trifluoromethyl-
6.95
394.3
pyrimidin-2-ylamino]-1,3-dihydro-indol-2-one
5-{4-[(Tetrahydro-furan-2R-ylmethyl)-amino]-5-
5.30
394.3
trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-
one
5-{4-[(Tetrahydro-furan-2S-ylmethyl)-amino]-5-
5.30
394.3
trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-
one
5-{4-[(5-Methyl-furan-2-ylmethyl)-amino]-5-
5.98
404.2
trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-
one
5-{4-[(1-Methanesulfonyl-pyrrolidin-2-ylmethyl)-
5.08
471.3
amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-
dihydro-indol-2-one
5-{4-[(Adamantan-2-ylmethyl)-amino]-5-
7.89
458.3
trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-
one
5-{4-[(Adamantan-2-ylmethyl)-amino]-5-
5.20
473.3
trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-
one
5-[4-(2-Methoxy-2-methyl-propylamino)-5-
5.87
396.3
trifluoromethyl-pyrimidin-2-ylamino]-1,3-dihydro-indol-2-
one
5-{4-[(endo-Bicyclo[2.2.1]hept-5-en-2-ylmethyl)-
6.74
416.3
amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-
dihydro-indol-2-one
(3-{[2-(2-Oxo-2,3-dihydro-1H-indol-5-ylamino)-5-
5.03
522.2
trifluoromethyl-pyrimidin-4-ylamino]-methyl}-benzyl)-
phosphonic acid dimethyl ester
5-[4-(3-Methyl-butylamino)-5-trifluoromethyl-
6.87
380.2
pyrimidin-2-ylamino]-1,3-dihydro-indol-2-one
5-{4-[(2-Hydroxy-cyclohexylmethyl)-amino]-5-
6.66
422.2
trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-
one
N-(4-Methoxy-3-{[2-(2-oxo-2,3-dihydro-1H-indol-
5.69
537.2
5-ylamino)-5-trifluoromethyl-pyrimidin-4-ylamino]-
methyl}-phenyl)-N-methyl-methanesulfonamide
5-{4-[(4-Ethanesulfonyl-morpholin-2-ylmethyl)-
5.11
501.3
amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-
dihydro-indol-2-one
5-(4-{[4-(Propane-2-sulfonyl)-morpholin-2-
5.35
515.2
ylmethyl]-amino}-5-trifluoromethyl-pyrimidin-2-ylamino)-
1,3-dihydro-indol-2-one
5-{4-[(4-Acetyl-morpholin-2-ylmethyl)-amino]-5-
4.43
451.2
trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-
one
5-{4-[(4-Propionyl-morpholin-2-ylmethyl)-amino]-
4.74
465.2
5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-
2-one
5-(4-{[4-(2,2-Dimethyl-propionyl)-morpholin-2-
5.43
493.2
ylmethyl]-amino}-5-trifluoromethyl-pyrimidin-2-ylamino)-
1,3-dihydro-indol-2-one
2-{[2-(2-Oxo-2,3-dihydro-1H-indol-5-ylamino)-5-
5.04
467.2
trifluoromethyl-pyrimidin-4-ylamino]-methyl}-morpholine-
4-carboxylic acid methyl ester
5-{4-[(4-Methoxyacetyl-morpholin-2-ylmethyl)-
4.44
481.2
amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-
dihydro-indol-2-one
5-[4-(3-Ethanesulfonyl-benzylamino)-5-
5.36
492.3
trifluoromethyl-pyrimidin-2-ylamino]-1,3-dihydro-indol-2-
one
5-{4-[(4-Methanesulfonyl-morpholin-2R-
4.84
487.3
ylmethyl)-amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-
1,3-dihydro-indol-2-one
5-{4-[(4-Methanesulfonyl-morpholin-2S-
4.86
487.3
ylmethyl)-amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-
1,3-dihydro-indol-2-one
5-{4-[(Pyrimidin-2-ylmethyl)-amino]-5-
4.53
402.3
trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-
one
5-{4-[(Pyrazin-2-ylmethyl)-amino]-5-
4.42
402.1
trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-
one
N-(4-Fluoro-3-{[2-(2-oxo-2,3-dihydro-1H-indol-5-
5.55
523.3
ylamino)-5-trifluoromethyl-pyrimidin-4-ylamino]-methyl}-
phenyl)-N-methyl-methanesulfonamide
5-{4-[(1-Methanesulfonyl-piperidin-3-ylmethyl)-
5.17
485.3
amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-
dihydro-indol-2-one
5-{4-[(4-Isobutyryl-morpholin-2-ylmethyl)-amino]-5-
5.03
479.2
trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-
one
5-[4-(3,3-Dimethyl-2-oxo-butylamino)-5-
6.00
408.2
trifluoromethyl-pyrimidin-2-ylamino]-1,3-dihydro-indol-2-
one
5-[4-(1,2-Dimethyl-propylamino)-5-
6.65
380.3
trifluoromethyl-pyrimidin-2-ylamino]-1,3-dihydro-indol-2-
one
5-[4-(2-Methoxy-1-methyl-ethylamino)-5-
5.57
382.3
trifluoromethyl-pyrimidin-2-ylamino]-1,3-dihydro-indol-2-
one
5-{4-[2-(1,1-Dioxo-1D 6 -isothiazolidin-2-yl)-
4.59
457.3
ethylamino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-
dihydro-indol-2-one
5-[4-(3-Methylamino-propylamino)-5-
3.47
381.3
trifluoromethyl-pyrimidin-2-ylamino]-1,3-dihydro-indol-2-
one
5-{4-[(Pyridin-3-ylmethyl)-amino]-5-
4.62
401.3
trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-
one
5-{4-[(6-Methanesulfonyl-pyridin-2-ylmethyl)-
4.89
479.3
amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-
dihydro-indol-2-one
5-{4-[3-(1,1-Dioxo-1,I,6-isothiazolidin-2-yl)-
5.45
519.2
benzylamino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-
dihydro-indol-2-one
5-[4-(1R-Phenyl-ethylamino)-5-trifluoromethyl-
6.42
414.4
pyrimidin-2-ylamino]-1,3-dihydro-indol-2-one
5-(4-Isopropylamino-5-trifluoromethyl-pyrimidin-
5.84
352.2
2-ylamino)-1,3-dihydro-indol-2-one
5-(4R-sec-Butylamino-5-trifluoromethyl-
6.22
366.2
pyrimidin-2-ylamino)-1,3-dihydro-indol-2-one
5-(4S-sec-Butylamino-5-trifluoromethyl-
6.23
366.2
pyrimidin-2-ylamino)-1,3-dihydro-indol-2-one
5-[4-(2-Methylamino-ethylamino)-5-
3.29
367.3
trifluoromethyl-pyrimidin-2-ylamino]-1,3-dihydro-indol-2-
one
5-[4-(1S-Phenyl-ethylamino)-5-trifluoromethyl-
6.42
414.3
pyrimidin-2-ylamino]-1,3-dihydro-indol-2-one
5-{4-[(2-Methanesulfonylmethyl-thiazol-4-
4.72
499.3
ylmethyl)-amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-
1,3-dihydro-indol-2-one
5-(4-Propylamino-5-trifluoromethyl-pyrimidin-2-
5.91
352.2
ylamino)-1,3-dihydro-indol-2-one
5-[4-(2-Hydroxy-1-methyl-ethylamino)-5-
4.49
368.2
trifluoromethyl-pyrimidin-2-ylamino]-1,3-dihydro-indol-2-
one
5-[4-(1-Hydroxymethyl-propylamino)-5-
4.85
382.2
trifluoromethyl-pyrimidin-2-ylamino]-1,3-dihydro-indol-2-
one
5-{4-[(5-Methanesulfonyl-pyridin-3-ylmethyl)-
4.55
479.4
amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-
dihydro-indol-2-one
5-{4-[(Pyridin-4-ylmethyl)-amino]-5-
4.49
401.2
trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-
one
5-[4-(1,3-Dimethyl-butylamino)-5-trifluoromethyl-
6.99
394.3
pyrimidin-2-ylamino]-1,3-dihydro-indol-2-one
N-Isopropyl-N-{3-[2-(2-oxo-2,3-dihydro-1H-indol-
5.12
487.3
5-ylamino)-5-trifluoromethyl-pyrimidin-4-ylamino]-
propyl}-methanesulfonamide
5-[4-(1S-Hydroxymethyl-2-methyl-propylamino)-
5.23
396.3
5-trifluoromethyl-pyrimidin-2-ylamino]-1,3-dihydro-indol-
2-one
N-Cyclohexyl-N-{3-[2-(2-oxo-2,3-dihydro-1H-
6.24
527.2
indol-5-ylamino)-5-trifluoromethyl-pyrimidin-4-ylamino]-
propyl}-methanesulfonamide
5-[4-(1,2,3,4-Tetrahydro-naphthalen-1-ylamino)-
440.4
7.17
5-trifluoromethyl-pyrimidin-2-ylamino]-1,3-dihydro-indol-
2-one
5-{4-[(1-Methanesulfonyl-pyrrolidin-2S-ylmethyl)-
5.07
471.2
amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-
dihydro-indol-2-one
5-{4-[(3-Methyl-thiophen-2-ylmethyl)-amino]-5-
6.18
420.4
trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-
one
5-{4-[(1-Methanesulfonyl-pyrrolidin-3R-
4.95
471.2
ylmethyl)-amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-
1,3-dihydro-indol-2-one
5-[4-(2-Hydroxy-1S-phenyl-ethylamino)-5-
5.28
430.3
trifluoromethyl-pyrimidin-2-ylamino]-1,3-dihydro-indol-2-
one
5-[4-(2-Hydroxy-1S-methyl-ethylamino)-5-
4.49
368.3
trifluoromethyl-pyrimidin-2-ylamino]-1,3-dihydro-indol-2-
one
5-[4-(1R-Hydroxymethyl-propylamino)-5-
4.85
382.2
trifluoromethyl-pyrimidin-2-ylamino]-1,3-dihydro-indol-2-
one
5-[4-(1-Pyrimidin-4-yl-ethylamino)-5-
4.84
416.3
trifluoromethyl-pyrimidin-2-ylamino]-1,3-dihydro-indol-2-
one
5-[4-(1,1-Dioxo-tetrahydro-1-thiophen-3-
4.67
426.3
ylamino)-5-trifluoromethyl-pyrimidin-2-ylamino]-1,3-
dihydro-indol-2-one
5-{4-[(1H-Imidazol-2-ylmethyl)-amino]-5-
3.27
390.3
trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-
one
5-[4-(2-Piperidin-2-yl-ethylamino)-5-
3.79
421.4
trifluoromethyl-pyrimidin-2-ylamino]-1,3-dihydro-indol-2-
one
5-[4-(Isobutyl-methyl-amino)-5-trifluoromethyl-
6.82
380.3
pyrimidin-2-ylamino]-1,3-dihydro-indol-2-one
N-Methyl-N-(3-{[2-(2-oxo-2,3-dihydro-1H-indol-
5.49
507.4
5-ylamino)-5-trifluoromethyl-pyrimidin-4-ylamino]-
methyl}-phenyl)-methanesulfonamide
N-Ethyl-N-(3-{[2-(2-oxo-2,3-dihydro-1H-indol-5-
5.67
521.3
ylamino)-5-trifluoromethyl-pyrimidin-4-ylamino]-methyl}-
phenyl)-methanesulfonamide
5-[4-(2-Methanesulfonyl-benzylamino)-5-
5.47
478.2
trifluoromethyl-pyrimidin-2-ylamino]-1,3-dihydro-indol-2-
one
N-Isopropyl-N-(3-{[2-(2-oxo-2,3-dihydro-1H-
5.81
535.3
indol-5-ylamino)-5-trifluoromethyl-pyrimidin-4-ylamino]-
methyl}-phenyl)-methanesulfonamide
5-{4-[(3,4,5,6-Tetrahydro-2H-[1,2′]bipyridinyl-3-
5.79
484.3
ylmethyl)-amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-
1,3-dihydro-indol-2-one
5-{4-[(1-Pyrimidin-2-yl-piperidin-3-ylmethyl)-
6.17
485.3
amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-
dihydro-indol-2-one
5-{4-[2R-(1-Methanesulfonyl-piperidin-2-yl)-
5.70
499.4
ethylamino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-
dihydro-indol-2-one
5-{4-[2S-(1-Methanesulfonyl-piperidin-2-yl)-
5.70
499.4
ethylamino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-
dihydro-indol-2-one
5-[4-(3-Methylsulfanyl-propylamino)-5-
5.83
398.2
trifluoromethyl-pyrimidin-2-ylamino]-1,3-dihydro-indol-2-
one
5-[4-(1S-Hydroxymethyl-3-methylsulfanyl-
5.02
428.2
propylamino)-5-trifluoromethyl-pyrimidin-2-ylamino]-1,3-
dihydro-indol-2-one
5-[4-(2-Hydroxy-1R-methyl-ethylamino)-5-
4.49
368.3
trifluoromethyl-pyrimidin-2-ylamino]-1,3-dihydro-indol-2-
one
5-[4-(1R-Hydroxymethyl-2-methyl-propylamino)-
5.23
396.4
5-trifluoromethyl-pyrimidin-2-ylamino]-1,3-dihydro-indol-
2-one
N-Ethyl-N-{3-[2-(2-oxo-2,3-dihydro-1H-indol-5-
5.31
473.3
ylamino)-5-trifluoromethyl-pyrimidin-4-ylamino]-propyl}-
methanesulfonamide
5-{4-[(1-Methanesulfonyl-pyrrolidin-3R-
4.94
471.4
ylmethyl)-amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-
1,3-dihydro-indol-2-one
5-[4-(1S-Hydroxymethyl-propylamino)-5-
4.86
382.3
trifluoromethyl-pyrimidin-2-ylamino]-1,3-dihydro-indol-2-
one
5-[4-(3,5-Dinitro-benzylamino)-5-trifluoromethyl-
6.04
490.1
pyrimidin-2-ylamino]-1,3-dihydro-indol-2-one
N-(2-{[2-(2-Oxo-2,3-dihydro-1H-indol-5-
5.84
493.1
ylamino)-5-trifluoromethyl-pyrimidin-4-ylamino]-methyl}-
phenyl)-methanesulfonamide
N-Isopropyl-N-{2-[2-(2-oxo-2,3-dihydro-1H-indol-
5.37
473.3
5-ylamino)-5-trifluoromethyl-pyrimidin-4-ylamino]-ethyl}-
methanesulfonamide
5-[4-(2-Hydroxy-1-phenyl-ethylamino)-5-
5.29
430.3
trifluoromethyl-pyrimidin-2-ylamino]-1,3-dihydro-indol-2-
one
5-[4-(1R-Hydroxymethyl-3-methyl-butylamino)-5-
5.59
410.4
trifluoromethyl-pyrimidin-2-ylamino]-1,3-dihydro-indol-2-
one
5-[4-(1S-Hydroxymethyl-3-methyl-butylamino)-5-
5.59
410.4
trifluoromethyl-pyrimidin-2-ylamino]-1,3-dihydro-indol-2-
one
5-{4-[(1-Methanesulfonyl-piperidin-2S-ylmethyl)-
5.16
485.3
amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-
dihydro-indol-2-one
5-{4-[(1-Methanesulfonyl-pyrrolidin-2R-
5.08
471.3
ylmethyl)-amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-
1,3-dihydro-indol-2-one
5-[4-(Methyl-pyridin-2-ylmethyl-amino)-5-
5.37
415.3
trifluoromethyl-pyrimidin-2-ylamino]-1,3-dihydro-indol-2-
one
5-{4-[(3-Methanesulfonyl-benzyl)-methyl-amino]-
5.66
492.3
5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-
2-one
N-Methyl-N-(2-{[2-(2-oxo-2,3-dihydro-1H-indol-
5.63
507.3
5-ylamino)-5-trifluoromethyl-pyrimidin-4-ylamino]-
methyl}-phenyl)-methanesulfonamide
5-[4-(Methyl-pyridin-3-ylmethyl-amino)-5-
5.25
415.4
trifluoromethyl-pyrimidin-2-ylamino]-1,3-dihydro-indol-2-
one
5-{4-[(1-Methanesulfonyl-piperidin-3-ylmethyl)-
5.69
499.4
methyl-amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-
1,3-dihydro-indol-2-one
5-[4-(Methyl-pyridin-4-ylmethyl-amino)-5-
5.12
415.3
trifluoromethyl-pyrimidin-2-ylamino]-1,3-dihydro-indol-2-
one
5-(4-Cyclopentylamino-5-trifluoromethyl-
6.47
378.3
pyrimidin-2-ylamino)-1,3-dihydro-indol-2-one
5-[4-(2,6-Dimethoxy-benzylamino)-5-
6.78
460.3
trifluoromethyl-pyrimidin-2-ylamino]-1,3-dihydro-indol-2-
one
5-{4-[(1,5-Dimethyl-1H-pyrazol-3-ylmethyl)-
4.99
418.3
amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-
dihydro-indol-2-one
5-[4-(2-Imidazol-1-yl-ethylamino)-5-
3.58
404.2
trifluoromethyl-pyrimidin-2-ylamino]-1,3-dihydro-indol-2-
one
5-{4-[(Pyridin-2-ylmethyl)-amino]-5-
4.95
401.4
trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-
one
5-[5-Trifluoromethyl-4-(2-trifluoromethyl-
6.57
468.2
benzylamino)-pyrimidin-2-ylamino]-1,3-dihydro-indol-2-
one
5-{4-[(3-Methyl-pyridin-2-ylmethyl)-amino]-5-
6.07
415.3
trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-
one
5-[4-(3-Methanesulfonyl-benzylamino)-5-
5.16
478.2
trifluoromethyl-pyrimidin-2-ylamino]-1,3-dihydro-indol-2-
one
5-{4-[2-(1-Acetyl-piperidin-2-yl)-ethylamino]-5-
5.22
463.4
trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-
one
5-{4-[2-(1-Propionyl-piperidin-2-yl)-ethylamino]-
5.65
477.4
5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-
2-one
5-{4-[2-(1-Cyclopropanecarbonyl-piperidin-2-yl)-
5.86
489.4
ethylamino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-
dihydro-indol-2-one
5-{4-[2-(1-Isobutyryl-piperidin-2-yl)-ethylamino]-
6.07
491.3
5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-
2-one
5-{4-[2-(1-Butyryl-piperidin-2-yl)-ethylamino]-5-
5.99
491.4
trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-
one
5-{4-[2-(1-Methoxyacetyl-piperidin-2-yl)-
5.19
493.4
ethylamino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-
dihydro-indol-2-one
5-{4-[2-(1-Cyclobutanecarbonyl-piperidin-2-yl)-
6.31
503.4
ethylamino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-
dihydro-indol-2-one
N-Methyl-N-{3-[2-(2-oxo-2,3-dihydro-1H-indol-5-
4.47
423.3
ylamino)-5-trifluoromethyl-pyrimidin-4-ylamino]-propyl}-
acetamide
N-Methyl-N-{3-[2-(2-oxo-2,3-dihydro-1H-indol-5-
4.89
437.45
ylamino)-5-trifluoromethyl-pyrimidin-4-ylamino]-propyl}-
propionamide
Cyclopropanecarboxylic acid methyl-{3-[2-(2-
5.07
449.3
oxo-2,3-dihydro-1H-indol-5-ylamino)-5-trifluoromethyl-
pyrimidin-4-ylamino]-propyl}-amide
N-Methyl-N-{3-[2-(2-oxo-2,3-dihydro-1H-indol-5-
5.24
451.3
ylamino)-5-trifluoromethyl-pyrimidin-4-ylamino]-propyl}-
isobutyramide
N-Methyl-N-{3-[2-(2-oxo-2,3-dihydro-1H-indol-5-
5.25
451.4
ylamino)-5-trifluoromethyl-pyrimidin-4-ylamino]-propyl}-
butyramide
2-Methoxy-N-methyl-N-{3-[2-(2-oxo-2,3-dihydro-
4.47
453.3
1H-indol-5-ylamino)-5-trifluoromethyl-pyrimidin-4-
ylamino]-propyl}-acetamide
Cyclobutanecarboxylic acid methyl-{3-[2-(2-oxo-
5.48
463.4
2,3-dihydro-1H-indol-5-ylamino)-5-trifluoromethyl-
pyrimidin-4-ylamino]-propyl}-amide
2,2,N-Trimethyl-N-{3-[2-(2-oxo-2,3-dihydro-1H-
5.80
465.3
indol-5-ylamino)-5-trifluoromethyl-pyrimidin-4-ylamino]-
propyl}-propionamide
2,N-Dimethyl-N-{3-[2-(2-oxo-2,3-dihydro-1H-
5.55
465.3
indol-5-ylamino)-5-trifluoromethyl-pyrimidin-4-ylamino]-
propyl}-butyramide
N-Methyl-N-{3-[2-(2-oxo-2,3-dihydro-1H-indol-5-
5.38
485.3
ylamino)-5-trifluoromethyl-pyrimidin-4-ylamino]-propyl}-
benzamide
Isoxazole-5-carboxylic acid methyl-{3-[2-(2-oxo-
4.91
476.2
2,3-dihydro-1H-indol-5-ylamino)-5-trifluoromethyl-
pyrimidin-4-ylamino]-propyl}-amide
Morpholine-4-carboxylic acid methyl-{3-[2-(2-
4.78
494.3
oxo-2,3-dihydro-1H-indol-5-ylamino)-5-trifluoromethyl-
pyrimidin-4-ylamino]-propyl}-amide
Ethanesulfonic acid methyl-{3-[2-(2-oxo-2,3-
5.29
473.3
dihydro-1H-indol-5-ylamino)-5-trifluoromethyl-pyrimidin-
4-ylamino]-propyl}-amide
Propane-1-sulfonic acid methyl-{3-[2-(2-oxo-2,3-
5.71
487.3
dihydro-1H-indol-5-ylamino)-5-trifluoromethyl-pyrimidin-
4-ylamino]-propyl}-amide
1,1,3-Trimethyl-3-{3-[2-(2-oxo-2,3-dihydro-1H-
5.53
488.3
indol-5-ylamino)-5-trifluoromethyl-pyrimidin-4-ylamino]-
propyl}-sulfonylurea
2,2,2-Trifluoro-N-methyl-N-{3-[2-(2-oxo-2,3-
5.80
477.2
dihydro-1H-indol-5-ylamino)-5-trifluoromethyl-pyrimidin-
4-ylamino]-propyl}-acetamide
N-Methyl-N-{2-[2-(2-oxo-2,3-dihydro-1H-indol-5-
4.23
409.2
ylamino)-5-trifluoromethyl-pyrimidin-4-ylamino]-ethyl}-
acetamide
N-Methyl-N-{2-[2-(2-oxo-2,3-dihydro-1H-indol-5-
4.61
423.2
ylamino)-5-trifluoromethyl-pyrimidin-4-ylamino]-ethyl}-
propionamide
Cyclopropanecarboxylic acid methyl-{2-[2-(2-
4.77
435.2
oxo-2,3-dihydro-1H-indol-5-ylamino)-5-trifluoromethyl-
pyrimidin-4-ylamino]-ethyl}-amide
N-Methyl-N-{2-[2-(2-oxo-2,3-dihydro-1H-indol-5-
4.94
437.2
ylamino)-5-trifluoromethyl-pyrimidin-4-ylamino]-ethyl}-
isobutyramide
N-Methyl-N-{2-[2-(2-oxo-2,3-dihydro-1H-indol-5-
4.95
437.2
ylamino)-5-trifluoromethyl-pyrimidin-4-ylamino]-ethyl}-
butyramide
2-Methoxy-N-methyl-N-{2-[2-(2-oxo-2,3-dihydro-
4.21
439.2
1H-indol-5-ylamino)-5-trifluoromethyl-pyrimidin-4-
ylamino]-ethyl}-acetamide
Cyclobutanecarboxylic acid methyl-{2-[2-(2-oxo-
5.17
449.3
2,3-dihydro-1H-indol-5-ylamino)-5-trifluoromethyl-
pyrimidin-4-ylamino]-ethyl}-amide
2,2,N-Trimethyl-N-{2-[2-(2-oxo-2,3-dihydro-1H-
5.57
451.4
indol-5-ylamino)-5-trifluoromethyl-pyrimidin-4-ylamino]-
ethyl}-propionamide
2,N-Dimethyl-N-{2-[2-(2-oxo-2,3-dihydro-1H-
5.26
451.4
indol-5-ylamino)-5-trifluoromethyl-pyrimidin-4-ylamino]-
ethyl}-butyramide
N-Methyl-N-{2-[2-(2-oxo-2,3-dihydro-1H-indol-5-
4.80
471.3
ylamino)-5-trifluoromethyl-pyrimidin-4-ylamino]-ethyl}-
benzamide
Isoxazole-5-carboxylic acid methyl-{2-[2-(2-oxo-
4.51
462.3
2,3-dihydro-1H-indol-5-ylamino)-5-trifluoromethyl-
pyrimidin-4-ylamino]-ethyl}-amide
Morpholine-4-carboxylic acid methyl-{2-[2-(2-
4.41
480.3
oxo-2,3-dihydro-1H-indol-5-ylamino)-5-trifluoromethyl-
pyrimidin-4-ylamino]-ethyl}-amide
N-Methyl-N-{2-[2-(2-oxo-2,3-dihydro-1H-indol-5-
4.77
445.1
ylamino)-5-trifluoromethyl-pyrimidin-4-ylamino]-ethyl}-
methanesulfonamide
Ethanesulfonic acid methyl-{2-[2-(2-oxo-2,3-
5.03
459.2
dihydro-1H-indol-5-ylamino)-5-trifluoromethyl-pyrimidin-
4-ylamino]-ethyl}-amide
Propane-1-sulfonic acid methyl-{2-[2-(2-oxo-2,3-
5.44
473.3
dihydro-1H-indol-5-ylamino)-5-trifluoromethyl-pyrimidin-
4-ylamino]-ethyl}-amide
1,1,3-Trimethyl-3-{2-[2-(2-oxo-2,3-dihydro-1H-
5.49
474.2
indol-5-ylamino)-5-trifluoromethyl-pyrimidin-4-ylamino]-
ethyl}-sulfonylurea
2,2,2-Trifluoro-N-methyl-N-{2-[2-(2-oxo-2,3-
5.49
463.2
dihydro-1H-indol-5-ylamino)-5-trifluoromethyl-pyrimidin-
4-ylamino]-ethyl}-acetamide
5-[4-(2-Hydroxy-ethylamino)-5-trifluoromethyl-
4.05
354.3
pyrimidin-2-ylamino]-1,3-dihydro-indol-2-one
5-(4-Cyclopropylamino-5-trifluoromethyl-
5.41
350.3
pyrimidin-2-ylamino)-1,3-dihydro-indol-2-one
5-(4-Cyclobutylamino-5-trifluoromethyl-
6.01
364.3
pyrimidin-2-ylamino)-1,3-dihydro-indol-2-one
5-[4-(1,4-Dimethyl-pentylamino)-5-
7.45
408.4
trifluoromethyl-pyrimidin-2-ylamino]-1,3-dihydro-indol-2-
one
5-[4-(3-Imidazol-1-yl-propylamino)-5-
3.77
418.3
trifluoromethyl-pyrimidin-2-ylamino]-1,3-dihydro-indol-2-
one
5-[4-(2-Phenoxy-ethylamino)-5-trifluoromethyl-
6.34
430.3
pyrimidin-2-ylamino]-1,3-dihydro-indol-2-one
5-[4-(1-Cyclohexyl-ethylamino)-5-trifluoromethyl-
7.61
420.4
pyrimidin-2-ylamino]-1,3-dihydro-indol-2-one
5-[4-(1-Hydroxymethyl-2,2-dimethyl-
5.64
410.4
propylamino)-5-trifluoromethyl-pyrimidin-2-ylamino]-1,3-
dihydro-indol-2-one
5-[4-(1-Methoxymethyl-propylamino)-5-
5.96
396.3
trifluoromethyl-pyrimidin-2-ylamino]-1,3-dihydro-indol-2-
one
5-[4-(Indan-2-ylamino)-5-trifluoromethyl-
6.78
426.4
pyrimidin-2-ylamino]-1,3-dihydro-indol-2-one
5-[4-(1,2,3,4-Tetrahydro-naphthalen-1-ylamino)-
7.16
440.3
5-trifluoromethyl-pyrimidin-2-ylamino]-1,3-dihydro-indol-
2-one
5-(4-Cycloheptylamino-5-trifluoromethyl-
7.21
406.3
pyrimidin-2-ylamino)-1,3-dihydro-indol-2-one
5-{4-[2-(2-Oxo-imidazolidin-1-yl)-ethylamino]-5-
4.04
422.3
trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-
one
4-[2-(2-Oxo-2,3-dihydro-1H-indol-5-ylamino)-5-
5.65
424.2
trifluoromethyl-pyrimidin-4-ylamino]-butyric acid ethyl
ester
5-[4-(2-Hydroxy-1-hydroxymethyl-ethylamino)-5-
3.72
384.2
trifluoromethyl-pyrimidin-2-ylamino]-1,3-dihydro-indol-2-
one
5-[4-(3-Hydroxy-2,2-dimethyl-propylamino)-5-
5.09
396.3
trifluoromethyl-pyrimidin-2-ylamino]-1,3-dihydro-indol-2-
one
5-{4-[(Isochroman-1-ylmethyl)-amino]-5-
6.36
456.3
trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-
one
5-[4-(4-Hydroxy-1,1-dioxo-tetrahydro-1&-
4.42
442.2
thiophen-3-ylamino)-5-trifluoromethyl-pyrimidin-2-
ylamino]-1,3-dihydro-indol-2-one
5-[4-(2-Methoxy-1-methyl-ethylamino)-5-
5.58
382.3
trifluoromethyl-pyrimidin-2-ylamino]-1,3-dihydro-indol-2-
one
5-[4-(trans-4-Methylsulfanyl-tetrahydro-furan-3-
5.37
426.3
ylamino)-5-trifluoromethyl-pyrimidin-2-ylamino]-1,3-
dihydro-indol-2-one
5-{4-[trans-2-(Pyrimidin-2-ylsulfanyl)-
6.32
488.3
cyclopentylamino]-5-trifluoromethyl-pyrimidin-2-
ylamino}-1,3-dihydro-indol-2-one
5-[4-(Indan-1-ylamino)-5-trifluoromethyl-
6.86
426.3
pyrimidin-2-ylamino]-1,3-dihydro-indol-2-one
5-{4-[2-(2-Hydroxy-ethylsulfanyl)-ethylamino]-5-
4.66
414.3
trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-
one
5-{4-[2-(Pyridin-3-yloxy)-propylamino]-5-
5.20
445.3
trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-
one
5-{4-[2-(6-Methyl-pyridin-2-yl)-ethylamino]-5-
5.00
429.3
trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-
one
5-{4-[(2,3-Dihydro-benzo[1,4]dioxin-2-ylmethyl)-
5.01
458.2
amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-
dihydro-indol-2-one
5-{4-[(1-Methyl-1H-pyrazol-4-ylmethyl)-amino]-5-
4.60
404.3
trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-
one
5-{4-[(4,5,6,7-Tetrahydro-benzothiazol-2-
5.93
461.2
ylmethyl)-amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-
1,3-dihydro-indol-2-one
5-[4-(1-Phenyl-3-[1,2,4]triazol-1-yl-propylamino)-
5.24
495.2
5-trifluoromethyl-pyrimidin-2-ylamino]-1,3-dihydro-indol-
2-one
5-(4-Isobutylamino-5-trifluoromethyl-pyrimidin-2-
6.12
366.4
ylamino)-1,3-dihydro-indol-2-one
5-[4-(2-Cyclohexyl-1-hydroxymethyl-
6.41
450.4
ethylamino)-5-trifluoromethyl-pyrimidin-2-ylamino]-1,3-
dihydro-indol-2-one
2-[2-(2-Oxo-2,3-dihydro-1H-indol-5-ylamino)-5-
5.26
396.3
trifluoromethyl-pyrimidin-4-ylamino]-propionic acid
methyl ester
5-(4-Cyclohexylamino-5-trifluoromethyl-
6.82
392.3
pyrimidin-2-ylamino)-1,3-dihydro-indol-2-one
5-[4-(3-Hydroxy-propylamino)-5-trifluoromethyl-
4.24
368.3
pyrimidin-2-ylamino]-1,3-dihydro-indol-2-one
5-{4-[2-(4-Methyl-1H-imidazol-2-yl)-ethylamino]-
3.54
418.3
5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-
2-one
5-[4-(Tetrahydro-furan-3-ylamino)-5-
4.89
380.3
trifluoromethyl-pyrimidin-2-ylamino]-1,3-dihydro-indol-2-
one
5-[4-(Dicyclopropylmethyl-amino)-5-
6.59
404.3
trifluoromethyl-pyrimidin-2-ylamino]-1,3-dihydro-indol-2-
one
5-{4-[2-(5-Methyl-4H-[1,2,4]triazol-3-yl)-
4.00
419.3
ethylamino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-
dihydro-indol-2-one
5-[4-(2-Ethylsulfanyl-ethylamino)-5-
5.99
398.3
trifluoromethyl-pyrimidin-2-ylamino]-1,3-dihydro-indol-2-
one
5-[4-(2-Phenoxy-propylamino)-5-trifluoromethyl-
6.57
444.2
pyrimidin-2-ylamino]-1,3-dihydro-indol-2-one
5-{4-[(1-Ethyl-5-oxo-pyrrolidin-3-ylmethyl)-
4.57
435.2
amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-
dihydro-indol-2-one
5-(4-{[1-(2-Methoxy-ethyl)-5-oxo-pyrrolidin-3-
4.44
465.2
ylmethyl]-amino}-5-trifluoromethyl-pyrimidin-2-ylamino)-
1,3-dihydro-indol-2-one
5-[4-(Benzhydryl-amino)-5-trifluoromethyl-
7.26
476.2
pyrimidin-2-ylamino]-1,3-dihydro-indol-2-one
5-{4-[2-(1-Methyl-1H-pyrazol-4-yl)-ethylamino]-
4.90
418.3
5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-
2-one
5-{4-[(4-Methyl-1H-imidazol-2-ylmethyl)-amino]-
3.40
404.2
5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-
2-one
5-{4-[(5-Cyclopropyl-1H-pyrazol-3-ylmethyl)-
5.00
430.2
amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-
dihydro-indol-2-one
5-{4-[2-(4-Methyl-thiazol-5-yl)-ethylamino]-5-
5.18
435.2
trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-
one
5-{4-[2-(1H-Benzoimidazol-2-yl)-ethylamino]-5-
4.39
454.2
trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-
one
5-{4-[(5-Methyl-[1,3,4]oxadiazol-2-ylmethyl)-
4.25
406.3
amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-
dihydro-indol-2-one
5-{4-[(5-Phenyl-4H-[1,2,4]triazol-3-ylmethyl)-
4.92
467.3
amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-
dihydro-indol-2-one
5-{4-[(1H-Indol-2-ylmethyl)-amino]-5-
6.10
439.3
trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-
one
5-{4-[(1,5-Dimethyl-1H-pyrazol-4-ylmethyl)-
4.77
418.3
amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-
dihydro-indol-2-one
5-{4-[(Benzothiazol-2-ylmethyl)-amino]-5-
5.77
457.2
trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-
one
5-{4-[(3-Methyl-isoxazol-5-ylmethyl)-amino]-5-
5.02
405.3
trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-
one
5-{4-[(4-Methyl-thiazol-2-ylmethyl)-amino]-5-
5.12
421.2
trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-
one
5-{4-[1-(4-Methyl-thiazol-2-yl)-ethylamino]-5-
5.62
435.2
trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-
one
5-{5-Trifluoromethyl-4-[(1,3,5-trimethyl-1H-
4.95
432.2
pyrazol-4-ylmethyl)-amino]-pyrimidin-2-ylamino}-1,3-
dihydro-indol-2-one
5-{4-[1-(2-Methyl-thiazol-4-yl)-ethylamino]-5-
5.69
435.3
trifluoromethyl-pyrimidin-2-ylamino}-1,3-dihydro-indol-2-
one
5-{4-[(3-Methyl-imidazo[2,1-b]thiazol-6-
5.03
460.3
ylmethyl)-amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-
1,3-dihydro-indol-2-one
5-{4-[1-(5-Methyl-4H-[1,2,4]triazol-3-yl)-
4.20
419.3
ethylamino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-
dihydro-indol-2-one
5-{4-[1-(3,5-Dimethyl-1H-pyrazol-4-yl)-
5.02
432.3
ethylamino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-
dihydro-indol-2-one
5-{4-[2-(3,5-Dimethyl-1H-pyrazol-4-yl)-
4.85
432.4
ethylamino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-
dihydro-indol-2-one
5-{4-[2-(4,6-Dimethyl-pyrimidin-2-yl)-
5.17
444.4
ethylamino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-
dihydro-indol-2-one
5-{4-[2-(4-Methyl-5,6,7,8-tetrahydro-quinazolin-
5.88
484.4
2-yl)-ethylamino]-5-trifluoromethyl-pyrimidin-2-ylamino}-
1,3-dihydro-indol-2-one
5-[4-(2-Thiazol-4-yl-ethylamino)-5-
5.18
421.3
trifluoromethyl-pyrimidin-2-ylamino]-1,3-dihydro-indol-2-
one
5-(4-Dimethylamino-5-trifluoromethyl-pyrimidin-
5.60
338.3
2-ylamino)-1,3-dihydro-indol-2-one
5-{4-[(1-Pyrimidin-2-yl-piperidin-3-ylmethyl)-
6.17
485.4
amino]-5-trifluoromethyl-pyrimidin-2-ylamino}-1,3-
dihydro-indol-2-one
5-[4-(Indan-1-ylamino)-5-trifluoromethyl-
6.85
426.3
pyrimidin-2-ylamino]-1,3-dihydro-indol-2-one
The present invention is not to be limited in scope by the specific embodiments described herein. Indeed, various modifications of the invention in addition to those described herein will become apparent to those skilled in the art from the foregoing description and the accompanying figures. Such modifications are intended to fall within the scope of the appended claims.
All patents, applications, publications, test methods, literature, and other materials cited herein are hereby incorporated herein by reference in their entireties.
|
The present invention relates to a compound of the formula 1
wherein R 1 -R 4 are as defined herein. Such novel pyrimidine derivatives are useful in the treatment of abnormal cell growth, such as cancer, in mammals. This invention also relates to a method of using such compounds in the treatment of abnormal cell growth in mammals, especially humans, and to pharmaceutical compositions containing such compounds.
| 2
|
PRIORITY DATA
[0001] This application is a continuation-in-part of co-pending U.S. application Ser. No. 09/891,206, filed Jun. 26, 2001, which claims priority to United Kingdom Application Serial No. 0015745.3, filed Jun. 27, 2000. Each of the above applications are incorporated by reference herein in their entirety.
BRIEF DESCRIPTION OF THE INVENTION
[0002] This invention relates to the treatment and prevention of bone diseases, to methods of enhancing bone formation and also to the treatment of bone fracture with a combination of a lanthanum compound and a bone enhancing agent, such as vitamin D.
BACKGROUND OF THE INVENTION
[0003] Throughout life, old bone is continuously removed by bone-resorbing osteoclasts and replaced with new bone which is formed by osteoblasts. This cycle is called the bone-remodeling cycle and is normally highly regulated, i.e. the functioning of osteoclasts and osteoblasts is linked such that in a steady state the same amount of bone is formed as is resorbed.
[0004] The bone-remodeling cycle occurs at particular areas on the surfaces of bones. Osteoclasts which are formed from appropriate precursor cells within bones resorb portions of bone; new bone is then generated by osteoblastic activity. Osteoblasts synthesise the collagenous precursors of bone matrix and also regulate its mineralization. The dynamic activity of osteoblasts in the bone remodeling cycle to meet the requirements of skeletal growth and matrix and also regulate its maintenance and mechanical function is thought to be influenced by various factors, such as hormones, growth factors, physical activity and other stimuli. Osteoblasts are thought to have receptors for parathyroid hormone and estrogen. Ostoeclasts adhere to the surface of bone undergoing resorption and are thought to be activated by some form of signal from osteoblasts.
[0005] Irregularities in one or more stages of the bone-remodeling cycle (e.g. where the balance between bone formation and resorption is lost) can lead to bone remodeling disorders, or metabolic bone diseases. Examples of such diseases are osteoporosis, Paget's disease and rickets. Some of these diseases are caused by over-activity of one half of the bone-remodeling cycle compared with the other, i.e. by osteoclasts or osteoblasts. In osteoporosis, for example, there is a relative increase in osteoclastic activity which may cause a reduction in bone density and mass. Osteoporosis is the most common of the metabolic bone diseases and may be either a primary disease or may be secondary to another disease or other diseases.
[0006] Post-menopausal osteoporosis is currently the most common form of osteoporosis. Senile osteoporosis afflicts elderly patients of either sex and younger individuals occasionally suffer from osteoporosis.
[0007] Osteoporosis is characterised generally by a loss of bone density. Thinning and weakening of the bones leads to increased fracturing from minimal trauma. The most prevalent fracturing in post-menopausal osteoporotics is of the wrist and spine. Senile osteoporosis, is characterised by a higher than average fracturing of the femur.
[0008] Whilst osteoporosis as a therapeutic target has been of, and continues to, attract a great deal of interest, tight coupling between the osteoblastic and osteoclastic activities of the bone remodeling cycle make the replacement of bone already lost an extremely difficult challenge. Consequently, research into treatments for prevention or prophylaxis of osteoporosis (as opposed to replacement of already-lost bone) has yielded greater results to date.
[0009] Oestrogen deficiency has been considered to be a major cause of post-menopausal osteoporosis. Indeed steroids including oestrogen have been used as therapeutic agents ( New Eng. J Med., 303, 1195 (1980)). However, recent studies have concluded that other causes must exist (J. Clin. Invest., 77, 1487 (1986)).
[0010] Other bone diseases can be caused by an irregularity in the bone-remodeling cycle whereby both increased bone resorption and increased bone formation occur. Paget's disease is one such example.
[0011] Lanthanum has been of prominence previously in medicine on account of its property of forming stable complexes with phosphate. This application has been evidenced in the treatment of hyperphosphataemia by application of lanthanum carbonate. U.S. Pat. No. 5,968,976 describes the preparation and use in a pharmaceutical composition of certain hydrates of lanthanum carbonate for the treatment of hyperphosphataemia.
[0012] Fernandez-Gavarron et al. ( Bone and Mineral, 283-291 (1988)) report on studies into the incorporation of 140-lanthanum into bones teeth and hydroxyapatite in vitro. Whilst the depth of uptake varied from an estimated 5 to 15 μm (dependent on experimental conditions), the authors' conclusion was that an exchange of lanthanum for calcium in hydroxyapatite may provide for increased resistance to acidic induced dissolution. Based on this suggested increased acid-resistance, the authors suggest that lanthanum's clinical usefulness as an adjunct in treating diseases such as osteoporosis, root caries and alveolar bone resorption might be explored.
[0013] Vijai S.Shankar et al. (Biochemical and Biophysical Research Communications, 907-912 (1992)) report that extracellular application of Lanthanum (III) induced a concentration-dependant elevation of cytosolic calcium in osteoclasts. The authors suggested that the osteoclast calcium receptor may be sensitive to activation and inactivation by the trivalent cation lanthanum.
[0014] Bernd Zimmermann et al. (European Journal of Cell Biology, 114-121 (1994)) report that lanthanum inhibited endochondral mineralization and reduced calcium accumulation in organoid cultures of limb bud mesodermal cells.
SUMMARY OF THE INVENTION
[0015] We have surprisingly found that lanthanum (III) compounds enhance bone formation and bone density and have beneficial effects on the activity and differentiation of bone cells.
[0016] Accordingly, the present invention relates to a method for enhancing bone formation in a mammal in need thereof comprising administering to the mammal an effective amount of a lanthanum compound, preferably lanthanum (III). In accordance with an embodiment of the invention the mammal is a human. The human may have a bone deficit or be at risk of developing a bone deficit. The invention also contemplates that the human has a bone remodeling disorder or is at risk of developing such disorder. Examples of bone remodeling disorders include osteoporosis, Paget's disease, osteoarthritis, rheumatoid arthritis, achondroplasia, osteochodrytis, hyperparathyroidism, osteogenesis imperfecta, congenital hypophosphatasia, fribromatous lesions, fibrous displasia, multiple myeloma, abnormal bone turnover, osteolytic bone disease and periodontal disease.
[0017] In an embodiment the bone remodeling disorder is osteoporosis, including primary osteoporosis, secondary osteoporosis, post-menopausal osteoporosis, male osteoporosis and steroid induced osteoporosis.
[0018] Also provided is a method for enhancing bone formation in a mammal having a bone deficit which does not result from a bone remodeling disorder. Such bone deficits may result, for example, from a bone fracture, bone trauma, or a condition associated with post-traumatic bone surgery, post-prosthetic joint surgery, post-plastic bone surgery, post-dental surgery, bone chemotherapy treatment or bone radiotherapy treatment.
[0019] In an embodiment of the methods of the invention the lanthanum (III) compound is lanthanum chloride, lanthanum carbonate, lanthanum salts, chelates or derivatives thereof, lanthanum resins or lanthanum absorbants.
[0020] In a further embodiment of the methods of the invention, the effective amount of lanthanum (III) compound is from 0.01 mg/Kg/Day to 100 mg/Kg/Day, preferably from 0.05 mg/Kg/Day to 50 mg/Kg/Day or from 0.1 mg/Kg/Day to 10 mg/Kg/Day.
[0021] The present invention also provides a method for increasing bone density in a mammal in need thereof comprising administering to said mammal an effective amount of a lanthanum (III) compound. Also provided is a method for stimulating osteoblast differentiation by contacting the osteoblasts with an effective amount of lanthanum (III) compound thereby stimulating differentiation. Still further is provided a method for inhibiting osteoclast differentiation by contacting osteoclasts with an effective amount of lanthanum (III) compound thereby inhibiting differentiation.
[0022] In a further embodiment, the invention provides a method for activating the bone formation activity of differentiated osteoblasts by contacting the osteoblasts with an effective amount of lanthanum (III) compound thereby stimulating bone formation. The invention also contemplates a method for simultaneously stimulating osteoblast differentiation and inhibiting osteoclast differentiation in a mammal having a bone remodeling disorder, or being at risk of developing a bone remodeling disorder, by administering to the mammal an effective amount of lanthanum (III) compound.
[0023] The invention also contemplates a method for enhancing bone formation in a mammal in need thereof by administering to the mammal an effective amount of a lanthanum (III) compound and at least one bone enhancing agent. Examples of suitable bone enhancing agents include a synthetic hormone, a natural hormone, oestrogen, calcitonin, tamoxifen, a bisphosphonate, a bisphosphonate analog, vitamin D, a vitamin D analog, a mineral supplement, a statin drug, a selective oestrogen receptor modulator and sodium fluoride.
[0024] The invention further contemplates the use of a lanthanum III compound for the preparation of a medicament for use in enhancing bone formation in a mammal in need thereof. In an embodiment the mammal is a human having a bone remodeling disorder or being at risk of developing such disorder. In a further embodiment, the invention contemplates a pharmaceutical composition for the treatment or prevention of a bone remodeling disorder comprising a lanthanum (III) compound and a bone enhancing agent.
[0025] The present inventors have also found that lanthanum compounds may be used to inhibit selectively osteoclast differentiation. At certain low concentrations osteoblast differentiation may be activated and increased bone formation may result from the manifestation of either or both of these phenomena.
[0026] According to one aspect of the invention, there is thus provided a method for inhibiting osteoclastic differentiation whereby to manage, treat or achieve prophylaxis of bone disease which comprises administering to a human or animal subject suffering from, or susceptible to bone disease a therapeutically or prophylactically effective amount of a lanthanum compound.
[0027] Viewed from a further aspect there is provided a method for activating osteoblastic differentiation whereby to manage, treat or achieve prophylaxis of bone disease which comprises administering to a human or animal subject suffering from, or susceptible to bone disease a therapeutically or prophylactically effective amount of a lanthanum compound.
[0028] In this text, “susceptible to bone disease” is intended to embrace a higher than average predisposition towards developing bone disease. As an example, those susceptible towards osteoporosis include post-menopausal women, elderly males (e.g. those over the age of 65) and those being treated with drugs known to cause osteoporosis as a side-effect (e.g. steroid-induced osteoporosis).
[0029] According to a still further aspect of the invention there is provided the use of a lanthanum compound for the preparation of a medicament for use in any method of the invention.
[0030] According to a yet further aspect of the invention there is provided the use of a lanthanum compound in any method of the invention.
[0031] According to a yet further aspect of the invention there is provided the use of a lanthanum compound for the preparation of a pharmaceutical composition for use in the diagnosis of bone disease or of bone fracture.
[0032] These and other aspects of the invention will become evident upon reference to the following detailed description and attached drawings. In addition reference is made herein to various publications which are hereby incorporated by reference in their entirety.
BRIEF DESCRIPTION OF THE DRAWINGS
[0033] The invention will be better understood by reference to the following drawings in which:
[0034] FIG. 1 is a bar graph showing the combined results of the effect of LA on bone resoption, where the bars represent the relative medium CrossLaps amounts per osteoclast±SD at different lanthanum concentrations;
[0035] FIG. 2 is a bar graph showing the combined results of the effect of LA on osteoclast differentiation, where the bars represent the relative TRAP 5b activities±SD at different lanthanum concentrations;
[0036] FIG. 3 is a bar graph showing the combined results of the effect of LA on osteoblast differentiation, where the bars represent relative specific activities of cellular alkaline phosphatase±SD at different lanthanum concentrations; and
[0037] FIG. 4 is a bar graph showing the combined results of the effect of LA on bone formation activity of mature osteoblasts, where the bars represent the amount of calcium released (mmol/L) from the bone nodules after HC1 extraction. ±SD at different lanthanum concentrations.
DETAILED DESCRIPTION OF THE INVENTION
[0038] As hereinbefore mentioned, the present invention provides a method for enhancing bone formation in a mammal in need thereof comprising administering to said mammal an effective amount of a lanthanum compound, preferably a lanthanum (III) compound, in combination with a bone enhancing agent or agents.
[0039] Bone formation, or osteogenesis, refers to the creation of new bone mass. This includes the process whereby new bone structure grows or the density of existing bone is increased. Osteoblasts form bone by producing extracellular organic matrix, or osteoid and then mineralizing the matrix to form bone. The main mineral component of bone is crystalline hydroxyapetite, which comprises much of the mass of normal adult bone.
[0040] As disclosed in parent application Ser. No. 09/891,206, the inventors have surprisingly found that lanthanum compounds significantly enhance bone formation in vitro and in vivo. Enhanced bone formation in vitro was observed when lanthanum (III) was added to cultures of mature osteoblasts in vitro at concentrations of from 100 to 15,000 ng/ml. Enhanced bone formation was quantitated by measuring the amount of calcium incorporated into bone nodules formed by the osteoblasts.
[0041] The present inventors have also found that lanthanum (III) enhanced bone formation in growing dogs. A dose of 2,000 mg/kg/day lanthanum enhanced bone formation and produced a significant increase in bone volume and density compared to control animals.
[0042] Lanthanum (III) compounds may be used in the methods of the invention to enhance bone formation in a range of mammals, including domestic animals, such as pigs, cattle, horses, sheep and goats and also including pets and experimental mammals, such as dogs, cats and rodents.
[0043] In an embodiment of the invention the mammal is a human in need of enhanced bone formation. In one aspect, the human in need has a bone deficit, which means that they will have less bone than desirable or that the bone will be less dense or strong than desired. A bone deficit may be localized, such as that caused by a bone fracture or systemic, such as that caused by osteoporosis. Bone deficits may result from a bone remodeling disorder whereby the balance between bone formation and bone resorption is shifted, resulting in a bone deficit. Examples of such bone remodeling disorders include osteoporosis, Paget's disease, osteoarthritis, rheumatoid arthritis, achondroplasia, osteochodrytis, hyperparathyroidism, osteogenesis imperfecta, congenital hypophosphatasia, fribromatous lesions, fibrous displasia, multiple myeloma, abnormal bone turnover, osteolytic bone disease and periodontal disease. Bone remodeling disorders include metabolic bone diseases which are characterised by disturbances in the organic matrix, bone mineralization, bone remodeling, endocrine, nutritional and other factors which regulate skeletal and mineral homeostasis. Such disorders may be hereditary or acquired and generally are systemic affecting the entire skeletal system.
[0044] Thus, in one aspect the human may have a bone remodeling disorder. Bone remodeling as used herein refers to the process whereby old bone is being removed and new bone is being formed by a continuous turnover of bone matrix and mineral that involves bone resorption by osteoclasts and bone formation by osteoblasts.
[0045] Osteoporosis is a common bone remodeling disorder characterised by a decrease in bone density of normally mineralised bone, resulting in thinning and increased porosity of bone cortices and trabeculae. The skeletal fragility caused by osteoporosis predisposes sufferers to bone pain and an increased incidence of fractures. Progressive bone loss in this condition may result in a loss of up to 50% of the initial skeletal mass.
[0046] Primary osteoporosis includes idiopathic osteoporosis which occurs in children or young adults with normal gonadal function, Type I osteoporosis, also described as post-menauposal osteoporosis, and Type II osteoporosis, senile osteoporosis, occurs mainly in those persons older than 70 years of age. Causes of secondary osteoporosis may be endocrine (e.g. glucocorticoid excess, hyperparathyroidism, hypoganodism), drug induced (e.g. corticosteroid, heparin, tobaco) or otherwise (e.g. chronic renal failure, hepatic disease and malabsorbtion syndrome osteoporosis). The phrase “at risk of developing a bone deficit”; as used herein, is intended to embrace mammals and humans having a higher than average predisposition towards developing a bone deficit. As an example, those susceptible towards osteoporosis include post-menopausal women, elderly males (e.g. those over the age of 65) and those being treated with drugs known to cause osteoporosis as a side-effect (e.g. steroid-induced osteoporosis). Certain factors are well known in the art which may be used to identify those at risk of developing a bone deficit due to bone remodeling disorders like osteoporosis. Important factors include low bone mass, family history, life style, estrogen or androgen deficiency and negative calcium balance. Postmenopausal women are particularly at risk of developing osteoporosis. Hereinafter, references to treatment of bone diseases are intended to include management and/or prophylaxis except where the context demands otherwise.
[0047] The methods of the invention may also be used to enhance bone formation in conditions where a bone deficit is caused by factors other than bone remodeling disorders. Such bone deficits include fractures, bone trauma, conditions associated with post-traumatic bone surgery, post-prosthetic joint surgery, post plastic bone surgery, post dental surgery, bone chemotherapy, post dental surgery and bone radiotherapy. Fractures include all types of microscopic and macroscopic fractures. Examples of fractures includes avulsion fracture, comminuted fracture, transverse fracture, oblique fracture, spiral fracture, segmental fracture, displaced fracture, impacted fracture, greenstick fracture, torus fracture, fatigue fracture, intraarticular fracture (epiphyseal fracture), closed fracture (simple fracture), open fracture (compound fracture) and occult fracture.
[0048] As previously mentioned, a wide variety of bone diseases may be treated in accordance with the present invention, for example all those bone diseases connected with the bone-remodeling cycle. Examples of such diseases include all forms of osteoporosis, osteomalacia, rickets and Paget's disease. Osteoporosis, especially of the post-menopausal, male and steroid-induced types, is of particular note. In addition, lanthanum compounds find use as antiresorption agents generally, as bone promotion agents and as anabolic bone agents. Such uses form another aspect of the present invention.
[0049] The present inventors have surprisingly found that lanthanum stimulates osteoblast differentiation. Osteoblast differentiation was measured in vitro cultures of bone marrow derived osteoprogenitor cells, which are capable of proliferating and differentiating into mature osteoblasts, capable of forming mineralised bone nodules. Differentation was measured by determining the specific activities of intracellular alkaline phosphatase. Low doses of lanthanum (100 ng/ml) were found to stimulate osteoblast differentiation.
[0050] The present inventors have also surprisingly found that lanthanum inhibits osteoclast differentiation in vitro, as measured by a decrease in TRAP (Tartrate-Resistant acid phosphatase) positive multinucleate cells in mouse bone marrow culture compared to control cultures. In many bone remodeling disorders, including osteoporosis, the bone deficit may be attributed to excess bone resorption by differentiated osteoclasts. The methods and compositions of the invention may be employed to inhibit osteoclast differentiation, thus inhibiting bone resorption. Some inhibition of bone resorption was found in vitro.
[0051] Low doses of lanthanum have thus been found to both enhance bone formation and stimulate osteoblast differentiation and also to inhibit osteoclast differentiation and bone resorption.
[0052] A range of lanthanum compounds may be used in the methods and compositions of the invention, preferably lanthanum (III) in a form that is bioavailable. Preferred lanthanum compounds include, for example, lanthanum salts and derivatives thereof, lanthanum resins and lanthanum absorbants. The lanthanum compound may, if desired, be in the form of a chelate. Examples of suitable lanthanum salts include lanthanum carbonate, lanthanum carbonate hydrate, lanthanum chloride.
[0053] An effective amount of lanthanum for use in the present invention is an amount of lanthanum (III)compound that will provide the desired benefit or therapeutic effect upon administration according to the prescribed regimen. Nonlimiting examples of an effective amount of lanthanum may range from about 0.01 mg/kg/day to about 100 mg/kg/day, preferably from about 0.05 mg/kg/day to about 50 mg/kg/day and more preferably from about 0.1 mg/kg/day to about 10 mg/kg/day.
[0054] The lanthanum compound orally administered to subjects in accordance with this invention is suitably administered in unit dosages varying from about 125 to about 1000 mg as elemental lanthanum. A typical dosage for an adult can be, e.g., 375 mg-6000 mg daily. More preferably, the dosage is 375-3750 mg/day.
[0055] The dose may also be selected to provide an effective plasma concentration of lanthanum ion.
[0056] Examples of an effective plasma concentration of lanthanum ion may range from about 0.1 ng/ml to about 1,000 ng/ml, preferably from about 1 ng/ml to about 500 ng/ml, more preferably from about 1 ng/ml to about 100 ng/ml.
[0057] The dose may further be selected to provide an effective level of lanthanum in and around the bone surface.
[0058] Examples of effective amounts in and around the major bone surfaces may range from 0.1 μg/g to 500 μg/g, preferably from 0.5 μg/g to 100 μg/g, more preferably from 1 μg/g to 25 μg/g.
[0059] The term “lanthanum compound” is used herein to denote any pharmacologically acceptable lanthanum compound capable of ensuring that the lanthanum is bioavailable. Preferred compounds include, for example, lanthanum salts and derivatives thereof, lanthanum resins and lanthanum absorbants. The lanthanum may if desired be in the form of a chelate. Hereinafter, the invention will be described with specific reference to certain lanthanum salts and derivatives.
[0060] In accordance with the present invention, the lanthanum compound is administered with a bone enhancing agent or agents. Bone enhancing agents are known in the art to increase bone formation, bone density or bone mineralisation, or to prevent bone resorption. Suitable bone enhancing agents include natural or synthetic hormones, such as estrogens, androgens, calcitonin, prostaglandins and parathormone; growth factors, such as platelet-derived growth factor, insulin-like growth factor, transforming growth factor, epidermal growth factor, connective tissue growth factor and fibroblast growth factor; vitamins, particularly vitamin D; minerals, such as calcium, aluminum, strontium and fluoride; statin drugs, including pravastatin, fluvastatin, simvastatin, lovastatin and atorvastatin; agonists or antagonist of receptors on the surface of osteoblasts and osteoclasts, including parathormone receptors, estrogen receptors and prostaglandin receptors; bisphosphonates and anabolic bone agents.
[0061] In one embodiment of the present invention, the lanthanum compound, in combination with vitamin D or an analog of vitamin D, is administered to a subject. Levels of 25-hydroxy vitamin D 2 are low at values less than about 16 ng/mL and replacement treatment aims for levels of greater than or equal to about 16 ng/mL. Levels of 1,25-dihydroxy vitamin D 2 are low at values less than about 22 pg/mL and replacement treatment aims for levels of greater than about 22 pg/mL.
[0062] Examples of vitamin D sources which may be so administered concurrently with the lanthanum compound in this invention include 1,25 dihydroxy-vitamin D, the active metabolite of vitamin D (calcitriol, rocalcitrol). Examples of suitable vitamin D analogs include doxercalciferol (Hectorol®, available from Bone Care International, Middleton, Wis.), and paricalcitol (Zemplar®, available from Abbott Laboratories, Abbott Park, Ill.).
[0063] A pharmaceutical composition can contain up to about 1 mg of 25-hydroxy vitamin D 2 or 1,25-dihydroxy vitamin D 2 . A pharmaceutical composition can also contain vitamin D 2 or vitamin D 3 in an amount up to 800 IU (where, e.g., vitamin D 2 is 850,000 IU/gram and vitamin D 3 is 100,000 IU/gram).
[0064] The lanthanum compounds/bone enhancing agents of the invention may be administered in the form of a pharmaceutical composition comprising the active ingredients in admixture or association with a pharmaceutically acceptable carrier or diluent. The active ingredients may be formulated into a composition suitable for administration by any convenient route, e.g. orally (including sublingually), topically, parenterally (including intravenous, intramuscular, intraperitoneal and subcutaneous administration) and rectally, oral administration being preferred. It should be understood, however, that the invention embraces all forms of administration which make the lanthanum compound and bone enhancing agent(s) systemically or locally available. Orally administrable compositions may, if desired, contain one or more physiologically compatible carriers and/or excipients and may be solid or liquid. The compositions may take any convenient form including, for example, tablets, coated tablets, capsules, lozenges, aqueous or oily suspensions, solutions, emulsions, syrups, elixirs and dry products suitable for reconstitution with water or another suitable liquid vehicle before use. The compositions may advantageously be prepared in unit dosage form. Tablets and capsules according to the invention may, if desired, contain conventional ingredients such as binding agents, for example syrup, acacia, gelatin, sorbitol, tragacanth or polyvinyl-pyrollidone; fillers, for example lactose, sugar, maize starch, calcium phosphate, sorbitol or glycine; lubricants, for example magnesium stearate, talc, polyethylene glycol or silica; disintegrants, for example potato starch; or acceptable wetting agents such as sodium lauryl sulphate. Tablets may be coated according to methods well known in the art.
[0065] Furthermore, dextrates can be an ingredient in a composition of the instant invention. The term “dextrates” as used herein refers to a purified mixture of saccharides that is mostly dextrose (e.g., not less than about 93.0% and not more than about 99.0%, calculated on the dried basis) and that results from a controlled enzymatic hydrolysis of starch. Dextrates can be either anhydrous or hydrated. “Dextrates” can refer to dextrates as defined its official monograph found in National Formulary 21 (printed by Webcom Limited in Toronoto, Cnada; 2003). Dextrates are available from JRS Pharma (Patterson, N.Y.) as Emdex®.
[0066] Liquid compositions may contain conventional additives such as suspending agents, for example sorbitol syrup, methyl cellulose, glucose/sugar syrup, gelatin, hydroxymethylcellulose, carboxymethylcellulose, aluminium stearate gel or hydrogenated edible fats; emulsifying agents, for example lecithin, sorbitan monooleate or acacia; non-aqueous vehicles, which may include edible oils, for example vegetable oils such as arachis oil, almond oil, fractionated coconut oil, fish-liver oils, oily esters such as polysorbate 80, propylene glycol, or ethyl alcohol; and preservatives, for example methyl or propyl p-hydroxybenzoates or sorbic acid. Liquid compositions may conveniently be encapsulated in, for example, gelatin to give a product in dosage unit form.
[0067] Formulations for oral delivery may be formulated in a delayed release formulation such that the lanthanum is delivered to the large intestine. This will lessen the interaction of lanthanum with dietary phosphate which results in the precipitation of lanthanum phosphate, which is poorly absorbed by the gut. Delayed release formulations are well known in the art and include for example, delayed release capsules or time pills, osmotic delivery capsules etc.
[0068] Compositions for parenteral administration may be formulated using an injectable liquid carrier such as sterile pyrogen-free water, sterile peroxide-free ethyl oleate, dehydrated alcohol or propylene glycol or a dehydrated alcohol/propylene glycol mixture, and may be injected intravenously, intraperitoneally, subcutaneously or intramuscularly.
[0069] Compositions for rectal administration may be formulated using a conventional suppository base such as cocoa butter or another glyceride.
[0070] Compositions for topical administration include ointments, creams, gels, lotions, shampoos, paints, powders (including spray powders), pessaries, tampons, sprays, dips, aerosols, pour-ons and drops. The active ingredient may, for example, be formulated in a hydrophilic or hydrophobic base as appropriate.
[0071] It may be advantageous to incorporate an antioxidant, for example ascorbic acid, butylated hydroxyanisole or hydroquinone in the compositions of the invention to enhance their storage life.
[0072] Administration in this invention may consist of one or more cycles; during these cycles one or more periods of osteoclastic and osteoblastic activity will occur, as well as one or more periods when there is neither osteoclastic nor osteoblastic activity.
[0073] Alternatively, administration may be conducted in an uninterrupted regimen; such a regimen may be a long term regimen, e.g. a permanent regimen.
[0074] It will be understood that the dosages of compositions and the duration of administration according to the invention will vary depending on the requirements of the particular subject. The precise dosage regime will be determined by the attending physician or veterinary surgeon who will, inter alia, consider factors such as body weight, age and symptoms (if any). The compositions may if desired incorporate one or more further active ingredients.
[0075] During the dosing regimen, administration may be effected once or more times per day, for example once, twice, three or four times per day.
[0076] FIGS. 1 to 4 show the effect of the lanthanum (III) ion on bone resorption, osteoclast differentiation, osteoblast differentiation and bone formation respectively.
[0077] The following non-limiting examples describing the effect of a lanthanum (III) ion-containing solution in vitro bone culture assays and in vivo study are illustrative of the present invention.
EXAMPLE 1
In Vitro Bone Resorption Assay
[0000] Test Substance
[0078] The test substance was lanthanum carbonate tetrahydrate (hereinafter lanthanum carbonate). 1 mg of lanthanum is equivalent to 1.9077 mg of lanthanum carbonate. Lanthanum carbonate was dissolved in 2M HCl to give a concentration of 28.6 mg/ml (i.e 15 mg/ml of lanthanum).
[0079] Aliquots of this stock solution were diluted with 2M HCl to result in solutions of varying concentrations, so that addition of one microliter of these solutions into the culture medium gave the final test concentrations of 100, 500, 1000, 5000 and 15000 ng/ml of lanthanum in culture medium. These solutions/concentrations are hereinafter referred to as LA100, LA500, LA1000, LA5000 and LA15000.
[0000] Control Substances
[0080] We used control groups in each assay to show that the assays were capable of detecting the effect of inhibition (bone resorption assay and osteoclast differentiation assay) or activation (osteoblast differentiation and bone formation). The control substances used were:
Bafilomycin Al (in bone resorption assay) 17β-estradiol (in osteoblast differentiation assay and bone formation assay)
[0084] In the osteoclast differentiation assay, the control group did not contain vitamin D.
[0085] The method of osteoclast culture on bone slices was originally described by Boyde et al. (1984) and by Chambers et al. (1984). For cell culture, we used a method slightly modified from the original methods (Lakkakorpi et al. 1989, Lakkakorpi and Väänännen, 1991). The rate of bone resorption in the cultures was originally determined by counting the number of resorption pits on each bone or dentine slice using a microscope with phase contrast objectives (Sundquist et al. 1990). Later, the pits were visualized using Wheat Germ Agglutinin lectin that specifically binds to the resorbed area in bone (Selander et al. 1994), making it possible to quantify the total resorbed area using a microscope and computer-assisted image analysis system (Laitala and Väänänen 1994, Hentunen et al. 1995). We used a commercially available method (CrossLaps for cultures, Osteometer Biotech, Herlev, Denmark) to detect the amount of collagen cross-links released into the culture medium as an index of the bone resorption rate (Bagger et al., 1999).
[0086] The study protocol uses a method where osteoclasts are cultured on bone slices and allowed to resorb bone. The system is ideal for determining the effect of drug candidates on the bone resorbing activity of osteoclasts. Drug candidates are added into the cell cultures at the beginning of the culture period, and the osteoclasts allowed to resorb bone for 3 days. The amount of bone resorbed during the culture period is determined and compared to the amount of bone resorbed in control cultures (those cultured in the absence of drug candidates). If the drug candidate inhibits the function of osteoclasts, the amount of bone resorbed in these cultures is significantly lower than in the control cultures.
[0000] Procedure:
[0087] Transverse 0.1 mm thick slices of cortical bone were cut from the diaphysis of fresh bovine femurs (Atria Slaughterhouse, Oulu, Finland) using a low-speed diamond saw, cleaned by ultrasonication in multiple changes of sterile distilled water, and stored at 4° C. before use. Long bones were removed from 1-day-old rat pups killed by decapitation. The bones were dissected free of adherent soft tissues, and the endosteal surfaces were curetted with a scalpel blade into the osteoclast culture medium (Dulbecco s Modified Eagle s Medium (DMIEM), (Gibco BRL, Paisley, UK)) supplemented with 100 IU/ml penicillin, 100 μg/ml streptomycin (Penicillin/Streptomycin solution, Gibco BRL, Paisley, UK), 20 mM HEPES buffer (Gibco BRL, Paisley, UK) and 10% heat-inactivated fetal calf serum, pH 6.9 (Gibco BRL, Paisley, UK). The resulting suspension of dispersed cells and bone fragments was agitated using a plastic pipette. Larger fragments were allowed to sediment for a few seconds and the supernatant was seeded onto the bone slices pre-wetted in the medium. After a settling period of 30 minutes at 37° C., the bone slices were washed by dipping in fresh medium, and then transferred to wells in 24-well culture dishes containing osteoclast culture medium. The bone slices were incubated in a humidified atmosphere of 95% air and 5% carbon dioxide at 37° C. for 72 hours.
[0088] After the culture period, the amount of bone resorption was determined by measuring the amount of collagen cross-links released into the culture medium using a commercial kit (CrossLaps for cultures, Osteometer Biotech) according to the manufacturer's instructions. The number of osteoclasts in each culture was determined by microscopic counting of the amount of TRAP-positive multinuclear cells, and the results are given as the number of collagen cross-links released per one osteoclast.
[0089] In this study, the effect of the lanthanum (III) ion on the bone resorbing activity of osteoclasts was tested.
[0090] The following sample groups were included:
Baseline (including vehicle) Control (Baseline+10 nM bafilomycin Al) Baseline+100 ng/ml lanthanum Baseline+500 ng/ml lanthanum Baseline+1000 ng/ml lanthanum Baseline+5000 ng/ml lanthanum Baseline+15000 ng/ml lanthanum
[0098] Six replicates were included in each group, and the test was performed twice. Bafilomycin Al, a highly potent inhibitor of osteoclast V-ATPase proton pump, was used as a control to show the ability of the test system to detect inhibition of bone resorption.
[0000] Tables of Results:
[0099] In the bone resorption assay, the amount of medium CrossLaps (nM) released into the culture medium was determined and the number of osteoclasts in the corresponding cultures calculated. The medium CrossLaps amounts were divided with the osteoclast numbers in the corresponding cultures, and the results are given on Table 1 as relative medium CrossLaps amounts per osteoclasts. The relative values were obtained by dividing each individual value with the mean value of the baseline group.
TABLE 1 Relative medium CrossLaps amounts per osteoclast in the first bone resorption assay Group 1 2 3 4 5 6 Mean ± SD Baseline 0.98 0.82 1.01 1.65 0.74 0.81 1.00 ± 0.34 Control 0.00 0.00 0.00 0.19 0.27 0.14 0.10 ± 0.11(***) LA 100 0.57 0.56 1.13 0.78 0.71 0.71 0.74 ± 0.21 LA 500 1.04 0.58 1.38 0.75 0.88 0.63 0.88 ± 0.30 LA 1000 1.14 1.09 0.89 1.76 1.07 1.11 1.18 ± 0.30 LA 5000 1.39 0.78 2.70 1.18 0.76 1.21 1.34 ± 0.71 LA 15000 0.57 0.58 0.57 0.96 2.53 1.11 1.05 ± 0.76
[0100]
TABLE 2
Relative medium CrossLaps amounts per osteoclasts
in the second bone resorption assay
Group
1
2
3
4
5
6
Mean ± SD
Baseline
0.75
1.33
0.88
1.98
0.53
0.53
1.00 + 0.56
Control
0.00
0.00
0.00
0.00
0.00
0.00
0.00 ± 0.00(***)
LA 100
0.38
0.75
0.78
0.94
0.67
0.96
0.74 ± 0.21
LA 500
0.50
2.14
0.50
1.03
0.47
0.63
0.88 ± 0.65
LA 1000
0.70
0.59
1.69
1.40
1.68
0.73
1.13 ± 0.51
LA 5000
0.48
1.18
0.77
0.98
1.99
1.81
1.20 + 0.59
LA 15000
0.29
1.08
0.62
0.87
0.47
0.45
0.63 + 0.29
[0101] All data shown on tables 1 and 2 were combined and analyzed. The combined results are shown on table 3 and FIG. 1 .
TABLE 3 Combined results of the effect of LA 100-LA 15000 on bone resorption Group number Mean ± SD Baseline 12 1.00 ± 0.44 Control 12 0.00 ± 0.00(***) LA 100 12 0.74 ± 0.20 LA 500 12 0.88 ± 0.48 LA 1000 12 1.15 ± 0.40 LA 5000 12 1.27 ± 0.63 LA 15000 12 0.84 ± 0.59
Results
[0102] In the bone resorption assay, there was no significant effect of the lanthanum (III) ion on either the amount of CrossLaps released into the culture medium or on the osteoclast number. The control substance, bafilomycin Al, completely inhibited bone resorption. As shown on table 3 and FIG. 4 , the lanthanum (III) ion has no statistically significant effects on the bone resorbing activity of individual mature osteoclasts at any of the concentrations tested. However, the dose-dependent inhibition of bone resorption with the lower concentrations (LA 100 and LA 500) should be noticed. The slight decrease seen with LA 15000 may be due to slight toxic effects of this high concentration.
REFERENCE
[0103] Bagger Y Z, Foged N T, Andersen L, Lou H, Qvist P (1999) CrossLaps for culture: An improved enzyme-linked immunosorbent assay (ELISA) for measuring bone resorption in vitro. J Bone Miner Res 14, Suppl. 1, S370.
[0104] Boyde A, Ali N N, Jones Si (1984) Resorption of dentine by isolated osteoclasts in vitro. Br Dcnt J 156: 216-220.
[0105] Chambers T J, Revell P A, Fuller K, Athanasou N A (1984) Resorption of bone by isolated rabbit osteociasts. J Cell Sci 66: 383-399.
[0106] Hentunen T A, Lakkakorpi P T, Tuukkanen J, Lehenkari P P, Sampath T K, Väänänen B K (1995) Effects of recombinant human osteogenic protein-1 on the differentiation of osteoclast-like cells and bone resorption. Biochem Biophys Res Commun 209: 433-443.
[0107] Laitala T, Väänännen H K (1994) Inhibition of bone resorption in vitro by antisense RNA and DNA molecules targeted against carbonic anhydrase II or two subunits of vacuolar H+-ATPase. J Clin Invest 93: 2311-2318.
[0108] Lakkakorpi F, Tuukkanan I, Hentunen T, Jarvelin K, Väänänen H K (1989) Organization of osteoclast microfilaments during the attachment to bone surface in vitro. I Bone Miner Res 4: 817-825.
[0109] Lakkakorpi P T, Väänänen H K (1991) Kinetics of the osteoclast cytoskeleton during the resorption cycle in vitro. J Bone Miner Res 6: 817.826.
[0110] Selander K, Lehenkari P, Väänänen H K(1994) The effects of bisphosphonates on the resorption cycle of isolated osteoclasts. Calcif Tissue Int 55: 368-375.
[0111] Sundquist K, Lakkakorpi P, Wallmark B, Väänänen H K (1990) Inhibition of osteoclast proton transport by bafilomycin A 1 abolishes bone resorption. Biochem Biophys Res Commun 168: 309-313.
EXAMPLE 2
In Vitro Osteoclast Differentiation Assay
[0112] A method known as mouse bone marrow culture system is the one most widely used to study osteoclast differentiation. Originally, this method was developed by Takahashi et al. (1988a). Osteoclast precursors in mouse bone marrow can be induced to form multinucleated osteoclast-like cells (MNC) in the presence of either an active metabolite of vitamin D 3 (1,25(OH) 2 D 3 ) or parathyroid hormone (PTH). MNC formed in mouse bone marrow cultures have been demonstrated to possess several features characteristic of osteoclasts. They form pits on bone or dentine slices (Takahashi et al. 1988a, Hattersley and Chambers 1989, Shinar et al. 1990); they express high levels of tartrate-resistant acid phosphatase (TRAP) and calcitonin receptors (Takahashi et al. 1988b, Shinar et al. 1990); and they respond to calcitonin (Takahashi et al. 1988a) and prostaglandin E 2 (Collins and Chambers 1992). Thus, the method is an ideal one with which to study both stimulators and inhibitors of osteoclast differentiation.
[0113] In the original culture system, the osteoclast formation was determined after an 8-day culture. In bone marrow, both non-adherent osteoclast precursors and stromal cells are present, the latter of which are needed to support osteoclast formation. The number of osteoclasts formed is generally determined by counting the number of TRAP-positive MNC containing at least three nuclei (Takahashi et al. 1988a). In the negative control, where 1,25(OH) 2 D 3 is not added, TRAP-positive MNC are not formed.
[0114] We have modified the original assay so that we culture 1×10 6 mouse marrow cells/ml for 6 days. With this modification, the number of TRAP-positive MNC/culture has been shown to be approximately 150 (Choi et al. 1998, Hentunen et al. 1998). Instead of counting of the number of differentiated osteoclasts formed, we measured the amount of TRAP liberated from osteoclasts into the culture medium using a fast, simple TRAP immunoassay (Halleen et al. 1999) presentation in the Annual Meeting of the American Society for Bone and Mineral Research, Sep. 30-Oct. 4, 1999, in St. Louis, Mo., USA. Our results show that the amount of TRAP released into the culture medium correlates significantly (r=0.94, p<0.0001, n=120) with the amount of osteoclasts formed.
[0000] Procedure:
[0115] 8-10-week old mice were killed with CO 2 . Tibia and femora were dissected free from adhering soft tissues. The bone ends were cut off with a scalpel and the marrow was flushed with α-Minimal Essential Medium (α-MEM, Gibco BRL, Paisley, UK) supplemented with 100 IU/ml penicillin and 100 μg/ml streptomycin. A 10 ml syringe with a 27 gauge needle was used for flushing. Cells were centrifuged at 600×G for 10 minutes and the cell pellet was resuspended in α-MEM containing 10% fetal calf serum. Cells were allowed to attach to plastic for 2 h at 37° C. in a 5% CO 2 incubator to allow removal of monocytes and macrophages. Nonadherent cells were duly removed, and the attached bone marrow cells were cultured in 24-well plates (1×10 6 cells/well=1 ml) for 6 days. Half of the media were changed at day 3 and the treatments replaced. At the end of the culture, the plates were fixed with 2% paraformaldehyde in PBS for 20 minutes. Osteoclast formation was determined by measuring TRAP activity from the culture media using the novel TRAP immunoassay (vide infra), where we use a polyclonal TRAP antiserum prepared in rabbits against purified human bone TRAP. The TRAP antibody was bound to anti-rabbit IgG coated microtiter wells (Gibco BRL, Paisley, UK), and medium TRAP was then bound to the antibody. The activity of bound TRAP was measured in sodium acetate buffer using pNPP as substrate.
[0116] In this study, the effect of the lanthanum (III) ion on osteoclast differentiation in the presence of 1,25-dihydroxyvitamin D3 was tested. The following sample groups were included:
Baseline (including vehicle) Control (Baseline without 1,25-dihydroxyvitamin D3) Baseline+100 ng/ml lanthanum Baseline+500 ng/ml lanthanum Baseline+1000 ng/ml lanthanum Baseline+5000 ng/ml lanthanum Baseline+15000 ng/ml lanthanum
[0124] Six replicates were included in each group, and the test was performed twice. Baseline without 1,25-dihydroxyvitamin D3 was used as a control to show the test system allows inhibition of osteoclast differentiation to be detected. As the results of LA100 did not give statistically the same result (significantly different or not compared with the baseline) in both of the two tests, we performed the test with LA100 one additional time.
[0000] Tables of Results:
[0125] In the osteoclast differentiation assay, the amount of TRAP 5b activity released into the culture medium was determined as an index of osteoclast number. The results are shown as relative TRAP 5b activities obtained by dividing each individual TRAP 5b activity with the mean TRAP 5b activity of the baseline group.
TABLE 4 Relative TRAP 5b activities in the first osteoclast differentiation assay Group 1 2 3 4 5 6 Mean ± SD Baseline 1.32 0.72 0.43 0.45 1.89 1.18 1.00 + 0.57 Control 0.16 0.17 0.18 0.11 0.11 0.20 0.16 ± 0.04(**) LA 100 0.81 0.96 0.43 1.39 0.98 0.65 0.87 + 0.33 LA 500 0.73 0.55 0.48 0.87 0.58 1.05 0.71 ± 0.22 LA 1000 0.58 0.82 0.35 0.40 0.98 0.45 0.60 + 0.25 LA 5000 0.44 0.40 0.41 0.36 0.51 0.52 0.44 ± 0.06(*) LA 15000 0.14 0.26 0.21 0.34 0.31 0.88 0.36 ± 0.27(*)
[0126]
TABLE 5
Relative TRAP 5b activities in the second
osteoclast differentiation assay
Group
1
2
3
4
5
6
Mean ± SD
Baseline
1.27
1.37
0.98
0.92
0.74
0.71
1.00 + 0.27
Control
0.17
0.34
0.14
0.10
0.11
0.06
0.15 ± 0.10(***)
LA 100
0.64
0.66
0.62
0.36
0.33
0.62
0.54 ± 0.15(**)
LA 500
1.16
1.30
0.85
1.33
0.76
1.01
1.07 ± 0.24
LA 1000
0.70
0.78
0.34
0.65
0.69
1.00
0.69 + 0.21
LA 5000
0.94
0.46
0.21
0.72
0.68
0.33
0.56 ± 0.27(*)
LA 15000
0.22
0.31
0.35
0.25
0.15
0.20
0.25 ± 0.07(**)
[0127] The assay with LA 100 was repeated one more time, because the results were significantly different from baseline in the second assay, and not significantly different in the first assay.
TABLE 6 Relative TRAP 5b activities in the third osteoclast differentiation assay with LA 100. Group 1 2 3 4 5 6 Mean ± SD Baseline 1.25 1.20 0.76 0.93 1.07 0.81 1.00 + 0.20 Control 0.08 0.07 0.20 0.10 0.25 0.13 0.14 ± 0.07(***) LA 100 0.71 0.96 0.42 0.47 0.87 0.69 0.69 ± 0.21(*)
[0128] All data shown on tables 4-6 were combined and analyzed. The combined results are shown on table 7 and FIG. 2 .
TABLE 7 Combined results of the effect of LA 100-LA 15000 on osteoclast differentiation Group number Mean ± SD Baseline 18 1.00 ± 0.36 Control 18 0.15 ± 0.07(***) LA 100 18 0.70 ± 0.27(**) LA 500 12 0.89 ± 0.29 LA 1000 12 0.65 ± 0.23(**) LA 5000 12 0.50 ± 0.20(***) LA 15000 12 0.30 ± 0.19(***)
Results:
[0129] In the osteoclast differentiation assay, a clear dose-dependent inhibition was observed with LA 500-LA 15000 that was statistically significant from LA 1000 to LA 15000. A statistically significant inhibition was also observed with LA 100. In the control group where vitamin D was omitted, osteoclast differentiation was significantly lower than in the baseline group.
REFERENCES
[0130] Halleen N, Alatalo S, Hentunen T A, Väänänen H K (1999) A novel TRAP 5b immunoassay for osteoclast cultures. J Bone Miner Res 14, Suppl. 1, S244.
[0131] Choi S J, Devlin R D. Menaa C, Chung H, Roodman G D, Reddy S V (1998) Cloning and identification of human Sca as a novel inhibitor of osteoclast formation and bone resorption. J Clin Invest 102: 1360-1368.
[0132] Collins D A, Chambers T J (1992) Prostaglandin E 2 promotes osteoclast formation in murine hematopoietic cultures through an action on hematopotetic cells. J Bone Miner Res 7: 555-561.
[0133] Hattersley G, Chambers T J (1989) Generation of osteoclastic function in mouse bone marrow cultures: multinuclearity and tartrate-resistant acid phosphatase are unreliable markers for ostcoclastic differentiation. Endocrinology 124: 1689-1696.
[0134] Hentunen T A, Reddy S V. Boyce B F, Dovlin R, Park H-R, Chimg H, Selander K S, Dallas M, Kurihara N, Galson O L, Goldring S R, Koop, B A Windle J J, Roodman G D (1998) Immortalization of osteoclast precursors by targeting bcl-X L , and simian virus 40 large T antigen to the osteoclast lineage in transgenic mice. J Clin Invest 102: 88-97.
[0135] Shinar D M, Sato M, Rodan G A (1990) The effect of hemopoietic growth factors on the generation of osteoclast-like cells in mouse bone marrow cultures. Endocrinology 126: 1728-1735.
[0136] Takahashi N, Yamana H, Yoshiki S, Roodman G D, Mundy G R, Jones S J, Boyde A, Suda T (1988a) Osteoblast-Like cell formation and its regulation by osteotropic hormones in mouse bone marrow cultures. Endocrinology 122:1373-1382.
[0137] Takahashi N. Akatsu T, Sasaki T, Nicholson G C, Moseley J M, Martin T J, Suda T (1988b) Induction of calcitonin receptors by 1 ,25-dihydroxyvitamin D 3 in osteoblast-like multinucleated cells formed from mouse bone marrow cells. Endocrinology 123: 1504-1510.
EXAMPLE 3
In Vitro Osteoblast Differentiation Assay
[0138] Osteoblasts are bone-forming cells which arise from mesenchymal stem cells. During the development of osteoblasts, three distinct periods have been identified and defined: 1) cell proliferation and secretion of extracellular matrix (ECM); 2) ECM maturation; and 3) ECM mineralization. During these periods, a sequential expression of osteoblast phenotype markers has been characterized. Alkaline phosphatase is associated with the bone cell phenotype and is actively expressed during the maturation of the osteoblast. With the onset of mineralization, large amounts of calcium are deposited into the mature organic matrix to form bone-like nodules. By following these markers, we are able to study all the stages of osteoblast differentiation in this culture system.
[0139] Several methods have been devised to study osteoblasts. The first of these involves isolation of cells from calvaria with the osteoblastic phenotype. However, these cells only represent the mature stage of osteoblasts, because only a small fraction of the calvarial cells are osteoblast precursors (Bellows and Aubin 1989, Bellows et al. 1994). Osteoblastic cell lines are convenient in use, but they may not behave as primary osteoblasts (Mundy 1995). It is conceivable that osteoblast precursors are present in bone marrow (Friedenstein 1976, Owen 1988), and bone marrow stromal cells have long been recognized as the source of osteoprogenitor cells.
[0140] We have established a culture model in which mouse bone marrow derived osteoprogenitor cells first proliferate and then differentiate to osteoblasts capable of forming mineralized bone nodules (Qu et al. 1998, Qu et al. 1999). We confirmed this by following the expression of several markers of the osteoblastic phenotype and by studying the morphology of cultures at light and electron microscopic level. Synthesis of fibrillar extracellular matrix with late deposition of calcium confirmed the differentiation and maturation of osteoblasts. Thus, this culture system fulfills requirements of an in vitro model useful for studying differentiation of osteoprogenitor cells into bone synthesizing osteoblasts.
[0000] Procedure:
[0141] Bone marrow cells were obtained from the femurs of 10-week old female NMRI mice. Animals were killed by cervical dislocation. Both femora were removed and the soft tissues were detached aseptically. Metaphyses from both ends were cut off and bone marrow cells were collected by flushing the diaphysis with culture medium: phenol red-free-a-modified essential medium (α-MEM (Gibco BRL, Paisley, UK)). A suspension of bone marrow cells was obtained by repeated aspiration of the cell preparation through a 22 gauge needle, and nucleated cells were counted with a hemocytometer. Cells were plated at 10 6 cells/cm 2 in T-75 tissue culture flasks in phenol red-free-α-MEM supplemented with 10% FCS, 10 −8 M dexamethasone, 50 μg/ml ascorbic acid, 10−2 M sodium β-glycerophosphate, 100 IU/ml penicillin and 100 μg/ml streptomycin. The cells were cultured for 6 days and half of the media replaced after 3 days. On day 6, subcultures were prepared. Cells were washed with warm PBS and adherent cells were detached using trypsin-EDTA. Trypsinized cells were passed through a syringe with a 22 gauge needle to make a single-cell suspension, counted and plated in 24-well plates at a density of 5×10 3 cells/ml. These osteoprogenitor cells were stimulated to differentiate towards mature osteoblasts by culturing them in the presence of 10 −10 M estrogen (17β-estradiol) for 8 days. The test substances were added at the beginning of the secondary culture without estrogen, and every time when the medium was changed.
[0142] The number of osteoblasts formed was determined by measuring cellular alkaline phosphatase (ALP) activity in the culture. Cells were disrupted by washing the cell layers twice with PBS, extracting into 200 μl 0.1% Triton X-100 buffer at pH 7.6 (Sigma, St. Louis, Mo., USA), and overnight freezing. ALP activity was determined calorimetrically using p-nitrophenylphosphate as substrate at pH 9.7 and determining the optical density at 405 nm. In parallel, protein contents of the wells were determined by the BIO-RAD protein assay, and the specific ALP activity is expressed as units/mg protein.
[0143] In this study, the effect of the lanthanum (III) ion on osteoblast differentiation was tested. The following sample groups were included:
Baseline (+vehicle) Control (Baseline+10-10 −10 M 17 -estradiol) Baseline+100 ng/ml lanthanum Baseline+500 ng/ml lanthanum Baseline+1000 ng/ml lanthanum Baseline+5000 ng/ml lanthanum Baseline+15000 ng/ml lanthanum
Tables of Results:
[0151] Osteoblast differentiation was determined by measuring cellular alkaline phosphatase (ALP) activities and total protein amounts from cell lysates. The ALP activities were divided with the corresponding protein amounts to obtain specific activities of ALP. The results are shown as relative specific activities obtained by dividing each individual value with the mean value of the baseline group.
TABLE 8 Relative specific activities of intracellular alkaline phosphatase in the preliminary osteoblast differentiation assay Group 1 2 3 4 Mean ± SD Baseline 0.94 1.10 0.94 1.02 1.00 + 0.07 Control 1.10 1.32 1.31 1.29 1.26 ± 0.10(**) LA 100 0.98 1.29 1.19 1.12 1.15 + 0.13 LA 500 0.96 0.98 0.99 1.11 1.01 + 0.07 LA 1000 0.69 1.13 0.92 1.01 0.94 ± 0.19 LA 5000 0.42 0.46 0.50 0.48 0.47 ± 0.03(***) LA 15000 0.51 0.49 0.47 0.54 0.50 ± 0.03(***)
[0152]
TABLE 9
Relative specific activities of intracellular alkaline phosphatase
in the first osteoblast differentiation assay
Group
1
2
3
4
5
6
7
8
Mean ± SD
Baseline
0.97
0.94
1.12
0.98
0.97
1.06
0.99
0.96
1.00 ± 0.06
Control
1.01
1.20
1.04
1.13
1.19
1.06
1.03
1.14
1.10 ± 0.08(**)
LA 100
1.25
0.98
1.31
0.77
0.95
1.04
1.13
0.98
1.05 + 0.17
LA 500
0.83
1.03
1.02
0.98
0.95
0.96
0.82
0.62
0.90 + 0.14
LA 1000
1.01
1.12
1.06
0.76
1.01
0.78
0.93
0.81
0.94 + 0.14
LA 5000
0.54
0.48
0.47
0.63
0.54
0.59
0.44
0.55
0.53 ± 0.06(***)
LA 15000
0.40
0.42
0.53
0.36
0.39
0.35
0.30
0.43
0.40 ± 0.07(***)
[0153]
TABLE 10
lative specific activities of intracellular alkaline phosphatase
in the second osteoblast differentiation assay
Group
1
2
3
4
5
6
Mean ± SD
Baseline
0.99
0.83
1.25
1.01
0.88
1.04
1.00 ± 0.15
Control
1.00
1.18
1.53
1.52
1.03
1.38
1.27 ± 0.24(*)
LA 100
0.91
0.94
1.34
1.20
1.00
1.43
1.14 + 0.22
LA 500
0.88
0.89
1.10
1.09
0.75
0.90
0.93 ± 0.14
LA 1000
0.73
0.71
1.19
0.81
0.72
1.09
0.88 + 0.21
LA 5000
0.31
0.51
0.51
0.49
0.28
0.40
0.41 ± 0.10(***)
LA 15000
0.27
0.13
0.33
0.32
0.29
0.31
0.28 ± 0.07(***)
[0154] All data shown on tables 8-10 were combined and analyzed. The combined results are shown on table 11 and FIG. 3 .
TABLE 11 Combined results of the effect of LA 100-LA 15000 on osteoblast differentiation Group number Mean ± SD Baseline 18 1.00 ± 0.09 Control 18 1.19 ± 0.17(***) LA 100 18 1.10 ± 0.18(*) LA 500 18 0.94 ± 0.13 LA 1000 18 0.92 ± 0.17 LA 5000 18 0.48 ± 0.09(***) LA 15000 18 0.38 ± 0.11(***)
Results:
[0155] The lanthanum (III) ion showed a clear dose-dependent response in the osteoblast differentiation assay. The highest test concentrations (LA 5000 and LA 15000) inhibited, and the lowest test concentration (LA 100) activated osteoblast differentiation significantly. No significant response was observed with LA 500 and LA 1000. The control substance, 17β-estradiol, activated osteoblast differentiation significantly.
REFERENCES
[0156] Bellows C G, Aubin J E (1989) Determination of the number of osteoprogenitors in isolated fetal rat calvarial cells in vitro. Develop Biol 113:8-13.
[0157] Bellows C G, Wang Y H. Heersche J N, Aubin J E (1994) 1,25-dihydroxyvitamin D 3 stimulates adipocytic differentiation in cultures of fetal rat calvarial cells: comparison with the effects of dexamethasone. Endocrinology 134:2221-2229.
[0158] Friedenstein A J (1976) Precursor cells of mechanocytes. Int Rev Cytol 47: 327-355.
[0159] Mundy R G (1995) Osteoblests, bone formation and mineralization. In: Bone remodeling and its disorders. Martin Dunitz Ltd pp. 29-30.
[0160] Owen M. Friendenstein A J (1988) Stromal stem cells: Marrow-derived osteogenic precursors. Ciba Found Symp 136:42-60.
[0161] Qu Q, Perälä-Heape M, Kapanen A, Dahllund J, Salo J, Väänänen, H K, Härkönen. P (1998) Estrogen enhances differentiation of osteoblasts in mouse bone marrow culture. Bone 22:201-209.
[0162] Qu Q, Härkönen P L, Väänänen H K (1999) Comparative effects of estrogen and antiestrogens on differentiation of osteoblasts in mouse bone marrow culture. J Cell Biochem 73: 500-507.
EXAMPLE 4
In vitro Bone formation Assay
[0163] The activity of mature osteoblasts can be determined by quantifying their ability to form mineralized bone matrix. This is done by demineralizing the formed bone matrix, and determining the amount of calcium released. Thus, this culture system fulfills requirements of an in vitro model useful for studying the bone formation activity of mature osteoblasts.
[0000] Procedure:
[0164] The mature osteoblasts obtained during the 8-day secondary culture in the absence of estrogen and any test substances described above were allowed to form bone nodules by culturing them for 7 additional days. At the end of the culture, the amount of calcium deposited during the culture period was determined, and the amount of bone formation (calcium deposition) calculated.
[0165] In order to quantify the amount of calcium deposited, the cell cultures were washed three times with Ca 2+ - and Mg 2+ -free PBS and incubated overnight at room temperature in 0.6M HCl. Extracts of 50 μl were complexed with 1 ml determined o-cresol-phthalein-complexon. The colorimetric reaction was determined at 570 nm in a spectrophotometer. Absolute calcium concentrations were determined by comparison with a calibrated standard provided by the vendor.
[0166] In this study, the effect of lanthanum carbonate on bone formation was tested. The following sample groups were included:
Baseline (including vehicle) Control (Baseline+10 −10 M 17β-estradiol) Baseline+100 ng/ml lanthanum Baseline+500 ng/ml lanthanum Baseline+1000 ng/ml lanthanum Baseline+5000 ng/ml lanthanum Baseline+15000 ng/ml lanthanum
Tables of Results:
[0174] The amount of bone formation was determined by measuring the amount of calcium deposited into bone nodules formed by mature osteoblasts. The results are shown as the amount of calcium released (mmol/L) from the bone nodules after HCl extraction. The baseline values are too low to show the results using relative amounts as was done in the other assays.
TABLE 12 Calcium deposition (mmol/L) in the preliminary bone formation assay Group 1 2 3 4 Mean ± SD Baseline 0 0 0 0 0.00 ± 0.00 Control 0.04 0 0 0.04 0.02 ± 0.02 LA 100 0 0 0 0 0.00 ± 0.00 LA 500 0 0 0 0.09 0.02 ± 0.05 LA 1000 0.10 0 0.11 0.05 0.07 ± 0.05(*) LA 5000 0.59 1.64 0.39 1.62 1.06 ± 0.66(***) LA 15000 1.48 0.16 0.50 1.41 0.89 ± 0.66(***)
[0175]
TABLE 13
Calcium deposition (mmol/L) in the first bone formation assay
Group
1
2
3
4
5
6
Mean ± SD
Baseline
0
0
0
0.02
0.02
0
0.01 ± 0.01
Control
0.15
0.21
0.14
0.10
0.15
0.16
0.15 ± 0.04(***)
LA 100
0.04
0.17
0.01
0.27
0
0.14
0.11 ± 0.11(*)
LA 500
0.44
0.15
1.32
0.27
1.31
1.10
0.77 ± 0.54(***)
LA 1000
0.95
1.66
1.47
1.41
1.00
1.25
1.29 ± 0.28(***)
LA 5000
1.31
1.55
1.56
1.52
1.40
1.39
1.46 ± 0.10(***)
LA 15000
1.46
1.42
1.56
1.11
1.11
1.08
1.29 ± 0.21(***)
[0176]
TABLE 14
Calcium deposition (mmol/L) in the second bone formation assay
Group
1
2
3
4
5
6
7
8
Mean + SD
Baseline
0
0.01
0
0.01
0
0
0.02
0
0.01 ± 0.01
Control
0.22
0.14
0.16
0
0.16
0
0.10
0.16
0.12 ± 0.08(**)
LA 100
0.04
0.18
0
0
0
0.28
0.14
0
0.08 ± 0.11
LA 500
0.17
0.30
1.41
0
0.02
0.46
1.17
1.40
0.62 ± 0.61(*)
LA 1000
1.09
0.81
1.34
1.56
1.76
0.02
1.52
1.02
1.14 ± 0.55(***)
LA 5000
1.70
1.44
1.64
1.52
1.08
1.63
1.30
1.48
1.47 ± 0.20(***)
LA 15000
1.24
1.46
1.22
1.68
1.62
1.18
1.21
1.56
1.40 ± 0.21(***)
[0177] The data shown on tables 13 and 14 were combined and analyzed. The results from table 12 were not included as there was no significant difference between the baseline and the control groups. The combined results are shown on table 15 and FIG. 4 .
TABLE 15 Combined results of the effects of LA 100-LA 15000 on bone formation activity of mature osteoblasts Group number Mean ± SD Baseline 14 0.01 ± 0.01 Control 14 0.13 ± 0.06(***) LA 100 14 0.09 ± 0.10(**) LA 500 14 0.68 ± 0.56(***) LA 1000 14 1.20 ± 0.45(***) LA 5000 14 1.47 ± 0.16(***) LA 15,000 14 1.35 ± 0.21(***)
Results:
[0178] All concentrations of the lanthanum (III) ion tested showed a highly significant activation of the bone formation activity of mature osteoblasts, the activation being highest with the highest test concentrations. The control substance, 17β-estradiol, activated bone formation significantly.
REFERENCES
[0179] Bellows C G, Aubin J E (1989) Determination of the number of osteoprogenitors in isolated fetal rat calvarial cells in vitro. Dev Biol 113:8-13.
[0180] Bellows C G, Wang Y H, Heersche J N, Aubin J E (1994) 1,25-dihydroxyvitamin D 3 stimulates adipocytic differentiation in cultures of fetal rat calvarial cells: comparison with the effects of dexamethasone. Endocrinology 134:2221-2229.
[0181] Friedenstein A J (1976) Precursor cells of mechanocytes. Int Rev Cytol 47:327-355.
[0182] Mundy R G (1995) Osteoblasts, bone formation and mineralization. In: Bone remodeling and its disorders. Martin Dunitz Ltd pp. 29-30.
[0183] Owen M, Friendentein A J (1988) Stromal stem cells: Marrow-derived osteogenic precursors. Ciba Found Symp 136:42-60.
[0184] Qu Q, Perälä-Heape M, Kapanen A, Dahllund J, Salo J, Väänänen H K, Härkönen, P (1998) Estrogen enhances differentiation of osteoblasts in mouse bone marrow culture. Bone 22:201-209.
[0185] Qa Q, Härkönen P L, Väänänen H K (1999) Comparative effects of oestrogen and antiestrogens on differentiation of osteoblasts in mouse bone marrow culture. J Cell Biochem 73: 500-507.
[0186] Animals for in Vitro Studies
Species/strain/age/sex Supplier Mouse/NMRI <8-12 w, male and University of Turku, The centre of female experimental animals, Turku, Finland Rat, Sprague-Dawley, 1 day University of Turku, The centre of experimental animals, Turku, Finland
Statistical Analyses of in Vitro Results
[0187] The mean and standard deviation (SD) of each group was determined. One-way analysis of variance (ANOVA) was used to study if the values obtained between different groups (baseline vs. controls and test substances) were statistically different (with p<0.05). Statistical significance is shown in each table and figure with asterisks, one asterisk (*) indicating a p-value between 0.05 and 0.01, two asterisks (**) a p-value between 0.01 and 0.001, and three asterisks (***) a p-value<0.001. No asterisks indicate that the results of the group do not differ significantly from the results of the corresponding baseline group.
[0000] Summary of in Vitro Results
[0188] The effects of the test concentrations of the lanthanum (III) ion on the activity and differentiation of bone cells are summarized on table 17, where (+) means significant activation, (−) significant inhibition, and (0) no effect. One character (+ or −) means a p-value between 0.05 and 0.01, two characters (++ or −−) a p-value between 0.01 and 0.001, and three characters (+++ or −−−) a p-value<0.001.
TABLE 17 The effects of LA on bone cells Dose, Bone Osteoclast Osteoblast Bone ng/ml resorption differentiation differentiation formation 100 0 −− + ++ 500 0 0 0 +++ 1000 0 −− 0 +++ 5000 0 −−− −−− +++ 15000 0 −−− −−− +++
Conclusions of in Vitro Studies
[0189] The lanthanum (III) ion is a powerful stimulator of the bone formation activity of mature osteoblasts at all concentrations tested, the best responses observed with the highest test concentrations (LA 5000 and LA 15000). However, these concentrations may also have cytotoxic effects on the osteoblast precursor cells, which may compensate the activation of mature osteoblasts in vivo.
[0190] LA 500 and LA 1000 also stimulate bone formation, but these concentrations do not decrease the formulation of osteoblasts in the osteoblast differentiation assay, suggesting that they have no cytotoxic effects on osteoblast precursor cells. However, LA 1000 decreases the formation of osteoclasts in osteoclast differentiation assay, suggesting that it may have cytotoxic effects on osteoclast precursor cells. The only significant effect of LA 500 in the four assays was the activation of bone formation. Thus, this concentration of LA may be useful in increasing the bone formation without cytotoxic effects.
[0191] LA 100 appears to activate both bone formation and osteoblast differentiation, and inhibit osteoclast differentiation and bone resorption (although the inhibition of bone resorption is not statistically significant). All these effects would strengthen bones.
EXAMPLE 5
In Vivo Bone Formation Study
[0000] Procedure:
[0192] The specimens taken from the iliac crest of growing immature dogs were analysed. The group was divided into a control and treatment group. The treatment group received 1000 mg/Kg of lanthanum carbonate administered orally twice daily. The groups were run for 13 weeks, after which time samples of bone were taken vertically through the iliac crest, embedded in methyl methacrylate based resin, sectioned and stained with toluidine blue and Von Kossa stain. The parameters measured were:
Trabecular and cortical bone mass Osteoid surface and volume Osteoblast surface Cortical osteoid volume Trabecular and cortical osteoclast number Resorptive surfaces in cortex and trabecular bone
Results:
[0199] The iliac crest of these animals is acting as a growth plate. The appearances are those of immature animals actively growing. There was very active bone remodeling throughout the specimens sampled and, in addition, there appeared to be bone modelling with very active periosteal osteoclasis on the cortical surface, and within the cortex on the other.
[0200] There was a marked difference in cortical thickness between the different animals and marked variation in the amount of bone within the biopsy specimen. This degree of variation was not restricted to either of the two groups of animals, or to animals of particular sex.
[0201] There was a statistically significant difference for the trabecular bone volume between the two groups. The trabecular bone volume was lower in the control group (approximately half that in the treatment group) than in the lanthanum treated group. There was no statistically significant difference in any of the other bone parameters investigated between the two groups.
[0202] There was an increase of trabecular bone volume in treated animals (about twice) compared to the control group. These results suggest that lanthanum influences bone growth at the growth plate.
[0203] For the purposes of Examples 6 and 7, the term “hydrated lanthanum carbonate” refers to lanthanum carbonate having a water content approximately equivalent to 4-5 moles of water.
EXAMPLE 6
Preparation of Stabilized Hydrated Lanthanum Carbonate and Vitamin D Chewable Tablets (250 mg, 500 mg, 750 mg, and 1000 mg)
[0204] The manufacturing process involves sieving and blending the active ingredients with the excipients followed by direct compression. More specifically the steps are as follows:
[0205] a) Blend the lanthanum carbonate, the vitamin D and the excipients (e.g., dextrates, colloidal silicon dioxide, talc (optional) and magnesium stearate).
[0206] b) Compress the blend using standard tooling to the target compression weight.
[0207] The following formulations illustrate tablets that can be made using the above manufacturing technique.
TABLE 18A Formulation A 250 mg Ingredient tablet 500 mg tablet Function Active Ingredients: Hydrated lanthanum 477.0 mg 954.0 mg Active (III) carbonate Vitamin D 2 Tablet 0.47 mg 0.94 mg Active Grade (850,000 IU/gram) Other Ingredients: Dextrates 1246.53 mg 2493.06 mg Stabilizes lanthanum carbonate Colloidal anhydrous 36.0 mg 72.0 mg Improves blending silica and flow Purified talc 30.0 mg 60.0 mg Lubricant or glidant Magnesium stearate 10.0 mg 20.0 mg Lubricant Total 1800 mg 3600 mg
[0208]
TABLE 18B
Formulation B
250 mg
Ingredient
tablet
500 mg tablet
Function
Active Ingredients:
Hydrated lanthanum
477.0
mg
954.0
mg
Active
(III) carbonate
Vitamin D 3 Tablet
0.47
mg
0.94
mg
Active
Grade
(850,000 IU/gram)
Other Ingredients:
Dextrates
1246.53
mg
2493.06
mg
Stabilizes
lanthanum
carbonate
Colloidal anhydrous
36.0
mg
72.0
mg
Improves blending
silica
and flow
Purified talc
30.0
mg
60.0
mg
Lubricant or glidant
Magnesium stearate
10.0
mg
20.0
mg
Lubricant
Total
1800
mg
3600
mg
[0209]
TABLE 18C
Formulation C
250 mg
Ingredient
tablet
500 mg tablet
Function
Active Ingredients:
Hydrated lanthanum
477.0
mg
954.0
mg
Active
(III) carbonate
Vitamin D 3 Tablet
4.0
mg
8.0
mg
Active
Grade
(100,000 IU/gram)
Other Ingredients:
Dextrates
1243
mg
2486
mg
Stabilizes
lanthanum
carbonate
Colloidal anhydrous
36.0
mg
72.0
mg
Improves blending
silica
and flow
Purified talc
30.0
mg
60.0
mg
Lubricant or glidant
Magnesium stearate
10.0
mg
20.0
mg
Lubricant
Total
1800
mg
3600
mg
[0210]
TABLE 18D
Formulation D
250 mg tablet
500 mg tablet
750 mg tablet
1000 mg tablet
Tablet
13
mm
18
mm
20
mm
22
mm
diameter
Formulation
Lanthanum
250
mg
500
mg
750
mg
1000
mg
carbonate as
elemental
lanthanum
Hydrated
477
mg
954
mg
1431
mg
1908
mg
lanthanum
carbonate
Vitamin D 2
0.47
mg
0.47
mg
0.94
mg
0.94
mg
Tablet Grade
850,000 IU/gram
Dextrates (hydrated)
532.7
mg
1065.9
mg
1598.7
mg
2131.9
mg
Colloidal
21.2
mg
42.4
mg
63.6
mg
84.8
mg
silicon dioxide
Magnesium
10.6
mg
21.2
mg
31.8
mg
42.4
mg
stearate
Total weight
1042
mg
2048
mg
3126
mg
4168
mg
[0211]
TABLE 18E
Formulation E
Percent by Weight
Formulation Components
in the Tablet
Hydrated lanthanum carbonate
45.8%
Vitamin D 3 Tablet Grade (100,000 IU/gram)
0.4%
Colloidal silicon dioxide (e.g., Aerosil ®
2.1%
200 available from Degussa Corp. (Piscataway, NJ))
Dextrates
50.7%
Magnesium sterate
1.0%
[0212]
TABLE 18F
Formulation F
Percent by Weight
Formulation Components
in the Tablet
Hydrated lanthanum carbonate
63.6%
Vitamin D 3 Tablet Grade (100,000 IU/gram)
0.5%
Glyceryl dibehenate
3.0%
Colloidal silicon dioxide (e.g., Aerosil ® 200)
2.0%
Sorbitol
29.9%
Talc
1.0%
[0213]
TABLE 18G
Formulation G
Percent by Weight
Formulation Components
in the Tablet
Hydrated lanthanum carbonate
63.6%
Vitamin D 3 Tablet Grade (100,000 IU/gram)
0.5%
Glyceryl dibehenate
3.0%
Colloidal silicon dioxide (e.g., Aerosil ® 200)
2.0%
Mannitol
29.9%
Talc
1.0%
[0214]
TABLE 18H
Formulation H
Percent by Weight
Formulation Components
in the Tablet
Hydrated lanthanum carbonate
63.6%
Vitamin D 3 Tablet Grade (100,000 IU/gram)
0.5
Glyceryl dibehenate
3.0%
Colloidal silicon dioxide (e.g., Aerosil ® 200)
2.0%
Xylitol
29.9%
Talc
1.0%
EXAMPLE 7
Preparation of Soft Gelatin Capsule Formulations of Hydrated Lanthanum Carbonate and 25-hydroxy Vitamin D 2 or 1,25-dihydroxy Vitamin D 2
[0215] The manufacture of soft gelatin capsule formulations of hydrated lanthanum carbonate and 25-hydroxy vitamin D 2 or 1,25-dihydroxy vitamin D 2 includes the following steps:
[0216] (1) 25-hydroxy vitamin D 2 or 1,25-dihydroxy vitamin D 2 and, optionally, an antioxidant (such as BHA (i.e., butylated hydroxyanisole available from Eastman Chemical Company, Kingsport, Tenn.), BHT (i.e., butylated hydroxytoluene available from Eastman Chemical Company, Kingsport, Tenn.) or DL-alpha-tocopherol (available from BASF, Florham Park, N.J.) are dissolved in a medium chain triglyceride (e.g., Miglyol™ 812 available from Sasol, Houston, Tex.);
[0217] (2) hydrated lanthanum carbonate is added as a suspension to form a paste; and
[0218] (3) the paste (i.e., fill composition having a maximum volume of 1 mL) would be encapsulated in a shell consisting of gelatin, glycerol, water, and, optionally, a plasticizer such as sorbitol (available from Roquette, Lestrem, France).
[0219] Below are examples of shell and fill compositions:
[0220] Shell composition #1 for a soft gelatin device: said composition comprising 38.0-46.0% by weight of gelatin, 14-25% by weight of sorbitol solution 70% (non crystallizable), 0.2-0.6% by weight of glycine, 0.02-0.03% by weight of butylated hydroxy anisole and 40.5-45.5% by weight of purified water.
[0221] Shell composition #2 for a soft gelatin device: said composition comprising 38.0-46.0% by weight of gelatin, 14-25% by weight of sorbitol solution, 70% (non crystallizable), 0.2-0.6% by weight of glycine, 0.02-0.03% by weight of butylated hydroxy anisole, 0.02-0.03% by weight of butylated hydroxy toluene, 40.5-45.5% by weight of Purified water.
Fill Composition #1 Lanthanum Carbonate hydrated 477.0 mg 25-hydroxy vitamin D 2 0-1.0 mg Butylated Hydroxyanisole 0.2 mg Medium Chain Triglyceride (e.g., MIGLYOL ™ 812) to 1000 mg Fill Composition #2 Lanthanum Carbonate hydrated 477.0 mg 25-hydroxy vitamin D 2 0-1.0 mg Butylated Hydroxytoluene 0.2 mg Medium Chain Triglyceride (e.g., MIGLYOL ™ 812) to 1000 mg Fill Composition #3 Lanthanum Carbonate hydrated 477.0 mg 25-hydroxy vitamin D 2 0-1.0 mg D-alpha tocopherol 20 mg Medium Chain Triglyceride (e.g., MIGLYOL ™ 812) to 1000 mg Fill Composition #4 Lanthanum Carbonate hydrated 477.0 mg 1,25-dihydroxy vitamin D 2 0-1.0 mg Butylated Hydroxyanisole 0.2 mg Medium Chain Triglyceride (e.g., MIGLYOL ™ 812) to 1000 mg Fill Composition #5 Lanthanum Carbonate hydrated 477.0 mg 1,25-dihydroxy vitamin D 2 0-1.0 mg Butylated Hydroxytoluene 0.2 mg Medium Chain Triglyceride (e.g., MIGLYOL ™ 812) to 1000 mg Fill Composition #6 Lanthanum Carbonate hydrated 477.0 mg 1,25-dihydroxy vitamin D 2 0-1.0 mg D-alpha tocopherol 20 mg Medium Chain Triglyceride (e.g., MIGLYOL ™ 812) to 1000 mg
[0222] Having illustrated and described the principals of the invention in preferred embodiments, it should be appreciated to those skilled in the art that the invention can be modified in arrangement and detail without departure from such principals. We claim all modifications coming with the scope of the following claims.
[0223] All publications, patents and patent applications referred to herein are incorporated by reference in their entirety to the same extent as if each individual publication, patent or patent application was specifically and individually indicated to be incorporated by reference in its entirety.
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The invention provides a method for enhancing bone formation, inhibiting osteoclastic differentiation and/or activating osteoblastic differentiation whereby to manage, treat or achieve prophylaxis of bone disease which comprises administering to a human or animal subject suffering from, or susceptible to bone disease a therapeutically or prophylactically effective amount of a lanthanum compound and a bone enhancing agent, such as vitamin D.
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BACKGROUND OF THE INVENTION
The invention relates to a heatable roll for a paper machine, paper finishing machine, or equivalent. The roll is heated by a heating medium which is introduced into the roll interior through at least one of the ends of the roll. The heating medium acts upon the material of the roll mantle, or the material of the roll, and is arranged to flow across the axial length of the roll. Thereafter, the heating medium is arranged to flow out of the roll through either one of the ends of the roll, i.e. the same end through which the heating medium entered into the roll or an opposite end.
The invention also relates to a method for heating a roll for use in paper machines, paper finishing machines or other paper machines. A heat transfer medium is introduced into a roll, circulated through the roll and removed from the roll. In this manner, the material of the roll mantle or the material of the roll is heated.
Further, the invention also relates to a method for maintaining a substantially constant temperature on an outer surface of the roll over which a paper web or board will pass.
In paper machines and paper finishing machines, in particular in calenders and super-calenders, heatable rolls are commonly used. The rolls are heated by means of a heat-transfer medium, such as hot water or oil.
There are mainly two different types of heatable rolls in the prior art. The first type of heatable rolls have a roll mantle, or are massive rolls, wherein substantially axial bores are formed in proximity to the outer face of the roll. The heating medium is made to flow through the bores from one end of the roll to an opposite end of the roll. Generally, a number of such bores are provided in the roll and are uniformly spaced in the direction of the circumference of the roll. The heating medium may be arranged to circulate in the bores either once in a direction from one end of the roll to the other, or twice, or even several times, so that in adjacent bores the heating medium flows in opposite directions. One such so-called "drilled roll" has been described earlier, e.g., in published European Patent Application No. EP-0 158 220.
On the other hand, a second type of heatable roll is a so-called double-mantle roll or rolls provided with an interior piece. This type of heatable roll is commonly used in paper machines. In this type of roll, an interior piece is fitted inside the roll mantle so that an annular intermediate space remains between the interior piece and an inner face of the roll mantle. The heating medium circulates in the annular space from one end of the roll to the other end of the roll. One such roll provided with an interior piece is described, e.g., in Finnish Patent No. 74,069.
A problem in prior art heatable rolls is that owing to the construction of the rolls, the profiles of the surface temperature in the rolls are almost always uneven. The rising differences in temperature in the axial direction of the roll are influenced by the construction and size of the roll. In rolls provided with interior pieces, typical differences in the surface temperature, on the surface over which the web runs, in the axial direction of the roll are in the range about 3° C. to about 6° C. On the other hand, in drilled rolls, a typical reduction of the surface temperature between the ends of the bores in the roll is in the range of about 3° C. while the maximum difference in temperature in the axial direction of the roll is in the range of about 9° C. and the difference in temperature in a cross-sectional plane of the roll is in the range of about 6° C.
The temperature differences in both types of prior art rolls produce dangerous and very detrimental thermal strains in the roll. Deformations which can be noticed in the smoothness of the paper, and which deteriorate the runnability of the machine, are also caused by such temperature differences. Therefore, a commonly imposed requirement on the variations in temperature in the working face, i.e. the outer face, of a roll is in the range of about ±1.5° C. Thus, in prior art rolls, it is a significant drawback that the rolls have not been able to conform with this requirement.
Reference is also made to U.S. Pat. No. 4,658,486 (Schonemann) which describes a heatable calendar roll having axial passages formed in the roll mantle for circulating a heating medium. However, it is a significant drawback that the roll described in this reference does not provide a substantially uniform temperature along the axial length of the roll mantle. This is because there are no means provided to increase the coefficient of heat transfer in the roll material in the flow direction of the heating medium.
OBJECTS AND SUMMARY OF THE INVENTION
It is an object of the present invention is to provide a heatable roll which is an improvement over prior art heatable rolls.
It is another object of the present invention to provide a new and improved method to heat a roll used in a paper machine.
It is yet another object of the present invention to provide a heatable roll having a face in which the differences in temperature are substantially lower than in prior art devices and substantially constant along the axial length of the roll and which rolls comply with the preferred requirements imposed on rolls by users of the rolls in paper machines.
It is still another object of the present invention to provide a new and improved roll in which the coefficient of heat transfer to the outer face of the roll increases as the heat transfer medium flows through the roll.
In view of achieving these objects, and others, the roll in accordance with the invention is provided with means by which the coefficient of heat transfer from the flowing heating medium that acts upon the material of the roll mantle to the material of the roll is increased in the flow direction of the heating medium.
The present invention provides a number of important advantages in comparison to prior art devices. In the present invention, the surface temperature of the roll mantle can be made substantially uniform and the amount of the heating medium used for the heating of the roll can be reduced substantially. For these reasons, the pumping capacity of the heating medium that is needed to heat the roll is not as high as in prior art devices. Moreover, a uniform temperature of the roll mantle has a highly favorable and significant effect on the quality of the paper. It is a further remarkable advantage that, by means of simple operations and/or modifications, the invention can be applied to existing prior art rolls.
BRIEF DESCRIPTION OF THE DRAWINGS
The following drawings are illustrative of embodiments of the invention and are not meant to limit the scope of the invention as encompassed by the claims.
FIG. 1 is a schematic, partly sectional longitudinal view of a drilled roll in accordance with the invention and used in a method in accordance with the invention.
FIG. 2 is a schematic cross-sectional view taken along the line II-II in FIG. 1.
FIG. 3 is a partial perspective view of the roll mantle of a drilled roll as shown in FIG. 1 and of an insulation piece in accordance with the invention arranged in one bore in the roll mantle.
FIG. 4 is a schematic, longitudinal sectional view of a roll provided with a displacement piece in accordance with the invention.
FIG. 5 is a schematic, partly sectional longitudinal view of a drilled roll in accordance with the invention and used in a method in accordance with the invention.
DETAILED DESCRIPTION OF THE INVENTION
In FIGS. 1, 2, 3 and 5, a heatable roll in accordance with the present invention is denoted generally with the reference numeral 10. The roll 10 comprises a roll mantle 11 having a pair of ends arranged on opposite axial sides of the roll. Roll ends 13,14 are fixed to each of the ends of the roll mantle 11 and are provided with axle journals 15,16, respectively. Bores 17 are arranged in the roll mantle 11 in proximity to an outer face, or surface, 12 of the roll 10. The bores 17 may be drilled into the roll mantle and extend from one end of the roll to an opposite end of the roll. In the embodiments shown in FIGS. 1, 2 and 3, bores 17 are arranged to run substantially in the axial direction of the roll 10.
As shown in FIG. 2, several bores 17 are arranged in the circumferential direction of the roll 10 and are distributed substantially evenly over the circumference. An axial central bore 18 is arranged to pass through the first roll end 13 of the roll and into the axle journal 15 provided therein. The axial central bore 18 may be formed, e.g., by drilling, through the material of the roll 10 and roll end 13. A pipe 19 or equivalent is placed through the central bore 18 and extends into the second roll end 14. The diameter of the pipe 19 is smaller than that of the central bore 18, so that an annular gap remains between the pipe and the central bore 18.
A heating medium is introduced into the roll 10 through the pipe 19. The heating medium flows into radial bores 14a formed in the second roll end 14 opposite the first roll end 13 so that the heating medium flows across the axial length of the roll 10 from one end to an opposite end of the roll such that the entire surface of the roll is heated. Radial bores 14a extend from the pipe 19 in a center portion of the roll 10 into bores 17 placed in the roll mantle 11. In a corresponding manner, radial bores 13a are formed in the first roll end 13 and extend from the bores 17 in the roll mantle into the annular gap in the central bore 18 placed in the first end. Thus, the heating medium flows from the pipe 19 through the radial bores 14a placed in the second roll end 14 into the bores 17 extending from end to end in the roll mantle 11, and from the bores 17 through the radial bores 13a formed in the first roll end 13 into the central bore 18 and further out of the roll 10.
In the embodiments shown in FIGS. 1,2 and 3, the coefficient of heat transfer from the flowing heating medium to the material of the roll mantle 11 is increased in the flow direction of the heating medium by providing suitable means in the roll mantle 11. For example, insulation pieces 1 can be arranged in each of the bores 17 of the roll mantle 11. The insulation pieces 1 might be provided with an outer shell having a decreasing thickness in the flow direction of the heating medium through the bores.
According to FIG. 3, the insulation pieces may consist, e.g., of a tube made of plastic or some other insulation material, into which tube an opening 2 has been formed. The opening 2 is parallel to the longitudinal, i.e. axial, direction of the tube and extends from one end of the tube to an opposite end so that the heating medium can flow therethrough. The size of the opening increases in the flow direction of the heating medium. The opening 2 in the tube is directed towards the outer face 12 of the roll mantle 11. Thus, in the embodiment illustrated in FIG. 3, the proportion of the material of the roll mantle 11 with which the heating medium is in direct contact is increased in the flow direction.
In this embodiment, since the temperature of the heating medium is lowered in the direction of the flow and since, on the other hand, the heating medium can act upon an increasing proportion of the material of the roll mantle 11 in the direction of the flow, the temperature of the roll mantle 11, and thus the outer surface of the roll, is not substantially changed in the axial direction of the roll. The reason the temperature of the heating medium is lowered is because a portion of the heat energy contained within the heating medium is transferred to the roll mantle to heat the roll as the heating medium progresses through the bores 17.
The insulation piece 1 may also be shaped in a manner different from that illustrated in FIGS. 1, 2 and 3. The main point is, however, that the insulation piece 1 should be shaped so that the transfer of heat is restricted in a controlled way in the axial direction of the roll, i.e. in the flow direction. In the manner, the surface temperatures on the roll 10 can be made uniform. At the same time, the conduction of heat can be guided efficiently towards the roll face 12.
In a preferred embodiment, a tubular piece is utilized as the insulation piece 1. In this embodiment, it is possible to accomplish the advantageous heat conduction so that the inner face of the tubular insulation piece 1 becomes conically wider in the flow direction, i.e. the interior diameter increases in the flow direction of the heating medium. In this embodiment, the wall thickness of the tube will become smaller in the flow direction. However, this is more difficult to arrange in practice than the formation of an opening 2 into a tubular insulation 1, which was described above.
In a drilled roll 10 as shown in FIG. 5, the invention may also be realized, for example, so that the inner surface 17a of the bores 17 formed into the roll mantle 11 are roughened. In this embodiment, the degree of roughness of the inner faces of the bores 17 is larger towards the second end of the bores 17, as compared with the first end through which the heating medium begins to flow through the bores 17. In this manner, it is possible to intensify the transfer of heat in the flow direction. This is, however, also more difficult to effect than the embodiment described above.
FIG. 4 shows a heatable roll provided with a displacement piece in accordance with the invention, which roll is denoted generally with the reference numeral 20. The roll 20 comprises a roll mantle 21 having a pair of opposite ends to which roll ends 23 and 24 are fixed. Roll ends 23,24 are provided with axle journals 25 and 26, respectively. The roll ends 23,24 are also provided with central through axial bores 27,28. In the interior of the roll mantle 21, a displacement piece 29 has been arranged. The displacement piece 29 is attached to the roll ends 23,24 by means of end pieces 30,31.
The diameter of the displacement piece 29 is smaller than the diameter of the interior of the roll mantle 21 so that an annular intermediate space 34 remains between the displacement piece 29 and the inner face of the roll mantle 35. Several through holes 32,33 have been formed into the circumference of both of the end pieces 30 and 31 of the displacement piece 29. Holes 32 and 33 are opened into the annular intermediate space 34.
The heating medium is introduced into the roll 20 through the axial bore 27 in the first roll end 23, from which it is passed through the holes 32 in the first end piece 30 into the intermediate space 34 between the displacement piece 29 and the roll mantle 21. In the intermediate space 34, the heating medium flows into the other end of the roll, from which it is passed through the holes 33 in the second end piece 31 into the axial bore 28 placed in the second roll end 24, and from there further out of the roll 20.
In the embodiment shown in FIG. 4, the coefficient of heat transfer from the flowing heating medium to the material of the roll mantle 21 is increased in the flow direction. This is accomplished by applying or producing a coating 3 on the inner face 35 of the roll mantle. The coating 3 is produced by any known process, e.g., by spraying, which coating is arranged so that the thickest portion of the coating is at the initial end of the flow, i.e. the end of the space 34 through which the heating medium enters. The thickness of the coating 3 is reduced in the flow direction towards the opposite end of the roll.
The coating 3 is made of a suitable insulation material, such as plastic or equivalent. Thus, at the initial end of the flow, where the temperature of the heating medium is highest, the thickness of the coating 3 that functions as an insulation layer is the largest. Therefore, the transfer of heat from the heating medium to the material of the roll mantle 21 is lowest at this point. In a corresponding manner, the thickness of the coating is reduced towards the other end of the roll, whereby the transfer of heat from the heating medium to the material of the roll mantle 21 becomes easier because the coefficient of heat transfer is higher. By means of this arrangement, the situation is achieved so that the temperature of the outer face 22 of the roll mantle is substantially uniform and invariable over the axial length of the roll.
In the embodiment of FIG. 4, in accordance with the invention, the change in the coefficient of heat transfer from the flowing heating medium to the material of the roll mantle can also be accomplished, e.g., so that the inner face 35 of the roll mantle is roughened so that its inner face is smoothest at the initial end of the flow and roughest at the final end of the flow.
In another embodiment, the insulation material 3 may consist of a net-like solution, or a tubular insulation, having an open area which increases towards the second and final end of the flow. Thus, the surface temperature of the roll mantle will be maintained substantially uniform because the heating medium cools as it progresses along the axial length of the tubular insulation. This is a result of the transfer of heat from the heating medium to the roll mantle through the tubular insulation. However, the coefficient of heat transfer will increase as the heating medium cools so that a substantially constant temperature will be present in the roll mantle.
In a corresponding manner, in the embodiments illustrated in FIGS. 1, 2 and 3, the tubes arranged in the bores in the roll mantle may be perforated, or have porous, net-like openings, i.e. so that the open area of the tubes or net is increased towards the second end of the roll.
The examples provided above are not meant to be exclusive. Many other variations of the present invention would be obvious to those skilled in the art, and are contemplated to be within the scope of the appended claims.
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The invention relates to a method for heating a roll and a heatable roll for use in a paper machine, paper finishing machine, or equivalent. The roll is heated by a heating medium which is introduced into the roll interior through at least one of the ends of the roll. The heating medium acts upon the material of the roll mantle or the roll and is arranged to flow across the axial length of the roll. The heating medium is arranged to flow out of the roll through either one of the ends of the roll. The roll is provided with means by which the coefficient of heat transfer from the flowing heating medium to the material of the roll is increased in the flow direction of the heating medium.
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This is a divisional of copending application Ser. No. 07/563,887 filed on 6 Aug. 1990 pending, which is a continuation of application Ser. No. 07/330,651 filed on 30 Mar. 1989 and now abandoned.
BACKGROUND OF THE INVENTION
In the past few decades, as both timber resources and available landfill sites have greatly diminished, the demand for recycling of printed papers, especially newsprint, has skyrocketed. Such recycling efforts have been aimed at developing processes whereby previously-used papers can be reprocessed and recycled for use. A major objective of such processes is the recovery of fibers which possess the physical properties and brightness of more expensive virgin pulp. End use considerations also play a major role in determining which parameters are critical for efficient recycling. Thus, for example, in newsprint ink holdout is of primary importance while in tissue, removal of fillers is critical to obtain a final product of satisfactory softness.
One major obstacle to the efficient recycling of such papers is the difficulties encountered in removing the ink from the printed paper before, during, or after the pulping process. This has become particularly difficult with newly developed inks and printing processes, which result in a much more tightly bound ink to the fibers. Improved deinking agents are needed to expand the utility of the deinking process.
The deinking process and deinking agents have been discussed in many articles (see e.g. Crow and Secor, Tappi Journal, July 1987, pp 101-100; Wasilewski, 1987 Pulping Conference Proceedings, pp 25-31; McCool and Silveri, 1987 Pulping Conference Proceedings, pp 33-39; and Gilkey et al., 1987 Pulping Conference Proceedings, pp 133-141). Briefly, all such processes involve the removal of the ink from the recycled paper by use of deinking agents such as detergents or surfactants, and the subsequent separation of this removed ink from the pulp. This separation is accomplished by washing, wherein the ink is dispersed in the aqueous system and removed with the water using mechanical processes such as centrifugation or screening, by flotation, wherein the ink is suspended in the aqueous system made hydrophobic, and subsequently "floated" away from the pulp in a froth (the froth is then drawn out of the system by a vacuum or mechanical overflow system), by mechanical means (flocculation, screening, centrifugation, etc.) or by a combination of these processes. Since none of these systems will completely remove all of the ink, the deinking agents must also contain compounds or functional groups which prevent redeposition of the removed ink on the cleaned fibers.
To date, deinking agents used in these processes have not satisfactorily fulfilled all these functions. For example, U.S. Pat. No. 4,518,459, Canadian Pat. No. 1,009,804. German Patent No. 2,903,150 and Japanese Patent Nos. 51,892/80, 117,690/82, 59,990/84, 155,794,85 and 117,690/82 disclose conventional detergents, and surfactants for use in deinking, whereas the use of a combination of surfactants and polymers is described in Japanese Pat. Nos. 75,889/86 and 85,089/87 and UK Pat. Application GB 2,178,079A (published Feb. 4, 1987). The mixtures produce a satisfactory gain in brightness of the pulp, but the pulp still contain residual ink, including large spots, which renders the pulp unsuitable for use in many applications.
Further, as new printing ink formulations and printing processes are developed, and the demand for recycling other types of waste papers (including films, foil coated papers, and pulp-colored papers) increases, there exists a real need for improved deinking agents which can effectively remove the printed ink from these furnishes.
SUMMARY OF THE INVENTION
It is an object of this invention to provide improved deinking agents which are capable of effectively removing ink from a recyclable paper leaving ink-free pulp suitable for incorporation in applications requiring high grade papers. It is further an object of this invention to provide deinking agents which can be used with a variety of printed media, including films, foil-coated papers, and pulp-colored papers.
The above and related objects are realized by the deinking agents of this invention, which are polyfunctional polymers of the two general formulas. The first formula is ##STR1## wherein: ##STR2## R 3 =H, or branched or straight chain C 1 -C 22 alkyl or alkylphenol
R 4 is H or C 1 -C 4 alkyl; ##STR3## (wherein R 5 is C 1 -C 4 alkyl or phenyl); W and Y=H or C 1 -C 4 alkyl; and ##STR4## (wherein M is ammonium or alkali metal, R 6 is C 1 -C 4 alkyl, and x is an integer of at least 1); or ##STR5## (wherein M is ammonium or alkali metal). When Z is the last compound, Y and W are preferably H and CH 3 , respectively. In the above agents: a and b are both positive integers of at least one and the ratio of a/b is 1/100 or greater; n is a positive integer of 10-100 and m=0-50 wherein the ratio of n/m is 1.5/1 or greater if m is not 0.
The second formula is ##STR6## wherein ##STR7## R 7 =C 6 -C 22 straight or branched chain alkyl or alkyl phenol and R 4 , W, Y, Z, a, and b are as above.
These agents are prepared by the reaction of an ethylenically unsaturated monomer with at least one surfactant macromonomer or hydrophobic monomer, and typically have molecular weights in the range of 2,000-100,000. Such agents can be added to the paper recycling mixture before, during, or after the pulping process, and are generally used at a treatment levels of 0.05%-1% (by weight based on the weight of dry pulp). These agents can be used in the flotation and wash and mechanical separation deinking processes, and will result in pulp of exceptional brightness, regardless of the deinking process used.
DETAILED DESCRIPTION OF INVENTION
The polyfunctional deinking agents of this invention comprise copolymers of ethylenically unsaturated monomers of the anionic type and one or more functional macromonomers. The macromonomers fall within three broad classes and, thus, the deinking agents comprise three classes of compounds.
Regardless of the class, the anionic-type ethylenically unsaturated monomers are of the following formula: ##STR8## wherein: W, Y are H or C 1 -C 4 alkyl
Z is selected from ##STR9## (in which case Y═H, and W═CH 3 ) wherein: R 6 is C 1 -C 4 alkyl, x is a positive integer of at least 1.
W and Y can be the same or different and are preferably H or CH 3 . Z is preferably ##STR10## and M is preferably sodium (Na).
In the first class of deinking agents, the ethylenically unsaturated monomer of the anionic type of copolymerized with at least one surfactant macromonomer. The surfactant macromonomers have one of the three following formulas: ##STR11## wherein: R is C 3 -C 22 alkenyl or carboxy alkenyl;
R 4 is H or C 1 -C 4 alkyl;
R 5 is C 1 -C 4 alkyl or phenyl. ##STR12## wherein: R 5 is the same as above;
R 3 is H or straight or branched chain C 1 -C 22 alkyl or alkylphenol;
Y is H or C 1 -C 4 alkyl. ##STR13## wherein R 5 , R 3 are the same as above.
In all of the above:
n is a positive integer of 10-100, preferably 20-50.
m is O or a positive integer of 0-50, preferably 4-20.
n/m is at least 1.5 when m≠0, preferably 2-3.
In this class of polymers, the amount of surfactant macromonomer copolymerized with the ethylenically unsaturated monomer is at least 10%, by weight, preferably 25-60%.
In the second class of functional polymers contemplated by this invention, the polymers are produced by the copolymerization of at least one (1) hydrophyllic surfactant macromonomer, at least one (1) hydrophobic monomer, and at least one (1) ethylenically unsaturated vinyl monomer of the anionic type.
The hydrophyllic surfactant macromonomers are of the three following formulas: ##STR14## wherein R=C 3 -C 22 alkenyl or carboxy alkenyl
R 5 is C 1 -C 4 alkyl or phenyl. ##STR15## wherein R 3 is H or C 1 -C 22 straight or branched chain alkyl or alkyl phenol and R 5 is as above. ##STR16## wherein Y═H or C 1 -C 4 alkyl an R 5 is as above.
The hydrophobic monomers are of the four following formulas: ##STR17## wherein R, R 5 , and Y are as above,
R 3 ' is C 1 -C 22 straight or branched chain alkyl or alkylphenol,
R 4 ' is C 1 -C 4 alkyl and R 7 is C 6 -C 22 straight or branched alkyl.
In this class of polymers, m and n are as defined above, the amount of hydrophobic monomer copolymerized is at least 1% by weight and the amount of hydrophyllic macromonomer copolymerized is at least 10% by weight. Preferably, the polymers comprise 2-5% hydrophobic monomer and 20-60% hydrophyllic macromonomer.
The third class of functional polymers contemplated by this invention comprises copolymers of at least one (1) hydrophobic macromonomer and at least one (1) ethylenically unsaturated monomer of the anionic type. The hydrophobic monomers are of the same formulas as the hydrophobic monomers of the second class and n and m are as in the first class. The amount of hydrophobic macromonomer copolymerized with the ethylenically unsaturated monomer is at least 1% by weight preferably 5-15%.
Regardless of the monomers used, the polymers produced have a molecular weight of at least 2000, preferably 5000-40,000. It is recognized, however, that the molecular weights can be increased as the particular applications dictate and, specifically, that polymers having molecular weights well in excess of 100,000 can be produced and utilized in deinking processes. The polymers can be produced by any convenient aqueous polymerization method, including solution polymerization in the presence of a suitable cosolvent, micellar polymerization, or emulsion polymerization. It is further contemplated that graft copolymerization methods can also be used to obtain functional polymers suitable for use in deinking. The actual method used will be dictated by personal preference, material availability and activity, as well as the properties of the particular monomers utilized.
The polymer produced can be used in any conventional deinking process including flotation, wash, and mechanical separation. Regardless of the process used, the polymer is added at a convenient time during the deinking process. Treatment levels range from 0.001 to 1% (by weight based on weight of dry pulp), preferably 0.01 to 0.7% by weight. However, these levels can vary depending upon the particular process employed, the particular furnish, and the particular functional polymer.
The functional polymers of this invention can be used with any furnishes which are commonly recycled (such as newsprint), as well as other furnishes such as laser printed papers, flexographic printed papers, pulp colored papers, foil-coated papers, plastic coated papers, etc. A list of commonly recycled papers is presented in circular PS-86 of the Paper Stock Institute of America (April, 1986, pp 4-8) incorporated herein by reference.
EXAMPLES
The following examples illustrate certain preferred embodiments of this invention and are not intended to be illustrative of all embodiments.
Example I Preparation of Deinking Polymers
Representative deinking polymers of this invention were prepared as described below.
Polymer A
In this example, a functional polymer comprising a surfactant macromonomer, monomethacrylate PEG 2000, and a vinyl monomer (acrylic acid) was prepared.
Briefly, a mixture of 450 g-deionized water and 20 g of isopropyl alcohol was charged to a 2 liter glass reactor equipped with a reflux condenser, stirrer, thermometer and two inlet ports for the addition of monomer and catalyst. After the mixture was refluxed for 10 minutes at 90° C., 300 g of a monomer mixture, comprising 100 g each of acrylic acid, monomethacrylate PEG (polyethylene glycol) 2000 (approx. 40 EO, mol wt.=2000) and deionized water, and 80 g of 1.875% aqueous sodium persulfate solution were continuously pumped into the reactor while the temperature was maintained at about 90±2° C. The system was then incubated at 90±2° C. for an additional 30 minutes, after which a 40 g charge of 2.5% aqueous sodium persulfate was added. The reaction mixture was subsequently maintained at 90+2° C. for an additional hour, and then neutralized to pH 7 with 50% caustic soda. The neutralized product was subsequently vacuum distilled, removing 70 g of distillate, and leaving viscous, clear straw-colored liquid product, with a solids content of 29.7% and a pH of about 7.0. The polymer produced had a weight average molecular weight (M.W.) of about 100,000 (as measured by gel permeation chromatography using sulfonated polystyrene as the standard). This was retained as Polymer A.
Polymer B-1 and B-2
In this example, a second functional polymer containing allyl alcohol ethoxylate (24 EO) and acrylic acid was prepared. Briefly the procedure followed was identical to that used in the preparation of Polymer A, except that the acrylic acid/allyl alcohol ethoxylate (24 EO) ratio was 80/20. Two preparations were made, differing in the amount of catalyst used. The products obtained had solids contents of 27.5% and 29.7% and respective weight average molecular weights of 75,000 (B-1) and 25,000 (B-2).
Polymer C
In this example, a functional polymer containing acrylic acid and allyl alcohol ethoxylate (44 EO) was prepared following the procedure of Polymer A. The weight ratio of acrylic acid to allyl 44 EO was 80/20.
The product had a solid content of 31% and a weight average molecular weight of 23,000.
Polymer D-1 and D-2
In this example, functional polymers derived from two anionic vinyl monomers (acrylic acid and maleic acid) and a hydrophobic monomer (t-octylacrylamide) were prepared. The formulations were as follows:
______________________________________Material D-1 D-2______________________________________A. toluene 250 g 250 g maleic anhydride 49.1 g 49.1 gB. toluene 70 g 70 g acrylic acid 71.5 g 69.9 g t-octyl acrylamide 1.4 g 5.5 gC toluene 35 g 35 g benzoyl peroxide 2.4 g 2.4 gD distilled water 400 g 400 g aqueous NaOH (25% W/V) 230 ml 230 ml______________________________________
Initially, the A part was charged to a 2 liter flask equipped with a thermometer, two addition funnels, stirrer, thermometer, and reflux condenser, and the system was heated to reflux; subsequently B and C were both slowly added simultaneously (B over 3 hours, C over 5 hours) with stirring. Once the addition was complete, the system was refluxed an additional 2 hours (a precipitate formed during this time), after which D was added. The toluene was then steam stripped from the system, and the pH was adjusted to 7.0-7.5.
Product D-1 had a solids content of 15.4% and a weight average molecular weight of 24,400, while D-2 had a solids content of 19.4% and a molecular weight of 20,200.
Polymer E
In this example, functional polymers derived from a surfactant monomer (allyl alcohol ethoxylate, 44 EO), a hydrophobic monomer (tridecyl methacrylate) and an anionic vinyl monomer (acrylic acid) were prepared. Briefly, a mixture of 450 g deionized water and 150 g n-propanol was charged to a 2 liter glass reactor equipped with a reflux condenser, stirrer, thermometer and two inlet ports for the addition of monomers and catalyst. After the mixture was refluxed for 10 minutes, a monomer mixture (comprising 135 g acrylic acid, 44 g allyl alcohol ethoxylate, 40 g deionized water, and 5 g tridecyl methacrylate) and 80 g of 1.25% sodium persulfate solution were continuously pumped into the reactor simultaneously over a period of three (3) hours, while the reaction temperature was maintained at 85° C. The system was subsequently incubated at 85° C. for an additional 10 minutes after the addition was complete, after which 20 g acrylic acid was pumped in, followed by 20 g of 2.5% sodium persulfate solution. The system was subsequently maintained at 85° C. for another hour, after which the reactor content was cooled to about 50° C. and neutralized to pH 7 with 50% caustic soda. The neutralized product was subsequently vacuum distilled to remove 280 g distillate, 50 g of deionised water was then added to form the final product, which was a white viscous liquid with a solids content of 28%. The polymer had a weight average molecular weight of 39,000.
Example II Deinking Procedures
The above polymers were subjected to testing in flotation and wash deinking systems using the following procedures:
Flotation
The flotation procedure utilized a standard Wemco cell. Briefly, 1910 ml water was heated to 40°-45° C. and charged to a Waring blender. Subsequently, the following is charged:
______________________________________a) Sodiun Silicate 1.0 mlb) 35% Sodium Peroxide 2.8 mlc) 50% NaOH 2.0 mld) DTPA (Kalex Penta) 0.15 mle) Polymer as per test______________________________________
and the system is mixed for one (1) minute. A total of 92 g paper (69 g newsprint, 23 g magazine) is added, and the entire system is pulped in the blender at high speed for 2 minutes, followed by low speed for 8 minutes.
The resultant pulp is then diluted with 5750 ml water at 40°-45° C., and transferred to the Wemco cell and frothed at 800 rpm for 5 minutes; the foam is collected from the system during this time through an outlet and 500 ml water is added to the system each minute to compensate for the foam removed. The amount of foam collected (in ml) is recorded and, after drying, the amount of fiber collected is determined (this is reported as a % of total fiber).
A pulp "pad" is then formed by filtering 1 liter of pulp on a Buchner funnel (through #4 paper) and subsequently pressing on a steel patten. The pads are evaluated for brightness by measuring reflectance on the Technibrite Micro TB-1C analyzer; this value is reported as a % of the reflectance of the MgO standard. This value is compared with the brightness of the raw pulp (pulper) and the gain in brightness is calculated. In general, the greater the gain in brightness, the better the degree of ink removal.
Wash
In this system, 1910 ml of water (as in the flotation procedure) is mixed with
______________________________________a) DTPA (Kalex Penta) 1.0 mlb) Sodiun Silicate 0.85 mlc) Polymer as per test______________________________________
for one minute. A total of 88 g newsprint is added, and the system is pulped as in the flotation procedure.
The deinked pulp is concentrated by straining through cheese cloth and manually squeezing dry. Fifty (50) g of this pulp is diluted with 2 liters of distilled water and disintegrated for 5 minutes in a standard commercial disintegrator. One (1) liter of this mixture is then filtered on a Buchner funnel and pressed on a steel patten, as in the flotation procedure to form a pad. The pad is examined as in the flotation procedure.
Example III--Flotation Deinking Test
To assess the utility of the polymers of this invention in the flotation deinking process, a variety of polymers were compared with those listed in Example I at different treatment levels. The procedure followed was that of the flotation described in Example II. The results are presented in Table I.
TABLE I__________________________________________________________________________Summary of Flotation Deinking Test ResultsBrightness (TAPPI) Fiber Foam Treatment Level After Finished Gain in Loss Collected (% wt. based onSample Pulper Pulp Brightness (%) (ml) dry pulp)__________________________________________________________________________I.sup.1 48.7 52.3 3.6 2.6 -- 0.20II.sup.2 51.2 55.7 4.5 3.7 850 0.20Polymer A 55.3 59.6 4.3 4.5 1150 0.20Polymer 54.2 57.6 3.4 4.3 1175 0.20B-1Polymer C 54.5 57.8 3.3 3.9 1000 0.20Polymer E 53.4 57.8 4.4 -- -- 0.20I.sup.1 53.1 56.2 3.1 4.3 -- 0.06II.sup.2 51.2 54.6 3.4 -- -- 0.06Polymer A 52.6 57.8 5.2 -- -- 0.06Polymer 52.1 56.9 4.8 -- -- 0.06B-1Polymer C 50.2 53.9 3.7 3.2 -- 0.06Polymer 51.7 56.1 4.4 -- 1200 0.06D-1Polymer 54.0 59.2 5.2 -- 1500 0.06D-2III.sup.3 52.0 56.2 4.2 4.1 1200 0.01IV.sup.4 52.2 56.0 3.8 3.7 1200 0.01Polymer A 53.0 57.8 4.8 5.0 1030 0.01Polymer 53.1 61.0 7.9 4.6 1225 0.01B-1Polymer 50.4 55.9 5.5 -- -- 0.01D-2Polymer A 50.0 58.4 8.4 4.0 1200 0.03Polymer 50.7 57.8 7.1 4.3 1250 0.03B-1__________________________________________________________________________ Notes .sup.1 A surfactant of the formula C.sub.16-18 H.sub.33-37 O (EO).sub.13 (PO).sub.6.5 H (EO = ethylene oxide, PO = propylene oxide) .sup.2 A commercial surfactant deinking agent. .sup.3 A surfactant of the formula C.sub.12-15 H.sub.25-31 O (EO).sub.9 H .sup.4 A surfactant of the formula C.sub.12-15 H.sub.25-31 O (EO).sub.4.5 (PO).sub.7 H
As shown, it can be seen that, at low treatment levels (below 0.20%), the polymers of this invention give a much better gain in brightness than the commercial surfactants. This indicates that a lower amount of deinking agent is required to obtain good ink removal.
Since some commercial surfactants are now used in conjunction with an accelerator or "auxilliary aid" to accomplish deinking, a series of experiments were conducted using such an aid, the sodium salt of polyacrylic acid (PAA) with commercial surfactants. The results are presented in Table II.
Again, it can be seen that the gain in brightness produced by the polymers of this invention is better than the gain observed with commercial agents, with or without the accelerators, even at very low treatment levels.
TABLE II__________________________________________________________________________Summary of Accelerator Test Results Ratio of Deinker/ Brightness (TAPPI) Fiber Treatment Level Accel. After Finished Gain in Loss (% by wt.) onDeinker Accel. (by wt.) Pulper Pulp Brightness (%) dry pulp)__________________________________________________________________________I None -- 53.1 56.2 3.1 4.3 0.06II None -- 51.2 54.6 3.4 -- 0.06Polymer A None -- 52.6 57.8 5.2 -- 0.06Polymer B-1 None -- 52.1 56.9 4.8 -- 0.06I PAA 20/80 54.4 57.7 3.3 3.6 0.06 (2,000 M.W.)I PAA 20/80 54.6 58.0 3.4 3.9 0.06 (90,000 M.W.)II PAA 50/50 55.4 57.7 2.3 -- 0.06 (2,000 M.W.)II PAA 80/20 51.4 54.2 2.8 -- 0.06 (90,000 M.W.)II Polymer A 80/20 53.3 56.9 3.6 -- 0.06II Polymer B-1 80/20 54.8 57.3 2.5 -- 0.06I Polymer A 50/50 52.7 56.3 3.6 3.6 0.06I Polymer B-.sub.-- 50/50 52.6 55.4 2.8 3.5 0.06I None -- 55.3 58.6 3.3 4.2 0.03Polymer A None -- 50.0 58.4 8.4 4.0 0.03Polymer B-1 None -- 50.7 57.8 7.1 4.8 0.03__________________________________________________________________________
Example IV Deinking of Laser Printed Paper
To assess the utility of the functional polymers of this invention in deinking laser printed papers, experiments were conducted following the procedure of Example III, except that laser printed paper was used. The results are presented in Table III.
TABLE III__________________________________________________________________________Summary of Laser Print Test ResultsBrightness (TAPPI) Fiber Foam Treatment Level After Finished Gain in Loss Collected (% wt. based onSample Pulper Pulp Brightness (%) (ml) dry pulp)__________________________________________________________________________B-2 74.06 82.07 8.01 4.40 1100 0.20C 79.95 86.97 7.02 4.66 1000 0.06C 74.63 82.69 8.06 3.48 1010 0.12__________________________________________________________________________
As shown, it can be seen that desirable gains in brightness are observed, even at low treatment levels.
Example V Wash Deinking Test
To assess the utility of the polymers of this invention in a wash deinking process, Polymers A and B were compared with two commercial surfactants following the procedure of Example II (treatment level=1.0% by wt. using newsprint). The results are presented in Table IV.
TABLE IV______________________________________Summary of Wash Test Results Finished PulpSample Brightness______________________________________C.sub.12-15 H.sub.25-31 O (EO)9.sub.H 58.4C.sub.12-15 H.sub.25-31 O (EO)4.5 (PO).sub.7 H 58.4Polymer A 61.3Polymer B-1 60.5______________________________________
As shown, it can be seen that the polymers of this invention produce brighter finished pulp.
It is apparent that many modifications and variations of this invention as hereinabove set forth may be made without departing from the spirit and scope thereof. The specific embodiments are given by way of example only and the invention is limited only by the terms of the appended claims.
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This invention presents a series of polyfunctional polymers useful as deinking agents. The polymers, which generally have molecular weights in the 2,000-100,000 range, can be used to effectively separate and remove ink in a variety of deinking processes, including flotation, wash, and mechanical, resulting in fibers of superior brightness.
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RELATED APPLICATIONS
[0001] The present application claims benefit of priority to U.S. Provisional Application No. 61/080,799, filed Jul. 15, 2008, which is incorporated herein by reference in its entirety.
BACKGROUND OF THE INVENTION
[0002] The present invention generally relates to information systems, and more specifically, to an electronic voting system.
[0003] Earlier electronic voting systems did not have the capability to produce a paper trail of votes cast. They did not allow for nor could they produce a voter verifiable way to insure that for each and every voter that voted, that their votes were: 1. Correctly and accurately recorded in the first place. 2. Correctly and accurately counted in the second place. 3. Verifiable by each individual voter before they left the voting location. 4. No erroneous voter induced over votes or under votes. 5. No erroneous system induced over votes or under votes. 6. No erroneous poll worker induced over votes or under votes. 7. No erroneous computer programmer induced over votes or under votes. 8. No intentionally induced over votes or under votes. 9. No accidentally or intentionally erased votes. 10. No accidentally or intentionally erased vote totals or results. 11. Absentee ballots were not mis-mailed, lost or misplaced.
[0004] No computerized electronic voting system has the capability to allow voters to vote, in a secure way, over the internet.
[0005] As can be seen, there is a need for an improved system for voting.
SUMMARY OF THE INVENTION
[0006] In one aspect of the present invention, a device for transmitting a ballot from a voter includes: a display; a data input device; a biometric input device; a case having an open and a closed position, the case protecting the display, the input device, and the biometric input device in the closed position, the case making the display, input device and biometric input device accessible by the voter in the open position; a communications medium; a microprocessor to control the display, the data input device, the biometric input device, and the communications medium; and a power supply that accepts alternating current and provides direct current to the microprocessor; wherein the device utilizes the biometric input device to validate the identity of the voter, utilizes the data input device to receive the ballot from the voter, and utilizes the communications medium to transmit the ballot.
[0007] In another aspect of the present invention, a system for voting includes: a secure computer having a database containing voter registration information; a data communications network; and a plurality of voting terminals, each voting terminal including a biometric input device, each voting terminal in communication with the secure computer utilizing the network; wherein each voting terminal validates the identify of a voter utilizing the biometric input device and the database, accepts a ballot from the voter, and transmits the ballot to the database over the network; and the secure computer tallies the ballots in the database.
[0008] In yet another aspect of the present invention, a method for voting includes: providing a voting terminal; providing a centralized database; verifying a voter's identity utilizing the voting terminal and the database; receiving ballot information from the voter utilizing the voting terminal; and communicating ballot information between the voting terminal and database.
[0009] These and other features, aspects and advantages of the present invention will become better understood with reference to the following drawings, description and claims.
BRIEF DESCRIPTION OF THE DRAWINGS
[0010] FIG. 1 depicts a perspective view of an embodiment of a voting terminal according to the present invention;
[0011] FIG. 2 depicts a perspective view of an embodiment of a voting terminal according to the present invention with legs extended;
[0012] FIG. 3 depicts a top plan view of an embodiment of a voting terminal according to the present invention;
[0013] FIG. 4 depicts a side elevational view of an embodiment of a voting terminal according to the present invention in the use position;
[0014] FIG. 5 is a block diagram of an embodiment of a voting system according to the present invention; and
[0015] FIG. 6 is a flow chart of an embodiment of a voting system according to the present invention.
DETAILED DESCRIPTION OF THE INVENTION
[0016] The following detailed description is of the best currently contemplated modes of carrying out exemplary embodiments of the invention. The description is not to be taken in a limiting sense, but is made merely for the purpose of illustrating the general principles of the invention, since the scope of the invention is best defined by the appended claims.
[0017] Various inventive features are described below that can each be used independently of one another or in combination with other features. However, any single inventive feature may not address any of the problems discussed above or may only address one of the problems discussed above. Further, one or more of the problems discussed above may not be fully addressed by any of the features described below.
[0018] Broadly, an embodiment of the present invention generally provides an electronic voting system. Embodiments include a voter database identification system, a voter identification verification system, a voter election system, and an election verification system. Embodiments may be called “Voter ID Election Verification System” or “VideVs.”
[0019] An embodiment of the present invention is an end to end computerized electronic voting system including a central computerized voter registration database, a wide area network (WAN) data communications network and electronic voting terminals housed in compact lightweight cases that also function as convenient stands for the voting terminals. An embodiment is an improvement to existing computerized electronic or paper based voting systems in use today. An embodiment addresses the present systems' deficiencies in a way that allows for a voter verified paper trail, multiple same ballot re-voting, a paper audit trail, ‘same way’ legal re-counts, secure internet absentee voting and Help America Vote Act (HAVA) compliant voting. This can be without the need for paper ballots, optical scanners, terminal printers, mailed absentee ballots and voter photo ID's, while maintaining the integrity of the secret ballot.
[0020] An embodiment of the present invention is a voting system with four main functions: a voter registration database/ID system, a voter ID verification system, a voter election system, and an election verification system.
[0021] Embodiments of the present invention may include the following:
A centrally located secure mainframe computer. This may be located at the local County Supervisor of Elections (SOE) office. On this mainframe or other computer is stored, in a machine readable format, the complete voter registration database of voter information. This mainframe computer is also used during elections to store and distribute all the various web based ballot pages for the voters to vote on. This mainframe computer also stores the complete voting record of every vote and ballot cast using this VideVs system. It is also used to store and tally votes and vote totals for election results. The computer is referenced herein as a “mainframe” in that it is a sufficiently powerful computer platform to perform these operations. A computerized voter registration database. This database is also on the mainframe computer in a machine readable format. This is a database of all registered voters and voter specific information (VSI) such as names, addresses, party, age, race, etc., and other demographic information as mandated by law and the SOE office. Also stored in this database is a voting record of votes cast or left blank, using this VideVs voting system, by every voter. Two live real time copies of this database are directly connected to the mainframe computer and a third and forth off line duplicate copies serve as backups one on site, one off site for security reasons. A county wide area network (WAN) data communications network. This may be a county network system of hardwired landlines, fiber optic cables and or wireless backbones or any combination of these as used by the county to communicate with and conduct county related day to day business with all public access county buildings and locations throughout the county. This may include buildings such as schools, libraries, courthouses, county government offices, parks and recreation centers, police and fire stations, etc. Voting terminals. These voting terminals are located throughout the county at WAN connected public access locations, voting centers, etc.
[0026] As depicted in FIGS. 1 , 2 , 3 and 4 , embodiments of a voting terminal 10 may include the following.
A storage/carrying case 12 . As seen in FIG. 1 , the cases 12 have an inter-locking design which makes them stackable. Each inter-locking design stackable case is of suitable size to house all the internal components. It can be larger or smaller as needed but in a preferred embodiment, each case may be approximately 24″×24″×3→ (L×W×H) when closed up as depicted in FIG. 1 . It may be made of a durable lightweight high strength plastic material. Any number of materials can be used for this but a preferred material may be injection molded high density nylon or HDPE plastic. Four integrated telescoping aluminum, or similar strength lightweight material, legs 14 of one basic design. The four legs 14 fold up inside the bottom of the case such that the two front legs become convenient side carrying handles. Each case, when opened for voting, can also sit flat on a table to allow easy access for voting by handicapped or wheelchair voters. An integrated AC/DC power supply provides a convenient AC outlet for another voting terminal, as depicted in FIG. 3 . An embodiment includes a power supply to power all internal electric components plus two power “good” indicator lights: an amber “AC Good” light 24 for alternating current and a green “DC Good” light 26 for direct current. A flat panel LCD display screen 16 . Three folding privacy screens that fold up to help cover and protect the LCD display screen when not in use, as depicted in FIG. 4 . A microprocessor controlled electronic system board 28 similar in form and function to those found in laptop style computers, as depicted in FIG. 5 , with the following integrated parts: four USB ports 29 ; a high speed Ethernet communications port 32 used for data communications with the mainframe computer 34 ; a bootable solid state (USB) storage device 30 with a preloaded machine readable microcode program for the initial system startup, operating system, display system, biometric finger scanner, and data communications with the mainframe computer. In an embodiment, no votes, vote totals, or voter information need be stored in the voting terminal, so that no direct recording electronic (DRE) is required. Electrical interconnection cables for data, signal and power, between the system board 28 , the display device 16 , the finger scanner 18 and the voter controlled input device. A network data communications cable. In an embodiment, Ethernet is the preferred communications medium between the voting terminal and the mainframe computer. A voter controlled input selection device. This can be combined with the display to produce a touch screen display 16 . Other embodiments use a tethered stylus, a tethered mouse, a wireless mouse, a wireless stylus, a touch pad or any number of alternative input selection devices that can be controlled by the voter. An AC power cord 20 . A biometric identification (ID) input device 18 . As depicted in FIG. 3 , the preferred method used is a finger scanning input device 18 that can be integrated into the voting terminal or located external to it but still inside the carrying case and hardwired into the terminal.
[0038] An embodiment of a voting terminal 10 may weigh approximately 8 lbs. when fully assembled with case 12 , telescoping folding legs 14 , a power supply, an AC electric cable 20 , an Ethernet data communications cable or port 32 , a biometric input device 18 and a touchscreen 16 or other voter controlled input selection device (not shown).
[0039] It should be further noted that any suitable combination of similar form and function components can be substituted and or used in place of the preferred ones listed herein as long as they provide for the same basic operation and function as those listed here. Many such similar components would come to mind of anyone skilled in the art and would be suitable substitutes for those described herein.
[0040] In an embodiment, basic operation of the present invention is as follows. The terminals are setup as depicted in FIGS. 2 and 4 in County government public access buildings, libraries, schools, parks, courthouses, etc., and other county network WAN connected public access buildings, voting centers and or precincts. Each terminal 10 is network connected through the county network/backbone back to a central computer 34 at the Supervisor of Elections (SOE) voting center.
[0041] In an embodiment, each terminal's internal hardware MAC address is pre-loaded into the network operating system (OS) that runs on the mainframe computer. Each machine MAC address becomes a valid user ID. Only these preloaded valid user ID's are allowed to login into the voting network. At power up each voting terminal runs a pre loaded machine readable microcode program that is stored on the internal USB boot device 30 . This initiates all internal devices, the display system 16 ; the voter controlled input selection device, and the biometric ID device 18 . It also initiates the network login and data communications to the mainframe computer. The terminal 10 then automatically logs into the network utilizing its internal hardware MAC address as a valid user ID. After the terminal establishes communications with the Supervisor of Elections mainframe computer it is now ready for voters to vote on it.
[0042] As depicted in the flowchart of FIG. 6 , to vote on an embodiment of the system, a voter walks up to any open terminal and initiates a voting session by touching the screen 16 . This is the preferred method when the terminals are configured with a touch screen 16 as the voter controlled input device. Alternate embodiments may have an additional attached input device, such as a keyboard (not shown). The voter then receives a visual prompt on the display screen, from the mainframe computer, to place their index finger on the biometric finger scanning input device 18 . The finger scan is sent back to the Supervisor of Elections (SOE) mainframe which then searches its database records for a match comparing it to all the other finger scans on record. While searching for a match, the mainframe computer sends the voter an electronic image of an on-screen keyboard. The voter is asked by the mainframe to use the onscreen keyboard to enter their correct name and address. The SOE mainframe system verifies the name and address with those found on record from the finger scan match. It then presents the voter with a copy of the correct web page ballot(s) for that voters' party affiliation, language, precinct, district, city, etc., that the voter resides in, for them to vote on. Ballot layout and designs may or may not be determined by local or state laws, and or the County SOE office.
[0043] In an embodiment, the voter makes selections on the touch screen for each issue. Write-in selections may be done via an on screen keyboard. Selections are transmitted in real time back to the SOE mainframe. No votes are kept in or stored in any of the voting terminals. If any items on a ballot page are left blank the voter receives a pop up message window on the display screen. In this pop up window the voter must confirm that it is their intention to leave some items blank before they are allowed to go on to the next page. After the voter has been presented with all appropriate ballot pages and has indicated his or her selections, they are then presented with a final summary screen(s) that shows all selections, blanks, etc., for all issues. Before casting a ballot the voter receives a final option to change/correct or leave it blank. After making final selections the voter receives a final pop up warning about any blank items still left on the ballot at which time the voter must indicate, in this pop up window, that it is their intention to leave them blank. To cast their ballot the voter receives a second prompt (not shown) to place their finger on the biometric finger scanning input device. The second scan is sent back to the mainframe which compares it with the voters first finger scan. The two scans must match to successfully cast a ballot. The mainframe then saves the voters selections in that voters personal database record and then sends back a “Thank You for Voting, your vote has been counted,” or a similar type acknowledgement message to the voter (not shown). Any interruption in this voting process such as a power outage or data communications error, prior to the mainframe recording the voters' ballot, results in no change in the voters' voting record. It is as if they haven't yet voted and are free to do so at any time. This feature of the system protects the voter and their right to vote in the event that there is any kind of interruption in the electronic voting process before it can be completed.
[0044] In an embodiment, the internal electrical components can be housed in any number of different case/terminal designs based on size, function, use, and portability. It can incorporate different internal components for different options and various screen sizes for different functions/results. Such flexibility of design will allow anyone skilled in the art to maximize functionality and usability for their specific device. However it is built and configured, whatever components are used its underlying basic function is to allow a biometric personally secure identification method whereby an individual can use this method, as a unique key, to lock and unlock access to only his or her own individual confidential personal database record information via the same biometric ID access method. Any agency or business with a large or ever growing database of individual confidential personal information and records such as doctors, lawyers, hospitals, law enforcement agencies, insurance companies, state, local and federal government agencies, and more, could utilize a system such as this to allow only each individual to lock or unlock any such access to their confidential database record of personal information. Embodiments will focus primarily on the use of this system as a computerized electronic voting system.
[0045] Embodiments provide an electronic voting system. The invention is not limited in scope to only this use. The uses mentioned herein are provided to illustrate a very few specific uses and are not intended to convey only these few uses. They are meant to convey the broad range and scope of the many possibilities of use to those skilled in the art. Indeed many different uses, besides those few mentioned herein, may come to mind to anyone skilled in the art. Many different forms of design and functional use will come to mind of anyone skilled in the art. Indeed many other possible variations and modifications of physical size and functional use should not be limited to only those listed herein. Many such alternative forms of physical design and functional use will pertain to this invention and are intended to be covered by this disclosure, the illustrative drawings and the numerous claims mentioned herein.
[0046] In an embodiment, each voter registers with a unique voter specific biometric key used to lock and unlock access to only their record. The preferred biometric key for this invention is a finger scan. When the voter registers and presents a finger scan the mainframe computer searches its database record of all other finger scans comparing each voter's finger scan to all others in the system. SOE personnel then process each voter accordingly. Due to the design of the database, any SOE database searches by SOE personnel will only display a voters name, address and precinct number. The database is structured this way in order to protect the integrity of the secret ballot and to keep confidential all voter specific information (VSI) and all individual voting records. Each voter must unlock his/her record to allow any such SOE access in order to view, print or change any VSI information.
[0047] In an embodiment, voting records cannot be viewed by SOE personnel or changed by anyone after an election is closed. Each voter presents their biometric key, in this case a finger scan, to vote on any active voting terminal. Because of the database structure and the centralized location of the mainframe computer, voting can be done on any voting terminal anywhere. Voters are no longer restricted to having to vote in a specific assigned location or precinct.
[0048] An embodiment of the system is also Help America Vote Act (HAVA) compliant with an audio ballot feature. This can be accomplished any number of ways. The preferred method is with the voter listening on headphones attached to an audio voting station. Voting is conducted by each voter listening to prerecorded MP3 or other suitable audio wave files of the entire ballot with suitable pauses and audio prompts with the voter indicating their selections by touching the screen anywhere using the touch screen like a giant yes/no button to make their selections known to the system. Voter selections are transmitted to the mainframe, recorded and an acknowledgement is then transmitted back to the voter via an audio response system that the voter hears in the headphones.
[0049] Each total election record, of all votes cast, becomes a permanent read only record of votes locked into the mainframe database record once the polls close and all eligible voters have voted with the mainframe storing a complete record of the election in all copies of the database. Once a voting record is locked by the SOE it can only be read and never changed or modified in any way.
[0050] The county can also generate revenue by charging and collecting fees for database searches of demographic and voting records. The collecting of any such fees would generate a revenue stream for the county. Due to the design of the database structure all demographic and voting record information is not specifically connected to each individual voter and as such is not VSI information. Therefore the integrity of the secret ballot is maintained.
[0051] An embodiment of an electronic voting system addresses existing short comings in the following ways. First of all the database design of voter registration, demographic and voting record information allows the system to function as described herein. Any such database of individual personal information records can be structured this way. This allows only the individual presenting their biometric ‘key’ to lock and unlock access to only their record of information. This is the preferred method of storing and accessing personal database information for the electronic voting system.
[0052] In an embodiment, each individual voter's record is structured like a pyramid. The top most level is the voters' name, address and city, which determines their corresponding voting precinct number. The next level down is that voter's biometric ID key. It can be a finger print, a finger scan, a retinal scan, a voice print, a series of security questions and voter supplied answers or any combination of these and or others. The preferred method used for this invention is a finger scan with further security hashing steps implemented by the mainframe. It is as unique an ID method to the individual as a finger print. However it is not a finger print and the finger scan cannot be reverse engineered to produce the finger print that generated it. This is a secure database ID system for the voting system. This finger scan ID key locks and unlocks the individuals name and address information to the pyramid of database records below it.
[0053] The next level down in an embodiment of the pyramid record is Voter Specific Information (VSI). This is personal information about that voter listed above it. Information such as but not limited to the following: age, date of birth, race, national origin, nationality, party affiliation, voting handicaps, language, citizenship status, convicted felon, etc. This is personal information required by the SOE office in order for that person to be legally registered to vote. Below this level of personal information are multiple separate layers of voting records, one for each election, for every past election conducted using an embodiment. One layer for each election held that the voter voted in or not. The pyramid database of information grows from the bottom downward. For every subsequent election a new layer is added to the bottom of the previous layers.
[0054] When the individual voter presents their biometric ‘key’ their demographic and voting records become directly connected to the voters' name. This makes all such information Voter Specific Information (VSI) and as such viewable by only the voter to verify their votes as cast or SOE personnel to assist with changes to only the demographic portion of that information. This may allow each voter the opportunity to see and verify their votes as cast while at the same time it also protects the confidentiality and integrity of the secret ballot system.
[0055] In an embodiment of a voting system there are no internal ballots to load or program into each and every terminal or to activate at the time of voting for each and every voter. Ballots are web based like internet web pages. The content and format must follow SOE, State and local guidelines for layout and content. They are programmed and loaded into the mainframe computer at the SOE central location.
[0056] An embodiment of the voting system allows for last minute changes of any ballot page right up to whenever voting actually starts and the local laws allow for. Any ballot changes are made to a master web page ballot on the SOE mainframe computer.
[0057] With an embodiment of a voting system there need not be any more dead candidates on the ballot because it was too late to change the wording. With an embodiment of a voting system there need not be any more withdrawn candidates on the ballot. With an embodiment of a voting system there need not be any more votes mistakenly cast. With an embodiment of a voting system there need not be any more “yes” to vote no or “no” to vote yes confusion because it is too late to change the wording of ballot issues.
[0058] An embodiment of a voting system is multi-language capable. Foreign language web pages can be designed as necessary for each and every foreign language as required.
[0059] Because ballots are controlled and transmitted from the central mainframe computer, with an embodiment only one ballot design is necessary for each language allowed for any national, state, county, district/precinct, or city/municipality elections.
[0060] An embodiment of a voting system is HAVA compliant with special audio feature terminals.
[0061] With an embodiment of the database design the correct precinct specific ballot, in the appropriate voters' language, is transmitted to each individual voter to vote on. Because of this capability voters are no longer restricted to voting in a specific location or precinct. This helps prevent voting in the wrong precinct, sending voters to a different precinct to vote, and last minute voters turned away because they came to the wrong precinct to vote. Any voter can vote anywhere on any terminal.
[0062] Embodiments of voting terminals can go anywhere. They are no longer precinct specific.
[0063] With an embodiment of a voting system no internal votes are stored in the terminals. Voting and vote recording is done in real time on the mainframe computer. Because of this there are no internal votes or vote totals in each terminal to download or copy to another device and transmit or transport to the central SOE office.
[0064] With an embodiment of a voting system there is no need for any more voting terminal security seals. Special tracking numbers are no longer necessary.
[0065] With an embodiment of a voting system there are no internal printers in each terminal to jam or malfunction. There are no recurring costs for ink, ribbons, paper or other internal printers, printer supplies or printer parts.
[0066] With an embodiment of a voting system multiple voting by a voter is not possible. The database design associates each individual voter to their own individual electronic ballot: “one person—one ballot−one vote.”
[0067] With an embodiment of a voting system it is possible for each and every voter to revote and change their vote, as local election laws allow for, again and again until the polls close. Each individual's ballot is tied to one and only one voter.
[0068] With an embodiment of a voting system this ballot to voter relationship allows the SOE the capability to trace each and every vote back to the individual voter that cast it with complete integrity of the secret ballot system. This capability allows each voter to check and verify only their own individual vote.
[0069] With an embodiment of a voting system the individual voting record is locked by the voter with their unique biometric key. A voting location, date, time stamp, and terminal number are also locked in each time a vote is cast.
[0070] With an embodiment of a voting system the complete voting record is locked permanently by the SOE when the polls close and the last voter has voted. There is no longer the need for printing hundreds of thousands of paper, absentee, provisional or optical scan ballots. There are no more printing errors on any ballots because there are no more printed ballots for either regular or absentee voting. Consequently there are no more incorrectly worded ballots mailed out. There are no more mis-mailed blank or incorrect ballots. There are no more postage, handling or print costs associated with paper or absentee ballots. There are no more last minute rush mass mailings. There are no more handling, sorting, processing, validating, hand counting, double counting etc. or storing of absentee ballots. There are no more lost or misplaced absentee ballots. There are no more uncounted absentee ballots.
[0071] An embodiment of a voting system allows for secure absentee voting via the internet. This capability enables overseas and military voting. There are many possible ways for absentee voters to vote. With an embodiment of the electronic voting system the preferred method for absentee voters to vote is as follows. Voters are mailed an authorization card with a security number generated from their unique biometric finger scan in order to login and vote. Absentee voter's login into a secure website. The voter must then enter their name and address and any additional security information required to verify their ID or answer a pre determined number of security questions. Absentee voters vote on the same web page ballots as the polling place voters do. They click a mouse on their selections and cast their ballot with a final security question.
[0072] In an embodiment, because of the biometric database design there is no more waiting in line at precincts or polling places to check voters picture ID's or signatures. ID verification is done in the mainframe computer real-time before each voter votes.
[0073] An embodiment of a voting system also has a paper trail feature. Even though there are no printers in any terminals or any sort of paper ballots whatsoever. This is accomplished in the following way. After a voter casts their ballot they can go to the SOE clerks on site in each voting center and request a printed copy. The clerk asks the voter to step up to a voting terminal and unlock their record with a biometric finger scan just like they did to vote. When the voter unlocks their voting record it is disconnected from the database and connected to their name. It now becomes voter specific information (VSI) directly connected to the voter's name. This direct connection to the voters' name allows only the voter to see their voting record. The SOE clerk cannot see the voting record. Thus the database design and biometric key access insure the integrity of the secret ballot and protects all voters voting records whenever the record is unlocked by the voter. The voter can verify their votes on the screen and select a “Print” option for a printed copy if they want a printed paper record to take with them. Finally a “Done” or “Exit” option locks their voting record back into the database and clears the terminal screen. A timeout feature automatically clears the screen and locks the record if the voter forgets to do so. This allows the voter to check and verify their vote and also allows the SOE to generate a paper vote trail for manual recounts or audit purposes.
[0074] In an embodiment, a paper trail audit and or full paper based recount is possible. The SOE office prints out the complete record of all votes cast in an election by precinct, city, district or county. Each and every individual vote, as cast, gets printed from the demographic database voting record for a particular election or candidate. It is not necessary for each voter to unlock their record to do this. Because each vote is not VSI connected to a unique voters' name the confidentiality of the secret ballot is maintained. The votes can then be hand counted or counted by machine or with optical scanners or as dictated by law, whichever method the SOE decides to use.
[0075] With an embodiment of a voting system there is no longer a need to cancel any electronic ballots. If the voter makes a mistake and casts a ballot in error all they need to do is initiate another voting session and correct or change their ballot.
[0076] With an embodiment of a voting system write in votes are possible using an on screen touch screen keyboard.
[0077] An embodiment of a voting system also captures voters' intent even if they want to cast a partial or fully blank ballot. This may help prevent under votes and guessing at the voters' intent.
[0078] With an embodiment of a voting system election recounts, either court ordered, automatic or those mandated by law, can be conducted in the exact same way as the original count was taken.
[0079] With an embodiment of a voting system you can audit terminal usage by each unique machine MAC address.
[0080] An embodiment of the database system allows you to automatically track heavily used terminals. This allows the SOE to rotate terminals to more evenly distribute their use. Problem terminals can be locked out at the mainframe.
[0081] The two front legs 14 when collapsed and folded up inside the bottom of the case become two integrated carrying handles.
[0082] The compact storage cases have an interlocking feature when stacked one on top of another to eliminate sliding and tipping when stacked for shipping or storage.
[0083] The new database design will allow the county SOE office to correct and clear up erroneous voter information presently stored in their voter registration data base. This will lead to more accurate and timely voter records.
[0084] An embodiment of a voting system can restore voter trust in the voting system. Voters will be able to see for themselves that their votes have been accurately recorded and counted and that only they, and no one else, can verify the accuracy and content of their own voting record.
[0085] Last minute voter initiated changes to their VSI information are possible.
[0086] Each voter can initiate corrections and or changes to their VSI record before or during an election. With the aid of SOE personnel a voter can unlock access to their VSI information to allow SOE personnel to make changes and or corrections such as a change of address.
[0087] Because of the database design and each voter's biometric key, picture ID's, presented at the polling places in order to vote, are no longer necessary.
[0088] With an embodiment you no longer have to mail out a voter registration card to each voter.
[0089] FIG. 1 shows the invention closed up inside the carrying case and stacked atop a second case. Note the recessed lip around the perimeter of the top which fits into a matching recessed area on the bottom of another case.
[0090] FIG. 2 shows the invention with its telescoping legs deployed. The two rear legs are angled out to the side for greater stability while the front legs, which form the two side carrying handles when folded up, are straight up and down. The AC power cord comes out the back and the lid is shown partially opened from the front and hinged at the back.
[0091] FIG. 3 is looking down inside the case with the lid fully removed for clarity sake. This figure shows the internal devices located inside the case. The case itself 12 , The touch screen voting terminal 16 , AC outlet and power switch 18 , Biometric finger scanner 22 , AC 24 and DC 26 power good indicator lights and the AC power cord 20 . The relative positions are for illustrative purposes only and do not necessarily reflect the final engineering production positions of these devices.
[0092] FIG. 4 shows the voting terminal as it would look from the right side deployed for voting. The telescoping legs 14 support the carrying case 12 . The touch screen voting terminal 16 can be set at two different viewing angles as illustrated here with the two privacy screens opened one to the left and one to the right. A third glare screen opens upward towards the top. The inside of the lid has positional stops that lock into the back of the touch screen terminal to securely hold it in place. The relative positions are for illustrative purposes only and do not necessarily reflect the final engineering production positions of these devices.
[0093] FIG. 5 is a block pictorial representation of the voting terminal, connected to the mainframe computer. It shows that the internal microprocessor controlled system board 28 connected to the touch screen display 16 , the biometric finger scanner 18 , and bootable operating system OS device 30 are connected to two of the available USB ports 29 . The communications port 32 through which all data communications are sent back and forth to the mainframe computer 34 located at the SOE office. The names and relative positions are for illustrative purposes only and do not necessarily reflect the final engineering production names and positions of these devices.
[0094] FIG. 6 is a simple block diagram of the basic overall voting process and does not necessarily reflect all possible combinations of steps that could be covered in the complete voting process. They are for illustrative purposes only and do not necessarily reflect the final voting process.
[0095] It should be understood, of course, that the foregoing relates to exemplary embodiments of the invention and that modifications may be made without departing from the spirit and scope of the invention as set forth in the following claims.
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An electronic voting terminal includes: a display; a data input device; a biometric input device; a case having an open and a closed position, the case protecting the display, the input device, and the biometric input device in the closed position, the case making the display, input device and biometric input device accessible by the voter in the open position; a communications medium; a microprocessor to control the display, the data input device, the biometric input device, and the communications medium; and a power supply that accepts alternating current and provides direct current to the microprocessor The device utilizes the biometric input device to validate the identity of the voter, utilizes the data input device to receive the ballot from the voter, and utilizes the communications medium to transmit the ballot. A system for voting also includes a centralized computer and voter registration database.
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BACKGROUND OF THE INVENTION
The invention relates to power supplies and battery chargers for portable defibrillators.
Portable defibrillators, such as the PD 1400 Series Products available from Zoll Medical Corporation of Burlington, Mass., deliver high energy shocks to a patient's chest for defibrillation. Typically, portable defibrillators employ batteries (e.g., lead acid batteries) to store power for generating such shocks. Eventually, the power stored in the batteries is used, and the batteries must be recharged from a source of AC power.
AC power supplies, which convert AC power to DC power, have been used for operating a portable defibrillator and for recharging the batteries in the portable defibrillator. Approaches to using AC power supplies include: building an AC power supply into the portable defibrillator; supplying an AC power supply in a separate box that includes a cord for attachment to the portable defibrillator; attaching the portable defibrillator into a "docking station" that contains an AC power supply (so that the combination of the docking station and the portable defibrillator is not itself portable); and removing the batteries from the portable defibrillator for charging in a separate AC powered unit (in which case the AC powered unit does not power the defibrillator). The conventional AC power supply is a "controlled voltage" supply that maintains a controlled, generally constant, DC output voltage for varying electrical load.
Controlled current supplies, which maintain a controlled, generally constant, DC output current for varying electrical load, have been used in other types of devices in which batteries need to be charged. Controlled current supplies offer advantages over controlled voltage supplies in that controlled current supplies can more rapidly charge batteries and can provide a more reliable indication that a battery is fully charged. Controlled current supplies are particularly well suited to charging lead acid and other types of batteries that tend to lose the ability to retain a charge when put into use before being fully charged. When such batteries are charged with a controlled voltage supply, the user sometimes will think that the battery is fully charged, both because charging takes so long (e.g., sixteen hours) and because the charger cannot reliably inform the user whether charging is complete, with the result that partially charged batteries are inadvertently put into use. Over time, use of partially charged batteries results in the batteries losing their ability to retain a charge. Though providing superior charging characteristics with regard to the time required to charge a battery, previous controlled current chargers have required complex support circuitry to implement them as AC power supplies for defibrillators. The difficulty with implementing controlled current chargers is that they must maintain a measure of the current supplied to the battery, and therefore, without support circuitry, require a known charging current into the battery to perform properly. When a defibrillator is operating, however, current levels may vary from as low as 500 milliamps up to eight amps. Thus, for the controlled current charger to be effective, support circuitry was needed to sense and integrate the current supplied to the defibrillator (as opposed to the current supplied to the battery) by the charger so that the charger could maintain a measure of the current supplied to the battery.
SUMMARY OF THE INVENTION
The invention provides a detachable power supply that can be quickly and securely attached to a portable defibrillator so that the power supply and the defibrillator form an integral unit. This ease of attachment is vital in the emergency situations in which portable defibrillators are typically employed. In addition, because the power supply can be securely attached to the defibrillator, and because the power supply is both compact and lightweight, use of the power supply does not significantly reduce from the portability of the defibrillator.
Though compact and lightweight, the detachable power supply offers the advantages of both controlled current and controlled voltage power supplies. When the defibrillator is turned on, the power supply operates in a controlled voltage mode, and thereby ensures that the defibrillator is powered by a predictable, generally constant, controlled input voltage. However, when the defibrillator is turned off, and the battery needs to be charged, the power supply operates in a controlled current mode. Use of the controlled current mode allows for quick charging of the battery, and thereby maximizes the likelihood that the battery will be in a fully charged state when a source of AC power is unavailable.
In one aspect, generally, the invention features a detachable power supply for supplying power from an external power source to a portable defibrillator for charging a battery of the portable defibrillator and operating the portable defibrillator. The power supply includes a housing shaped to attach to the defibrillator, and a latch connected to the housing for mechanically attaching the power supply to the defibrillator so that the power supply and the defibrillator form a portable, integral unit. Typically, the height and width of the housing are dimensioned so that the housing conforms to the dimensions of the portable defibrillator. Such dimensioning eases handling and storage of the defibrillator when the power supply is attached, and thereby prevents the power supply from negatively impacting the portability of the defibrillator.
The power supply also includes an electrical connector connected to the housing to supply power to the defibrillator. The connector is located so that it engages a mating electrical connector on the defibrillator as the latch is engaged to connect the power supply to the defibrillator. Use of such a connector, as opposed to, for example, a cord, dramatically simplifies connection of the power supply to the defibrillator, and ensures that, when the power supply is physically attached to both the defibrillator and the external power source, the power supply will be able to supply power to the defibrillator.
Finally, the power supply includes an external power connection, typically a cord, for bringing external power into the power supply and a power module installed within the housing and having a power circuit that converts power from the external power source to a form useable by the portable defibrillator. The output of the power module is connected to the electrical connector to deliver power to the defibrillator.
To allow quick connection of the power supply to the defibrillator, the latch can include a mechanism for attaching the power supply to the defibrillator without manipulating the latch. The power supply can also include an elongated hook member for insertion into a slot located in a housing of the defibrillator. In this case, the hook member, in combination with the latch, secures the power supply to the defibrillator. Typically, the hook member is located near the top of the power supply and the latch is located near the bottom of the power supply.
To allow quick detachment of the power supply from the defibrillator, the power supply can also include a latch release that, when pressed, enables detachment of the power supply from the defibrillator. This latch release can be lockable to prevent detachment of the power supply from the portable defibrillator.
For safety purposes, the power supply can include an interlock switch that connects the electrical connector to the power module when the power supply is attached to the portable defibrillator, and isolates the electrical connector from the power module when the power supply is detached from the portable defibrillator. This ensures that the electrical connector will never be powered when the power supply is not connected to the defibrillator, and thereby eliminates any risk that a person handling the power supply would be shocked by the power supply.
To enhance portability, the housing of the power supply can include a recess for storage of the cord. Typically, the recess is a depression extending around the full circumference of a portion of the housing. The depression is sized so that the cord may be wrapped around the housing and be substantially fully contained within the depression. The housing can also include a separate recess for storage of a plug of the cord.
To provide optimal charging and operational performance, the power module of the power supply can be alternately operable in both a controlled current mode and a controlled voltage mode. Typically, the power module operates in the controlled voltage mode when the defibrillator is turned on. The power module typically operates in the controlled current mode only when the defibrillator is turned off and a current supplied to the defibrillator when the power supply operates in the controlled voltage mode is less than or equal to a predetermined value.
In another aspect, generally, the invention features a controlled current/controlled voltage power supply for supplying power from an external power source to a portable defibrillator for charging a battery of the defibrillator and operating the defibrillator. The power supply includes an external power connection for bringing external power into the power supply, a power module, and a controller. The power module has a power circuit that converts power from the external power source to a form useable by the portable defibrillator, is alternately operable in either a controlled current mode or a controlled voltage mode, and has an output connected to deliver power to the defibrillator. The controller switches the power module between the controlled current mode and the controlled voltage mode.
This dual-mode power supply provides rapid battery charging which, as noted above, is of particular significance when the defibrillator employs lead acid or other types of batteries that tend to lose their ability to retain charge when put into service before being fully charged. Because this power supply rapidly charges the battery, it reduces the likelihood that the battery will be put into service before being fully charged. In addition, because this power supply operates in a controlled voltage made suitable for directly powering the defibrillator, it further reduces the likelihood that a partially charged battery will need to supply power to the defibrillator.
Other features and advantages of the invention will be apparent from the following description of the preferred embodiments and from the claims.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a perspective view of a detachable power supply and a portable defibrillator.
FIG. 2 is a perspective view of the power supply of FIG. 1.
FIG. 3 is a cutaway side view of the power supply of FIG. 2 taken along line 3--3 of FIG. 2.
FIG. 4 is a block diagram of the power supply of FIG. 2.
FIG. 5 is a circuit diagram of an output circuit of a power module of the power supply of FIG. 2.
FIG. 6 is a state diagram for a charging procedure implemented by the power supply of FIG. 2.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
FIGS. 1 and 2 show a portable defibrillator 16 and detachable power supply 10. The detachable power supply 10 includes a continuous and elongated hook member 12 located near the top of the power supply and a latch 14 (see FIG. 2) located near the bottom of the power supply for attachment to the portable defibrillator 16. Power supply 10 is attached by placing hook member 12 in a slot 18 in the upper housing of the defibrillator and engaging the latch. The power supply is detached by pressing a latch release 20 to disengage the latch.
Specifically, the top of the power supply is held in place against the defibrillator by the engagement of hook member 12 with slot 18. The power supply is swung into place so that a portion 22 of latch 14 secures the bottom of the power supply to a portion 23 of the lower housing of the defibrillator. The power supply is released by pressing on latch release 20, which protrudes through the top edge of the power supply. Thus, the power supply can be attached to and released from the defibrillator with a single hand, and without manipulating the latch.
Latch 14 is a piece of stamped sheet metal which, when attached, links the housing of the power supply to the housing of the defibrillator. The latch, which can be disengaged only when unstressed, is designed so that increased pull on the housings to separate them makes the latch harder to disengage.
Referring also to FIG. 3, latch 14 is locked by putting a screw 24 (FIG. 2) through a hole 26 in latch release 20 and into a threaded insert 28 in a metal cover plate 30 of the power supply. When screw 24 is in place, the position of the latch release is fixed, and the latch pivots around its engagement with the latch release at point A. In this configuration, the power supply can still be attached to the defibrillator, but cannot be detached without using a tool. The latch is disengaged, and the power supply is detached, by taking a tool (e.g., a screwdriver) and pushing on the back edge of the latch (near point B) so that the latch disengages at point C. (The power supply cannot be detached by removing screw 24 because, when the power supply is attached to the defibrillator, screw 24 is located between the power supply and the defibrillator.)
When screw 24 is not in place, latch release 20 is free to move up and down, and the latch pivots around its engagement at point B with the housing of power supply 10. The latch release is biased upward by pressure exerted on the latch by a spring 32 located within the power supply. When the latch release is pressed downward, pivoting of the latch about point B causes the latch to disengage at point C. Once the latch is disengaged, the power supply is removed by swinging the bottom of the power supply away from the defibrillator, and removing the hook member from the slot.
Power supply 10 makes electrical connection with portable defibrillator 16 through pins 34a-34e (see FIG. 4), referred to collectively as pins 34, located within a port 36. Pins 34 fit within a socket 38 on the defibrillator. For safety reasons, power pin 34a is only active when the power supply is attached to the defibrillator. When the power supply is attached to the defibrillator, an extension (not shown) on the defibrillator closes two series interlock switches 39 (see FIG. 4) located within a recess 40 on the power supply, and thereby activates power pin 34a. Interlock switches 39 isolate power pin 34a from a power module 58 (see FIG. 4) of the power supply when the power supply is detached from the defibrillator.
Power supply 10 also includes a ruggedized base 42 and an eight-foot, integral cord 44. For storage of integral cord 44, base 42 includes an indentation 46 around its periphery and a recess 48 at its back end. Indentation 46 and recess 48 are configured so that integral cord 44 can be wrapped around indentation 46 and a plug 50 of integral cord 44 can be secured in recess 48. Recess 48 is configured so that plug 50 is flush with the surface of base 42 when stored within recess 48, which allows the defibrillator to stand on end even when the power supply is attached and plug 50 is secured in recess 48.
Another external feature of the power supply is a set of five indicator LEDs (light emitting diodes) 52a-52e, referred to collectively as indicator LEDs 52, located along the top of the power supply. Yellow indicator LED 52a is lit when the power supply is connected to a source of AC power and capable of operating the defibrillator and/or charging a battery 54 of the defibrillator. Yellow indicator LED 52b is lit when battery 54 is installed in the defibrillator and is receiving a charge. Green indicator LED 52c is lit when battery 54 is fully charged and therefore ready for use. Yellow indicator LED 52d is lit when a fault is detected in the power supply or battery 54. Finally, flashing yellow indicator LED 52e is activated when the power supply needs to be connected to a source of AC power, which occurs when the power supply is attached to the defibrillator and not connected to a source of AC power, battery 54 is in place, and the defibrillator is turned off. An audible signal is also produced by a beeper 56 (see FIG. 4). Beeper 56 is programmable so that the audible signal is sounded only upon expiration of a predetermined delay period (e.g., after the power supply has needed to be, and has not been, connected to a source of AC power for thirty minutes).
The power supply is 10.5 inches (26.7 cm) wide, 4 inches (10.2 cm) high, and 2.5 inches (6.4 cm) deep, and weighs 3.1 pounds (1.4 kg). While the housing of the power supply is made typically from a molded polymer, other materials such as, for example, coated magnesium could also be used. The power supply is configurable to operate with AC input voltages of 90-135 (110) or 190-265 (220) volts at frequencies of 50 or 60 Hz, and also works with a 165 volt square wave converter, such as is commonly available in ambulances. The power supply powers the defibrillator regardless of whether a battery is present in the defibrillator.
Referring to FIG. 4, power supply 10 includes a power module 58 and a control module 60. Power module 58 includes an input line filter 62 that is connected to integral cord 44 and shapes the input voltage therefrom, a voltage selector 64 that allows configurable selection between input voltages of 110 volts and 220 volts, and an output circuit 66 that, in response to control inputs, produces either a controlled voltage or a controlled current. Power module 58 also includes a heat sink 68 connected to heat producing components 70, 72 of, respectively voltage selector 64 and output circuit 66. A thermal shutdown device 74 that shuts down power module 58 in response to excessive heat is also connected to heat sink 68.
Output circuit 66 operates in either a controlled voltage charging mode, in which it delivers a generally constant output voltage of about 11.75 volts at up to 3.5 amps; a low voltage charging mode, in which it delivers a generally constant output voltage of about 10.75 volts at up to 10.0 amps; a controlled current charging mode, in which it delivers a generally constant output current of up to 0.835 amps at a voltage of up to 16.5 volts, and a battery search mode, in which it delivers a generally constant output voltage of 15 volts at up to 0.3 amps. Though the controlled voltages or currents are generally constant, some variation is allowed. For example, in the preferred embodiment, the 11.75 volt output voltage in the controlled voltage charging mode can vary between 11.5 and 12 volts, while the 10.75 volt output voltage in the low voltage charging mode can vary between 10.3 and 10.9 volts. Similarly, the output current in the controlled current charging mode can vary between 0.735 and 0.935 amps.
Referring to FIG. 5, output circuit 66 rectifies the alternating voltage and current from the transformer secondary (T1) through the two legs of a center tap 100 V Schottky diode (CR12). During the dead time between power cycles, both diode legs are forward biased and the magnetizing current in the transformer appears as an offset between the two currents. Leakage spikes from the transformer are snubbed to a safe reverse voltage level by R21 and C15.
The rectified transformer voltage appears across an output filter that includes a 33 μH inductor (L2) and two 680 μF capacitors (C16 and C17). During power transfer, the rectified transformer voltage energizes the inductor and provides output current to the load. During dead time, the inductor provides the energy delivered to the load. The inductor current is continuously flowing for normal operating loads greater than 1.6 A.
The output voltage (PS -- PWR) of output circuit 66 is sensed by a set of resistors (R24 through R29) that includes a potentiometer (R26) for factory adjustment. A tap off these resistors, which has a nominal value of 2.5 volts, connects to a reference pin (R) of a band gap device (U2). This connection functions as the negative input of an error amplifier of a feedback control loop. This loop is stabilized by compensation provided by C19, C20, and R31.
The output voltage of output circuit 66 is regulated to hold the reference pin of the band gap device (U2) sufficiently above 2.5 V to cause the cathode (K) of the band gap device to sink a required current through the diode of the optocoupler IS01. The current required through the optocoupler diode is determined by the current required through the transistor of IS01 (which is located in voltage selector 64). The current through the transistor of IS01 sets the duty cycle of the output of voltage selector 64 to a value that allows output circuit 66 to produce a desired output voltage. Bias current for the optocoupler diode is provided from the output of output circuit 66 through R30 and CR15, and from the auxiliary output (AUX -- PWR) of output circuit 66 through R35 and CR16. Bias current is redundantly supplied by the auxiliary output for fault condition operation. In normal operation, the auxiliary output is set between 6.5 volts and 7.5 volts, and diode CR16 is back-biased so that noise from the auxiliary output is not coupled into the control circuit.
The control circuitry connected to the output of output circuit 66 draws approximately 12 mA. Because the product application requires the output to be connected directly across a battery, the battery would be drained by this control circuitry if line power were not provided to output circuit 66. To avoid draining the battery, the control circuitry is switched on and off through an NPN transistor (Q7). Current to turn on this transistor is provided from a tap winding off of the transformer and a resistor network (R22 and R23).
Output circuit 66 is set so that its output voltage (PS -- PWR) does not exceed 17.6 volts. If the voltage exceeds this level, an over voltage protection circuit is activated. This circuit includes a 17 volt zener diode (CR18) that, when the output voltage exceeds 17.6 volts, conducts enough to drive the gate of an SCR (CR17) above threshold. When the gate of the SCR is driven above threshold, current is driven through the diode of optocoupler IS02 through R32 from the auxiliary output. Current flowing through the diode of optocoupler IS02 inhibits the production of power by voltage selector 64 until the output voltage drops to the point where the IS02 diode no longer conducts. At that point, voltage selector 64 is again able to produce power.
The auxiliary output (AUX -- PWR) is set by an LM317T adjustable three terminal regulator (U3). In normal operation, input power to this device is provided by a tap off of the transformer. However, the auxiliary must be kept turned on during transitions for which the power supply is back driven by a battery. In those cases, auxiliary power is provided from the battery through Q8 and CR19. Q8 has a particular functional window within which it is operational. When the power supply is not providing any power, Q7 is off, which turns Q8 off and ensures that the battery is not drained. When the power supply is providing normal operating power, CR19 is back biased by the tap winding.
Output circuit 66 interfaces with control module 60 through an eight conductor cable harness terminated on each end with an eight position crimp terminal housing which mates with a PCB mounted connector. The pin assignment at the interface is as follows:
______________________________________Pin Number Function Title______________________________________1 Output (+) PS.sub.-- PWR2 Output (+) PS.sub.-- PWR3 Output (-) PS.sub.-- GND4 Output (-) PS.sub.-- GND5 Auxiliary (+) AUX.sub.-- PWR6 Current Control I.sub.-- CTRL7 Voltage Control V.sub.-- CTRL8 No Connection N/A______________________________________
Two conductors each are provided for both the output power and output ground to minimize voltage drops under heavy load. The output is regulated on the power supply and therefore does not compensate for drops through the connector.
The output voltage is nominally set to 10.75 volts. When required by the system, the voltage setting is changed by connecting the voltage control line (V -- CTRL) to a fixed voltage (5 volts or 0 volts) through one of a set of fixed resistances in control module 60. This control signal changes the voltage/impedance characteristics of the reference pin of U2. Through the possible control signals, control module 60 can set the voltage within a range of 10.75 volts to 16.25 volts. The control line is protected from electro static discharge with a series, one kiloohm resistor (R33).
The output current is sensed by control module 60. This current sense signal is used to provide over current protection and current control as required by the system. The control signal to the power supply is in the form of a sink current through the diode of optocoupler IS01. When active, this control signal overrides the voltage control because the cathode (K) of U2 enters an open circuit mode when the output voltage causes the U2 reference voltage to fall below 2.5 V.
To provide over current protection while the output collapses, the diode of IS01 receives current from the auxiliary output in addition to the main output. Control module 60 thus can drive the main output down to zero volts in severe over current conditions.
Referring again to FIG. 4, control module 60 includes a microprocessor 76 that has overall control of the power supply. Microprocessor 76 is an 87C752 processor running at 6.144 MHz with two kilobytes of internal ROM and 64 bytes of internal RAM. Microprocessor 76 includes a six bit I/O port and two eight bit I/O ports.
A control circuit 78 responds to signals from microprocessor 76 and a BOOST signal from the defibrillator to supply control signals to output circuit 66. The defibrillator turns on the BOOST signal when the defibrillator is producing a pace pulse or otherwise needs to receive defibrillation charge energy. In control module 60, the BOOST signal, which is received on pin 34c, is input into a comparator that produces a digital (high/low) output. This digital output is supplied to microprocessor 76 for control of the power supply and, in particular, output circuit 66. In addition, to ensure that the power supply immediately responds to the BOOST signal, the digital output is supplied directly to control circuit 78.
Measurement circuits 80 monitor the output voltage of output circuit 66, the current supplied to battery 54, and other signals, to provide information that allows microprocessor 76 to determine the charge status of battery 54.
Other components of control module 60 include beeper/LED drive circuitry 82 that activates LED 52e and beeper 56 under the conditions described above, and a power supply circuit 84 that supplies operating power to microprocessor 76, control circuits 78, measurement circuits 80, and beeper/LED drive circuitry 82. Power supply circuit 84 is powered by the auxiliary output (AUX -- PWR) of output circuit 66.
Generally, microprocessor 76 configures the power supply to deliver a controlled voltage when the defibrillator is turned on, and either a controlled voltage or a controlled current when the defibrillator is turned off. Use of a controlled current reduces the time required to charge a battery of the defibrillator from about sixteen hours to about three hours.
More specifically, as illustrated in FIG. 6, microprocessor 76 controls delivery of power according to a procedure 100 that microprocessor 76 invokes approximately once every 10 milliseconds. In implementing procedure 100, processor 76 monitors several characteristics of the power supply and the defibrillator, including the voltage level of battery 54, the current supplied to the defibrillator, the on/off state of the defibrillator, and the presence or absence of battery 54 and/or the BOOST signal from the defibrillator. Microprocessor 76 determines the on/off state of the defibrillator from a signal received on pin 34d.
At initialization, the power supply operates in an IDLE state 102. In IDLE state 102, output circuit 66 operates in low voltage mode if the power supply is connected to the defibrillator and the BOOST signal from the defibrillator is on, and otherwise operates in controlled voltage mode.
The power supply transitions from IDLE state 102 to a CONSTANT VOLTAGE state 104 when the power supply is connected to the defibrillator, the defibrillator is turned off, battery 54 is present, and the BOOST signal is off. In making the transition, microprocessor 76 resets an integrated total charge value.
In IDLE state 102, if portable defibrillator is turned off, microprocessor 76 determines whether battery 54 is present by implementing a battery search procedure. First, microprocessor 76 places output circuit 66 in battery search mode. After waiting for 50 milliseconds to allow the output voltage to reflect the change in the charging mode, microprocessor 76 measures the current being delivered to the defibrillator. If this current exceeds 100 milliamps, the microprocessor 76 determines that battery 54 is present. Otherwise, microprocessor 76 determines that battery 54 is not present. Thereafter, microprocessor 76 places output circuit 76 in controlled voltage mode and waits for 50 milliseconds to allow the output voltage to reflect the change in the charging mode. Typically, microprocessor 76 activates the battery search mode once every 500 milliseconds.
In CONSTANT VOLTAGE state 104, output circuit 66 operates in the controlled voltage mode. During charging, microprocessor 76 periodically adds a measure of the current being supplied to the defibrillator to the integrated total charge value, and thereby maintains a measure of the total charge being supplied to battery 54.
The power supply transitions from CONSTANT VOLTAGE state 104 to a CONSTANT CURRENT state 106 when the average current supplied to the defibrillator is less than or equal to a predetermined controlled current charging rate. The power supply returns to IDLE state 102 from CONSTANT VOLTAGE state 104 when the power supply is disconnected from the defibrillator or the defibrillator is turned on. (If battery 54 is not present, this will cause the current to fall below the controlled current charging rate.)
In CONSTANT CURRENT state 106, output circuit 66 operates in the controlled current mode and supplies current at the controlled current charging rate. Microprocessor 76 continues to periodically add the current being supplied to the defibrillator to the integrated total charge value. The power supply transitions from CONSTANT CURRENT state 106 to a TOP OFF state 108 when the average battery voltage remains level for three minutes, or begins to drop. The power supply transitions from CONSTANT CURRENT state 106 to IDLE state 102 when the power supply is disconnected from the defibrillator, the defibrillator is turned on, or battery 54 is not present. In CONSTANT CURRENT state 106, microprocessor 76 determines that battery 54 is not present if the measured battery voltage exceeds 15.5 volts.
In TOP OFF state 108, output circuit 66 continues to operate in the controlled current mode and supplies current at the controlled current charging rate. The power supply transitions from TOP OFF state 108 to a READY state 110 when a time period equal to the integrated total charge value divided by sixteen elapses. The power supply transitions from TOP OFF state 108 to IDLE state 102 when the power supply is disconnected from the defibrillator or the defibrillator is turned on.
In READY state 110, output circuit 66 operates in the controlled voltage mode, and microprocessor 76 activates LED 52c to indicate that battery 54 is fully charged. After LED 52c is activated, the power supply transitions to a FLOAT state 112.
In FLOAT state 112, output circuit 66 operates in the controlled voltage mode. The power supply transitions from FLOAT state 112 to IDLE state 102 when the power supply is disconnected from the defibrillator, the defibrillator is turned on, or battery 54 is not present. As in IDLE state 102, microprocessor 76 determines whether battery 54 is present by switching output circuit 76 to the battery search mode.
Finally, if at any time during charging microprocessor 76 detects a fault in the power supply, microprocessor 76 causes the power supply to transition to a FAULT state 114. In FAULT state 114, output circuit operates in low voltage mode if the BOOST signal is on, and otherwise operates in controlled voltage mode. To indicate the presence of a fault, microprocessor 76 turns on LED 52d and, if LED 52c is on, turns off LED 52c (microprocessor 76 also turns off LED 52c in IDLE state 102). The power supply remains in FAULT state 114 until the fault is corrected, at which point the power supply transitions to IDLE state 102.
Other embodiments are within the following claims.
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A detachable power supply for supplying power from an external power source to a portable defibrillator for charging a battery of the portable defibrillator and operating the portable defibrillator includes a housing shaped to attach to the portable defibrillator and a latch connected to the housing for mechanically attaching the power supply to the defibrillator so that the power supply and the defibrillator form a portable, integral unit. The power supply also includes an electrical connector connected to the housing to supply power from the power supply to the defibrillator, the connector is located so that it engages a mating electrical connector on the defibrillator as the latch is engaged to connect the power supply to the defibrillator, an external power connection for bringing external power into the power supply, and a power module installed within the housing, the power module having a power circuit that converts power from the external power source to a form useable by the defibrillator, the output of the power module being connected to the electrical connector to deliver power to the defibrillator. Typically, the power module is alternately operable in both a controlled current mode and a controlled voltage mode.
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This application is a continuation of application Ser. No. 691,909, filed Jan. 16, 1985, now U.S. Pat. No. 4,885,681, issued Dec. 5, 1989.
BACKGROUND OF THE INVENTION
The present invention relates to a high speed virtual machine system (VMS), and more particularly to method and system for reducing an I/O simulation overhead of the VMS.
The specifications of the Japanese Patent Application Kokai No. 55-76950 laid open on Jun. 24, 1975, No. 56-19153 laid open on Feb. 23, 1981 and No. 55-42326 laid open on Mar. 25, 1980 and the U.S. Pat. No. 4,459,661 (Saburo Kaneda et al., Apr. 21, 1982), which was filed with the Convention priority based on the latter Japanese Patent Application Kokai, disclose virtual machine systems.
FIG. 1 shows the configuration of a real computer system 9000. Numeral 1000 denotes a central processing unit (CPU), numeral 2000 denotes a main memory, numeral 3000 denotes an I/O processor (IOP), and numeral 4000 denotes an I/O controller (IOC). Numeral 100 denotes a signal line between the CPU 1000 and the main memory 2000, numeral 200 denotes a signal line between the CPU 1000 and the IOP 3000, numeral 300 denotes a signal line between the IOP 3000 and the main memory 2000, and numeral 400 denotes a signal line between the IOP 3000 and the IOC 4000. The real computer system 9000 is operated under a control of a resource management (CPU, main memory and I/O devices) of an overall system of an operating system (OS) on the main memory 2000.
The configuration of a virtual machine system (VMS) is shown in FIG. 2. A real computer system 10000 has a similar hardware configuration (CPU, main memory and I/O devices) as that shown in FIG. 1 but it has a VMS control program (VMCP or simply CP) on the main memory 2000. A plurality of logical machines (called virtual machines (VM)) are logically configured by a hardware simulation function of the VMCP. The VM's 10000-1 (VM1), 10000-2 (VM2) and 10000-3 (VM3) each is logically configured to have the same hardware configuration as the real computer system (called a host system) 10000. The OS-N (N=1, 2, 3) which controls the VM exists on each main memory 2000-N (N=1, 2, 3) of each VM, and those OS's run concurrently under one host system. The hardware configuration (CPU, main memory, IOP and IOC) in each VM of FIG. 2 is logically configured by the VMCP and most portions of the substance thereof exist on the corresponding hardware configuration in each virtual machine configured by the host system. For example, as its main memory, the VM may exclusively occupy a portion of the main memory 2000 of the host system or may share the main memory 2000, and as its I/O devices, the VM may share the I/O devices of the host system or may exclusively occupy the I/O device. Alternatively, there may be no corresponding I/O device on the host system and the I/O device may be virtually configured by simulation by the VMCP. In any case, the OS on the main memory 2000-N (N=1, 2, 3) on each VM can see the same hardware configuration (CPU, main memory, IOP and IOC) as that of the host system. It should be noted that the architecture (hardware configuration and function as viewed from the OS) of each VM may be somewhat different from the architecture of the host system. Similarly, the architectures of the respective VM's may be different from each other. For example, a machine instruction set of the host system may not be exactly identical to a machine instruction set of each VM. However, a completely different machine instruction set is excluded from the VMS in the present invention because it increases the load of the VMCP and increases the scale of the host system emulation mechanism. The virtual machine VM in the present invention requires that most of the machine instructions can be directly executed with the same performance as that (execution speed) of the host system on the host system without intervention of the VMCP. While only three VM's are shown in FIG. 2, any number of VM's may be included and the upper limit thereof is determined by compromise between the resource capacitance of the host system and the performance of the VM. The host system has a privileged state and a nonprivileged state. A machine instruction which imparts a significant influence to the system (e.g. I/O instruction or system interrupt mask change instruction) is called a privileged instruction and it can be used only in the privileged state. This is well known in the art.
FIG. 3 shows the memory hierarchy of the virtual machine VM1 of FIG. 2. Numeral 2060 denotes a virtual space generated by the OS1 on the VM1. The OS1 exists on the main memory 2000-1 of the VM1. The main memory 2000-1 of the VM1 is copied on the main memory 2002 of the host system. (The main memory 2000 of the host system is divided into a hardware system area 2001 and a programmable area 2002 as shown in FIG. 7.). The copy is given by an address translation table 2010. FIG. 4a shows an address translation table 2010(1). The address translation table contains entries corresponding to addresses v2 on the main memory 2000-1 of the VM1 and corresponding addresses r on the main memory 2002. A start address of the address translation table 2010(1) is stored in one control register (Real Address Translation Table Origin Register (RATOR)) 1110 of basic control registers 1100 (see FIG. 7) in the CPU 1000 when the OS1 on the VM1 operates on the main memory 2000-1. In the present case, the address translation table 2010(1) exists on the main memory 2000-1 of the VM 10000-1, that is, on the main memory 2002 of the host system, and the start address is set in the register 1110 described by an address in the main memory 2002 of the host system.
Numeral 2060 in FIG. 3 denotes a virtual storage generated by the OS1 on the VM1 and a copy thereof to the main memory 2000-1 of the VM1 is given by an address translation table 2040 managed by the OS1. FIG. 4b shows a format of the address translation table. It contains entries corresponding to addresses v3 of the virtual storage 2060 and corresponding addresses v2 of the main memory 2000-1 of the VM1. A start address of the address translation table 2040 is stored in one control register (VATOR) 1120 of the basic control registers 1100 (see FIG. 7) of the CPU 1000 when the OS1 of the VM1 is running on the virtual storage 2060. In the present case, since the address translation table 2040 exists on the main memory 2000-1 of the OS1, the start address is described by an address system of the main memory 2000-1 of the OS1. The address translation table 2010(1) (called a translation table A) is managed and updated by the VMCP for the VM's, and the address translation table 2040 (called a translation table B) is managed and updated by the OS on each VM for its own virtual storage. The main memory 2002 of the host system is referred to as a level 1 memory, the main memory 2000-N (N=1, 2, 3, . . . ) of each VM is referred to as a level 2 memory, and the virtual storage 2060 generated by the OS on each VM (usually the OS generates a plurality of virtual storages) are collectively referred to as a level 3 memory. The virtual storage is usually divided into pages of a predetermined size (e.g. 4KB) and mapped into the main memory for each page, and a certain number of continuous pages (e.g. 256 pages, 1MB) are called one segment, as is well known in the art. Numeral 2020 in FIG. 3 denotes I/O operation command words (CCW) generated by the VMCP to start its own I/O operation. Since the VMCP operates on the level 1 memory, the CCW 2020 is generated at the level 1 memory address. It is called a level 1 CCW. The level 1 CCW need not be address-translated, and when an I/O start command is issued to the level 1 CCW, it is directly interpreted by the IOP 3000 and sent to the IOC 4000. The IOC 4000 executes each CCW for each I/O device. Numeral 2030 denotes a CCW prepared by the OS on the VM and is described by the level 2 memory address. The level 2 CCW is prepared by the OS on the VM. When an I/O start instruction is issued to the CCW from the OS on the VM, it may be translated to an equivalent level 1 CCW through the VMCP and the I/O start may be effected by the equivalent level 1 CCW through the VMCP. However, this leads to increase an overhead of the VMCP. Accordingly, in the alternative method, the VMCP intervenes to indicate an address of the address translation table from the level 2 memory to the level 1 memory (translation table A) to the IOP 3000, and the IOP 3000, looking up the translation table 2010, translates the data address in the level 2 CCW (or level 2 memory address) to the level 1 memory address. In this method, the intervention of the VMCP is reduced and the overhead is reduced. The OS on the VM in many cases executes on the level 3 memory and hence the CCW generated by the OS on the VM in many cases exists on the level 3 memory. Numeral 2050 in FIG. 3 denotes a CCW described by the level 3 memory address, that is, a level 3 CCW. When the start I/O instruction is issued to the level 3 CCW by the OS on the VM, it indicates an address of the address translation table from the level 3 memory to the level 2 memory (translation table B) and the address of the translation table from the level 2 memory to the level 1 memory (translation table A) to the IOP 3000 (FIG. 7), and the IOP 3000 looks up the translation table B to translate the data address of the level 3 CCW (level 3 memory address) to the level 2 memory address and looks up the translation table A to translate the translated level 2 memory address to the level 1 address in order to execute the CCW.
FIG. 4c shows an address translation buffer 3030 provided in a local storage in the IOP 3000 (FIG. 7) to reduce the address translation overhead in the IOP 3000. A field 1 of the address translation buffer 3030 contains VM numbers (VM #), a field 2 contains start addresses of the translation table A and the translation table B, a field 3 contains identification flags thereof, a field 4 contains CCW data addresses before translation and a field 5 contains level 1 memory addresses after translation. The IOP 3000 (FIG. 7) looks up the address translation buffer to translate the address, and if it is not found, looks up the translation table B and the translation table A to translate the address and register the translated address in the translation buffer 3030. The address translation buffer is a high speed local storage in the IOP 3000 and it is faster than the speed of looking up the translation tables B and A on the main memory 2002. It should be noted that the level 2 CCW, the level 3 CCW and the data buffers thereof should be fixed on the level 1 memory during the I/O execution. FIG. 5 illustrates a manner of dividing a continuous area of the main memory 2002 of the host system to use the divided sub-areas as the main memories for the respective VM's. When such VM's are used, a predetermined address displacement α is added to the address of the main memory of the VM to obtain the address of the main memory 2002 of the host system. In FIG. 5, the address displacement for the VM1 is α 1 and the address displacement for the VM2 is α 2 . In this case, the address translation 2010 from the level 2 memory address to the level 1 memory address may be a mere table to manage lower limit addresses and upper limit addresses of the respective VM's, as shown by 2010(2). In this case, it is easy to address-translate the level 2 CCW and an entry of the address translation buffer 3030 for the level 2 CCW (entry of "0" field 3 of the address translation buffer 3030) is not necessary. Alternatively, as shown in FIG. 5, the translation table 2010(2) is read into the local storage in the IOP 3000 (FIG. 7), the address displacement α is obtained by the VM # and it is added to translate the address (translation from the level 2 memory address to the level 1 memory address). A high speed VM mode is provided for the VM in which the entire main memory of the VM (FIG. 3) is resident in the main memory 2002 of the host system and fixed therein or it occupies a continuous area of the main memory of the host system as shown in FIG. 5. In the high speed VM mode, most privileged instructions issued by the OS on the VM are directly executed (execution without the VMCP in the almost same performance as that of the host system). However, the I/O instruction on the VM requires the intervention by the VMCP as will be described later.
Referring to FIG. 6, a manner in which the start IO instruction issued by the OS on the VM is executed by the VMCP is explained. The OS on the VM designates a sub-channel number (sub-channel #) which corresponds to the I/O device to issue the start I/O instruction. Since this sub-channel # is one under the VM, it is called a virtual sub-channel #. The VMCP translates it to a corresponding real sub-channel #. The correspondence is determined at the time of defining the VM. The VMCP checks the level of the CCW to which the start I/O instruction was issued by the OS on the VM. Usually, it is represented by an operand of the start I/O instruction. Let us assume that the start I/O instruction is issued to the level 3 CCW. In FIG. 6, the CCW 2810 is the CCW on the level 2 memory and the data address thereof is the level 3 memory address. The VMCP adds the operand 2800 to the CCW 2810 generated by the OS to issue the start I/O instruction. The operand 2800 contains a field L indicating the level of the CCW. When L=3, CCWs (2810) are the level 3 CCWs, and the operand 2800 contains the start address (VATOR) of the translation table B, a segment size (SS) and a page size (PS) of the level 3 memory which is the virtual space created by the OS on the VM. It also contains the start address RATOR of the translation table A, a segment size (SS), a page size (PS) of the level 2 memory when the level 2 memory is the virtual space created by the VMCP, and also contains an address to the CCW (2810). They are sent to the IOP 3000 (FIG. 7) through the line 200 upon the issuance of the start I/O instruction by the VMCP and basic information is set in the corresponding sub-channel register 3011. Similar basic information is stored in the corresponding sub-channel control block in the sub-channel control blocks 2090 shown in FIG. 7. (See sub-channel control block 2091 of FIG. 10). The IOP 3000 (FIG. 7) uses the address translation table in the sub-channel to execute the CCW 2810 generated by the OS while it translates the address.
FIG. 7 shows a hardware configuration in the prior art VMS and a block diagram concerning the I/O execution. A CPU 1000 includes a prefix register 1010 including an address of an area prefix (PSA) containing hardware interrupt information, CPU control registers 1100 and a program status word (PSW) 1020 containing a CPU basic status (such as an interrupt control bit or a machine instruction address to be executed next). It also includes an I/O instruction execute circuit 1030, an I/O interrupt circuit 1040, an I/O instruction execution microprogram 1050 and an I/O interrupt processing microprogram 1060. The V-bit representing a VM mode is present in 1090 as a VMS flag. During the running of VM, this bit is set to "1" by the VMCP. The high speed VM mode flag H exists in 1090. The VMS control flag 1090 may be in another form. For example, a VMCP mode (hypervisor mode) and a VM mode may be provided and the VM mode may include the preferred or high performance VM mode and the non-preferred VM mode. They are more or less similar, as described above, the IOP 3000 executes the level 3 CCW or the level 2 CCW (see FIG. 3) while using the information of the address translation buffer 3030 (see FIG. 4C) under the control of the microprogram 3020 in accordance with the address translation information (FIG. 6) contained in the sub-channel control blocks 2090 and the sub-channel registers 3010. The main memory 2000 in FIG. 7 is divided into a hardware system area (HSA) 2001 and a programmable area 2002. The HSA 2001 contains hardware information to be used by the CPU 1000 and the IOP 3000 and it can be accessed and updated by the microprograms 1050, 1060 and 3020 of the CPU and the IOP but cannot be accessed by a machine instruction opened to a normal user of the CPU 1000. The programmable area 2002 can be accessed by a machine instruction and it is a main memory area as viewed from the OS or the VMCP. I/O instruction, such as start I/O instruction, and step I/O instructions request the operations of the I/O devices, and these I/O requests issued from those I/O instructions are queued in an I/O request queue 2070 in a form of request queue. It comprises control blocks 2071 containing I/O request real sub-channel numbers interconnected by address pointers. After queuing to the I/O request queue, a start signal is sent to the IOP 3000 through the line 200. The IOP 3000 accesses the I/O request queue 2070 in the HSA 2001 and sequentially reads out request queue elements 2071 to process the I/O request. The I/O interrupt request is queued in the I/O interrupt request queue 2080 in the priority order of real interruption. A structure therefor is shown in FIG. 9. Eight interruption priority orders 0, 1, 2, 3, 4, 5, 6 and 7 are available and they are assigned by the operands together with the sub-channel numbers when the I/O instructions are issued. FIG. 10 shows a sub-channel control block 2091 in the sub-channel control blocks 2090 (FIG. 7). The sub-channel control blocks are arranged in the order of the real sub-channel numbers and their locations are uniquely determined by the real sub-channel numbers. The start address of the sub-channel control block 2090 is set in one control register in the control registers 1100 of the CPU 1000 (FIG. 7). The interruption priority order can be assigned to each sub-channel. Let us assume that the OS on the VM issues the I/O instruction while designating the sub-channel number and one of the interruption priority orders 0-7. Since the VM mode bit 1090 in FIG. 7 is "1", the I/O instruction executing μp(microprocessor) 1050 transfers the control to the VMCP. The control is transferred to the VMCP by a new PSW in the PSA 2100 of the VMCP as a kind of interruption. Since the address of the PSA of the VMCP has been set in the VMCP prefix register 1010 (FIG. 7) when the VM was started, it is referred to.
The VMCP handles the sub-channel number designated by the OS on the VM as a virtual sub-channel number, translates it to a real sub-channel number, manages a real sub-channel status and if the real sub-channel is available, designates the address translation information 2800 shown in FIG. 6 and issues an I/O instruction in place of the OS on the VM.
The interruption priority order designated by the OS on the VM is the virtual interruption priority order. The VMCP issues the I/O instruction while using the virtual interruption priority order as the real interruption priority order. Accordingly, the real interruption priority order is shared by the OS's on the VM's. Accordingly, the I/O interrupt requests from the sub-channels of the OS's on the VM's are mixedly queued in the real interruption priority order queue of the I/O interrupt request queue 2080 of FIG. 9.
The reasons for intervention by the VMCP to the execution of the I/O instruction from the OS on the VM are as follows.
(i) The virtual sub-channel number designated by the OS on the VM must be translated into the real sub-channel number.
(ii) Since the real sub-channel may be shared by the OS's on the VM's, sub-channel scheduling therefor is required.
FIG. 11 shows a manner of controlling the I/O interruption. The I/O interrupt request from the sub-channel is detected by the IOP 3000 and the corresponding sub-channel control block is queued in the I/O interrupt request queue 2080 (see FIG. 7). A structure of the I/O interrupt request queue is shown in FIG. 9, and the sub-channel control blocks are queued in the order of the real interruption priority. A bit of a corresponding real interruption pending register 1042 shown in FIG. 11 is set to "1". When the bit of the interruption pending register 1042 and the bit of the corresponding real interruption priority order mask register 1041 are both "1" and an I/O mask of the PSW 1020 is "1", the I/O interruption is initiated for the corresponding real interruption priority order and the control is transferred to the I/O interrupt processing microprogram 1060. The above operation in carried out by a hardware circuit shown in FIG. 11.
In the VMS, the real interruption priority order is shared by the OS's on the VM's as described above. Accordingly, during the running of the VM, the bits of the real interruption priority order mask register 1041 are set to the OR function of the interruption priority order masks of the OS's on the VM's or to "1" so that the interruption is always accepted. The I/O mask of the PSW 1020 is also set to "1". Consequently, if a bit of the real interruption pending register 1042 is changed to "1" by the I/O interrupt request from the sub-channel, an output of the one of AND gates 1046 becomes "1", an output of an OR gate 1043 becomes "1" and an output of an AND gate 1044 becomes "1" so that the I/O interrupt processing microprogram 1060 is immediately started by the I/O interrupt circuit shown in FIG. 11. The I/O interrupt processing microprogram 1060 dequeues the sub-channel queued in the corresponding highest interruption priority order I/O interrupt request queue (FIG. 9) to reflect the interruption to the prefix of the VMCP. If the interrupt request queue of the real interruption priority order is vacant, the bit of the real interruption priority order real interruption pending register 1042 is set to "0". As a result, the interruption pending is cleared. By the reflection of the interruption to the VMCP, the control is transferred to the I/O interrupt processing program of the VMCP. The real subchannel number which requested the I/O interruption as the I/O interrupt parameter and the corresponding VM number are also transferred to the VMCP. The VMCP carries out the following processing to reflect the I/O interruption to the VM.
(i) Translates the real sub-channel number to the virtual sub-channel number.
(ii) Checks the interruption priority mask register of the VM and the I/O mask of the PSW to determine if the I/O interruption is acceptable.
(iii) If the VM accepts the interruption, the interruption is indicated to the prefix PSA of the VM.
(iv) If the VM does not accept the interruption, the interruption is made pending by the VMCP.
Since the real interruption priority order is shared by the VM's, the mask must be set to an OR function (usually "1") of the corresponding masks of the VM's. As a result, the VMCP may be interrupted even for the noninterruptable order in the VM. In such a case, the I/O interruption is made pending by the VMCP. Accordingly, simulation by the intervention of the VMCP is required for the I/O instruction to the sub-channel.
As described above, in the I/O execution of the OS on the VM in the prior art virtual machine system, the function of the IOP for directly executing the level 3 CCW and the level 2 CCW exists but the VMCP always intervenes and the simulation is required. Accordingly, the simulation overhead of the VMCP increases for a load having a high I/O issuance frequency.
SUMMARY OF THE INVENTION
It is an object of the present invention to reduce the simulation overhead of an I/O instruction and the I/O interruption of the OS on the VM by VMCP and support direct execution of the I/O instruction on the VM and the I/O interruption by hardware and microprogram.
In accordance with the present invention, in a system having a virtual machine system (VMS) in which at least one operating system can be simultaneously run under one real computer system (host system) and a control program (VMCP) for controlling the VMS, whether an I/O device of the host system is dedicated to or occupied by an OS or not in accordance with information stored in the real computer system is determined, and if the I/O device designated by an I/O instruction other than an I/O start instruction issued by the OS is dedicated to the OS which is currently being run, the I/O instruction is issued to that I/O device, and if it is not dedicated to the OS which is currently running, the OS is interrupted and control is transferred to the VMCP.
BRIEF DESCRIPTION OF THE DRAWINGS
The present invention will be apparent from the following detailed description taken in conjunction with the accompanying drawings, in which:
FIG. 1 is a block diagram of a real computer system by a conventional OS;
FIG. 2 is a block diagram of a prior art virtual machine system (VMS);
FIG. 3 shows a memory hierarchy in a prior art virtual machine (VM);
FIGS. 4-11 show prior art examples in which;
FIGS. 4A to 4C show address translation tables;
FIG. 5 shows the VM main memory which occupies a continuous area of a real main memory;
FIG. 6 shows an operand of an I/O instruction issued by a VMCP to simulate the I/O of the VM; and sub-channel registers;
FIG. 7 shows a configuration of a host system;
FIG. 8 shows an I/O request queue;
FIG. 9 shows an I/O interrupt request queue;
FIG. 10 shows real sub-channel control blocks;
FIG. 11 shows an I/O interrupt circuit;
FIGS. 12 to 22 relate to the present invention in which:
FIG. 12 shows a configuration of a host system;
FIG. 13 shows a prefix control table;
FIG. 14 shows a device address translation table and priority order translation table;
FIG. 15 shows a main memory address translation table;
FIG. 16 shows real sub-channel control blocks;
FIG. 17 shows a start VM instruction;
FIG. 18 shows a VM number register;
FIG. 19 shows VMS control flags;
FIGS. 20A and 20B illustrate a manner of assigning interruption priority orders;
FIGS. 21A -21D shows a VMS interrupt control registers;
FIG. 22 shows a VMS I/O interrupt circuit.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
The preferred embodiments of the present invention are now described. FIG. 12 shows an overall configuration of one embodiment of the present invention.
Elements of a CPU 1000' are similar to those of FIG. 7 but some of them are expanded in function. An HSA 2001 includes the same elements as those in FIG. 7. (I/O request queue 2070, I/O interrupt request queue 2080 and real sub-channel control blocks 2090'.). However, a prefix control table 2300, a translation table address management table 2400 and a VM management table 2700 include new information.
A programmable area 2002 includes the same elements as those of FIG. 7 (VMCP PSA 2100, VM1 PSA 2110, VM2 PSA 2120, (PSA's of other VM's), VMCP 2200, level 2 memory to level 1 memory address translation tables 2010 and level 3 memory to level 2 memory address translation tables 2040). However, an interruption priority order number translation table 2500 and sub-channel number translation tables 2600 include new information. An IOP 3000' is similar to the IOP 3000 in FIG. 7 in configuration but expanded in function. The new information included in the HSA 2001 and the programmable area 2002 is now explained.
FIG. 13 shows the prefix management table 2300. It includes the VMCP PSA address, VM1 PSA address, VM2 PSA address and VM3 PSA address. While not shown in FIG. 13, other VM PSA's may be registered. The PSA addresses are referred by a microprogram of the CPU 1000' and they are addresses in a host system programmable area 2002. The VM PSA address is imparted as one of start instruction operands when the VM is started and it is stored in the corresponding entry of the prefix management table 2300 when the instruction is executed. A start address of the prefix management table 2300 is stored in one of the control registers 1100' of the CPU 1000' (see FIG. 12). The prefix management table is optional. A case where it is used will be explained later. FIG. 14 shows the translation table address management table 2400. It contains a start address of the sub-channel number translation table 2600 and a start address of the interruption priority order translation table 2500, for each VM. A start address of the translation table address management table 2400 is also stored in one of the control registers 1100' of the CPU 1000'. A method of looking up the sub-channel number translation table 2600 and the interruption priority order translation table 2500 is shown in FIG. 14. A virtual sub-channel number (two bytes) is divided into D0.256 and Dl, and a first half table 2601 pointed to by the content of the corresponding entry of the address management table 2400 is looked up by D0. An address of a second half table 2602 is contained in the D0-th entry of the first half table 2601 so that a D1-th entry of the second half table 2602 is looked up. In this manner, the corresponding real sub-channel number D0'.256+D1' is obtained. The virtual interruption priority order is translated to the corresponding real interruption order by merely reading the corresponding entry of the translation table 2500. The sub-channel number translation table 2600 and the interruption priority order translation table 2500 are prepared by the VMCP when they are designated by the VMCP command or when the VM is defined from the VM defining information, and designated by the start instruction operand when the VM is started, and stored in the corresponding entry of the translation table address management table 2400 when the start instruction is executed. The translation tables 2600, 2500 and 2400 are optional. Those translation tables are not necessary so long as the VM which uses the I/O execution system of the present invention in the VMS obeys a rule of virtual sub-channel number being equal to a real sub-channel number, and virtual interruption priority order being equal to real interruption priority order.
FIG. 15 shows the content of the VM management table 2700. It contains sizes (Z0, Z1, . . . ) of the main memories of the corresponding VM's, and address (RATOR0, RATOR1, . . . ) of the level 2 memory address to level 1 memory address translation table 2010. Such information is derived from the VM definition information and stored in the corresponding entry of the VM control table 2700 in the HSA 2001 by the start VM instruction. A start address of the VM control table 2700 is stored in one of the control registers 1100' (see FIG. 12) in the CPU 1000'. A start address of the control block in the HSA 2001 is stored in the control register 1100' in the CPU 1000' as is done in the prior art system. When the VM which supports the I/O execution system of the present invention is limited to one which occupies the continuous area on the main memory 2002 (FIG. 5) as a main memory therefor, the VM management table 2700 may be replaced by a translation table 2010(2) which defines upper and lower limits. When the translation table 2010(2) shown in FIG. 5 is used, the upper and lower limit addresses α i and α i+1 (i=1, 2, 3,. . . ) are designated by the VM start instruction, and the corresponding entry of the translation table 2010 (2) is set in the HSA 2001 as the instruction is executed. FIG. 16 shows the real sub-channel control blocks 2090', one real sub-channel control block 2091' thereof and a VM information area 2092' thereof. The VM information area 2092' includes status field, VM number, virtual sub-channel number, corresponding real sub-channel number, virtual interruption priority order, corresponding real interruption priority order and CCW address translation information 2094. The status field includes flags indicating whether the sub-channel is occupied or not and whether the sub-channel is in an I/O direct execution suppress mode or not. The CCW address translation information 2094 has the same content as the address translation information 2092 of FIG. 10. The information in the VM information area 2092' is set from the VM definition information when the VM is defined, or when it is designated by the VMCP command, or when the I/O instruction is executed.
The dedication of the real sub-channel or the dedication of the real interruption priority order is designated when the VM is defined or by the VMCP command. When a real sub-channel is dedicated, the following fields in the VM information area 2092' are set.
A sub-channel dedication flag in the status field 2093
The I/O direct execution mode suppress flag is normally set to "0" and the I/O direct execution mode is set to a support state.
A VM number to which the sub-channel is dedicated,
Virtual sub-channel number and real sub-channel number
Start address (RATOR, see FIG. 4a) of the dedicating VM main memory (level 2 memory) to level 1 memory address translation table, in the CCW address translation information 2094. If the VM occupies the main memory shown in FIG. 5, the upper and lower limits thereof α i and α i+1 (i=1, 2, 3, . . . ) may be set.
In the shared sub-channel, such information is set as required when the I/O instruction is executed. In this case, it is set in the corresponding field on the VM information area of the I/O issuing VM.
FIG. 17 shows the format of the start VM instruction. Numeral 2900 denotes the start VM instruction and numeral 2910 denotes an operand. The operand 2910 contains the VM number, VM PSW, VM PSA address, start address of the sub-channel number translation table 2600 (FIG. 14), start address of the interruption priority order translation table 2500 (FIG. 14), start address RATOR (see FIG. 4a) of the VM main memory to host system main memory address translation table 2010 (FIG. 15) and VM main memory size. (For the latter two, when the VM to be started uses the continuous area of the main memory 2002 shown in FIG. 5 as the VM main memory, the upper and lower limits α i and α i+1 (i=1, 2, 3, . . . ) may be designated. Of those operand information, the VM running PSW, VM PSA address, real interruption priority order status and VMS control flags are determined when the VM is started, and other information is determined by the VM definition information when the VM is defined. The real interruption priority order status, real interruption priority order dedication status and VMS control flags will be explained later. Those operands are set by the VMCP. The start VM instruction is not necessarily of the format shown in FIG. 17, although the information shown in FIG. 17 is needed as the operands. FIG. 18 shows a VMS control register 1080. A register 1081 contains the VM number of the currently running VM and is set by the start VM instruction. The content of the register is given by the content of one field of the operand 2910 (FIG. 17) of the start VM instruction. FIG. 19 shows the VMS control flags 1090' (see FIG. 12). The flags are initialized by one field of the operand of the VM start instruction (FIG. 17). The flags have the following meanings, respectively.
V: It is "1" during running of the VM. It is "0" during running of the VMCP or running in the real computer mode. It is set to "1" by the start VM instruction and set to "0" when the control is transferred to the VMCP by the interruption. It is similar to the prior art system (FIG. 7).
H: It is set to "1" when a privileged instruction may be directly executed during the running of VM. When this flag is "1", most privileged instructions in the running of VM are directly executed by the instruction execute circuit of the CPU 1000'. When H is "1", it is a high speed VM mode, similar to the prior art system (FIG. 7).
R: It is set to "1" when the OS on the VM is limited such that the virtual sub-channel number is equal to the real sub-channel number, and the virtual interruption priority order is equal to the real interruption priority order. When this flag is "1", the sub-channel number translation and the interruption priority order translation by the microprogram are eliminated. (In this case, the translation tables 2400, 2600 and 2500 shown in FIG. 14 are not necessary.)
D: It is "1" when the direct I/O execution by the VM (without the intervention of the VMCP) in accordance with the present invention is enabled. It is initially set to "1" by the start VM instruction of the VMCP.
In general, a VM can accept an I/O interruption from an I/O interruption priority order only if both the VM's PSW I/O mask is "1" and the I/O interruption priority order mask of the VM is "1". When the currently running VM has an I/O interruption pending factor on a shared I/O interruption priority order, and the pending is caused by the fact that the shared I/O interruption priority order mask of the VM is "1", and the VM's PSW I/O mask, however, is "0", the N is set to "1". The pending factor is actually managed by the VMCP for the VM.
The N is used when an I/O instruction which checks the I/O interrupt request of the VM is issued from the OS on the VM. That I/O instruction checks the I/O interruption from an I/O interruption priority order whose mask of the VMis "1". The N is initialized by the VMCP by the start VM instruction. It is used when an instruction for checking the I/O interrupt virtual interruption priority order mask is "1" is executed. It is initialized by the VMCP by the start VM instruction.
FIGS. 20a and 20b show a method of assigning the real interruption priority orders. 32 real interruption priority orders 0-31 are used. The real interruption priority order 0 is the highest priority order and is exclusively used by the VMCP. The real interruption priority orders to be dedicated to the VM's are assigned to the VM's in the ascending order starting from the real interruption priority order 1 (descending order in the interruption priority order). The shared interruption priority orders are assigned to the VM's in the descending order starting from the real interruption priority order 31 (ascending order in the interruption priority order). In FIGS. 20a and 20b, the real interruption priority order 1 is assigned to the virtual interruption priority order 0 of the VM1 and it is exclusively used, and the real interruption priority order 31 is assigned to the virtual interruption priority orders 1-7 and it is shared by the VM's. For the VM2 and VM3, the assignment is done as shown in FIGS. 20a and 20b. The virtual interruption priority order in the VM1 is actually 0 or (1-7). Accordingly, there are two real interruption priority orders which can be effectively used by the OS on the VM1. The restriction to the OS can be permitted. The particular interruption priority order to be dedicated to the VM should be determined under an overall plan of the VMS and controlled by the VMCP. The exclusive or shared status of the real interruption priority order thus determined is given by the operand of the start VM instruction (see FIG. 17) and set into the real interruption priority order dedicated status register 1049 (FIG. 21) when the instruction is executed.
FIG. 21 shows the real interruption priority order mask register 1041', real interruption pending register 1042', real interruption priority order status register 1045 and real interruption priority order dedication status register 1049. Those are all included in the I/O interrupt circuit 1040' of FIG. 12. The registers 1041' and 1042' are similar to those in the prior art system but have increased number of bits. In FIG. 21, they have 32 bits which are four times as large as 8 bits in the prior art system, in order to support the dedication system of the real interruption priority order in the VM. The explanation thereof is omitted because the meaning is the same. The meaning of the real interruption priority order status register 1045 is described below. It means that when the bit n (0-31) is "0", the real interruption priority order n is dedicated to the currently running VM. In another case, it is set to "1". The content of the real interruption priority order dedication status register 1049 is described below. When a bit c (0-31) is "0", it means that the real interruption priority order c is dedicated to a VM, and when the bit c is "1", it means that the real interruption priority order c is shared. The registers 1045 and 1049 are initialized by the operand of the start VM instruction. The real interruption priority order mask register 1041' is controlled and updated by the VMCP. The real interruption pending register 1042' is set by the IOP 3000' (FIG. 12) and reset by the I/O interrupt processing microprogram 1060' (FIG. 22).
FIG. 22 is a circuit diagram of the I/O interrupt circuit 1040' of the present invention. For the sake of simplicity, only ten real interruption priority orders are shown in FIG. 22 but there are actually 32 orders connected in a similar manner. Let us assume that the real interruption priority order c (c=0-31) has an interruption pending factor (that is, the sub-channel having the interrupt request is queued to the real interruption priority order (c) level queue of the I/O interrupt request queue 2080 and the corresponding bit of the pending register 1042' is set to "1"). If the interruption priority order c is dedicated to the currently running VM, the corresponding bit of the real interruption priority order status register 1045 is zero, and the OR gate 1048 outputs the content of the I/O mask of the PSW so that the I/O interrupt mask of the PSW 1020 is effective. Accordingly, only when the corresponding bit of the corresponding real interruption priority order mask register 1041' is "1" and the I/O mask of the PSW is "1", the corresponding output of the AND gate 1047 is "1", the I/O interruption is started and the control is transferred to the I/O interrupt processing microprogram 1060'. When the interruption priority order c is shared or dedicated to another VM, the corresponding bit of the register 1045 is "1", the corresponding output of the OR gate 1048 is "1" and the I/O mask of the PSW 1020 is ignored so that the I/O interruption is started if the bit of the corresponding real interruption priority order mask register 1041' is "1". After the processing of the interruption by the microprogram 1060', if the interrupt request queue of the interruption priority order c is vacant, the corresponding bit of the pending register 1042' is cleared to "0" by the microprogram.
The manner in which the I/O instruction of the OS on the VM and the I/O interruption are executed and processed by the hardware, microprogram and information on the main memory is now explained.
The following presumptions are made and the VM is in the high speed VM mode.
(i) The entire main memory of the VM is resident in the main memory of the host system.
(ii) The direct I/O execution of the OS on the VM (without the intervention of the VMCP, including the direct execution of the I/O interrupt) is supported only for the dedicated sub-channel and the sub-channel having the dedicated interruption priority order.
When the VM is started, the VMCP sets the operand of the start VM instruction of FIG. 17 and the value of the bit c of the real interruption priority order mask register 1041' in a manner shown below.
When the real interruption priority order c (0-31) is dedicated to the currently running VM, its mask is set to the mask of the corresponding virtual interruption priority order (only one is assumed for the sake of simplicity) of the OS on the VM.
When the interruption priority order c is dedicated to other VM, its mask is set to the value of an AND function of the mask of the corresponding virtual interruption priority order of the VM and the I/O mask of the PSW of the VM. Alternatively, the bit c may be set to "0" if the delay of the interruption of the interruption priority order c does not cause a problem.
When the interruption priority order c is shared by the VM's, the bit c is set to "1".
When the virtual interruption priority order mask is changed during the running of the VM, the change is immediately reflected to the real interruption priority order mask register 1041' (FIG. 21). Accordingly, the instruction to change the virtual interruption priority order mask of the OS may be simulated via the VMCP or the change may be reflected to the register 1041' by the microprogram processing of the CPU, as is done in the prior art system. When the VM in the high speed VM mode is started, the PSW of the VM is set in the VM PSW of the operand of the start VM instruction of FIG. 17 and it is set in the PSW 1020 (FIG. 12) of the CPU 1000'. Accordingly, the I/O mask of the PSW coincides with the I/O mask of the running VM. The coincidence is attained because the change of the PSW of the OS during the VM run is immediately reflected to the PSW 1020. The instruction to change the PSW of the OS may be reflected to the PSW 1020 of the CPU 1000' by the direct execution or may be reflected by the simulation via the VMCP. After those settings, the control is transferred to the OS on the VM by the start VM instruction (FIG. 17). As the instruction is executed, the currently running VM number register 1081 of FIG. 18, PSW 1020 (FIG. 12) of the CPU 1000', the corresponding entry of the prefix control table of FIG. 13, the corresponding entry of the translation table address, management table 2400 of FIG. 14, the corresponding entry of the VM management table of FIG. 15, real interruption priority order status register 1045 of FIG. 21 and VMS control flags of FIG. 19 are initialized.
Let us assume that the I/O instruction is issued from the OS on the VM. The I/O execute circuit 1030' of the CPU 1000' carries out the following processings under the control of the microprogram 1050'.
(1) If not in the high speed VM mode (VMS control flag H="0", see FIG. 19), the OS is interrupted and control is transferred to the VMCP by reflecting the interruption to the PSA 2100 of the VMCP by using the prefix register 1010 of the VMCP (FIG. 12).
(2) In the high speed VM mode (VMS control flag H="1"), whether the VM is in an I/O direct execution mode (VMS control flag D="1") or not is checked (FIG. 19).
(3) When D="0", the OS is interrupted and control is transferred to the VMCP.
(4) When D="1", the VMS control flag R is checked. If R="0", the corresponding virtual sub-channel number translation table 2600 is looked up to translate the given virtual sub-channel number to a real sub-channel number. If the virtual interruption priority order is given by the instruction operand, the interruption priority order translation table is looked up to translate it into the real interruption priority order. Whether it is dedicated or not is checked by the real interruption priority order dedication status register 1049, and it is written into the status field of the VM information area 2092' of the sub-channel control block (FIG. 16).
The correspondence between the virtual interruption priority order and the real interruption priority order is also written. When R="1", no translation is required and the same values are written.
(5) When the real sub-channel control block 2091' (FIG. 16) obtained is the dedicated sub-channel and has the dedicated interruption priority order, the I/O instruction is executed. The subsequent operation is similar to that in the real computer system. When an asynchronous I/O device operation is required, the sub-channel is queued in the I/O request queue 2070 (FIG. 8). A condition code and control are returned to the program which issued the I/O.
(6) If the real sub-channel obtained is the shared sub-channel or the interruption priority order is shared, the OS is interrupted, control is transferred to the VMCP and the simulation is effected. The remaining processes are entrusted to VMCP's simulation.
(7) If the I/O instruction issued by the OS on the VM is one which examines an I/O interrupt request whose virtual interruption priority order mask is "1", the following processing is carried out. The interrupt request is checked for the dedicated real interruption priority order of the current running VM. If there is no I/O interrupt request, the shared interruption priority order should be checked. Since the VMCP manages the interrupt pending for the shared interruption priority order, it is necessary to transfer the control to the VMCP. However, since this is contrary to the principle of direct execution, the control flag N (FIG. 19) of the VMS is used. When N="1", it means that VMCP holds the I/O interrupt the shared interruption priority order and its virtual interruption priority order mask is "1". Accordingly, the OS is interrupted and control is transferred to the VMCP. When N="0", there is no such I/O interrupt pending and the OS need not be interrupted and the direct execution is permitted. The I/O interrupt processing is now explained.
(1) The I/O interrupt request from the I/O device is detected by the IOP 3000' and the corresponding real sub-channel control block is queued in the corresponding real interruption priority order of the I/O interrupt request queue 2080 of the HSA 2001 (see FIG. 9), as is done in the prior art system.
(2) The IOP 3000' shown in FIG. 22 sets the corresponding bit of the real interrupt pending register 1042' to "1", as is done in the prior art system.
(3) The real interruption priority order mask register 1041' is set in the manner described before. The I/O interrupt circuit of FIG. 22 operates in the manner described above. Let us assume that the I/O interruption was started and the control was transferred to the I/O interrupt processing microprogram 1060'.
(4) If the interruption occurs with the real dedicated interruption priority order of the VM, the VM can accept the interruption for the virtual interruption priority order because of the settings in the real interruption priority order mask register 1041' and the real interruption priority order status register 1045. If the VM cannot accept the interruption, the I/O interruption cannot occur for that real interruption priority order by the actions of the I/O mask of the PSW 1020 and the registers 1041' and 1045, and the control is not transferred to 1060' but it is made pending by the hardware.
(5) The I/O interrupt microprogram 1060' carries out the following processings.
(i) Dequeues the real sub-channel of the I/O interrupt request queue 2080 (FIG. 9) on the real interruption priority order c requested the interruption.
(ii) Checks the VM mode flag bit V and the high speed VM mode flag H of the VMS control flag 1090' (FIG. 19), and if V="0" or H="0", reflects the interruption to the PSA of the VMCP. The PXR 1010 of the VMCP (FIG. 12) is used and control is transferred to the VMCP.
(iii) If V="1" and H="1", checks the I/O direct execution mode bit D of the VM. If D="0", it is not the I/O direct execution mode, and reflects the interruption to the PSA of the VMCP.
(iv) If D="1", the following processings are carried out.
(a) Whether the sub-channel is dedicated or not is determined by the status field (FIG. 16) in the real sub-channel control block, and if it is the shared sub-channel, reflects the interruption to the PSA of the VMCP.
(b) If the real interruption priority order c requesting the interruption is dedicated to the currently running VM, that is, if the corresponding bit of the real interruption priority order status register 1045 is "0" (see FIG. 21), reflects the interruption to the PSA of the currently VM to continue the current VM. The VM prefix register 1070 (FIG. 12) is used. The I/O interrupt information to the VM prefix is reflected by the virtual sub-channel number in the real sub-channel control block 2092' or the virtual interruption priority number.
(c) When the real interruption priority order c is dedicated to another VM, the interruption is reflected to the VMCP. Then, the interruption is reflected to the PSA of the VM by the VMCP.
(d) When the real interruption priority order c is shared, the interruption is reflected to the VMCP. Then, the interruption is reflected to the VM by the VMCP. The VM may not accept the interruption. In such a case, the I/O interruption is held pending by the VMCP.
As described above when the sub-channel is dedicated and has the dedicated real interruption priority order, the I/O direct execution (without the intervention of the VMCP) of the OS on the VM is supported for that sub-channel. For the I/O interruption, only the I/O interruption from the sub-channel dedicated to the current running VM is directly executed. For the I/O interruption from the sub-channel dedicated to another VM, the VMCP is to intervene because of necessity for scheduling of the VM's.
The direct I/O execution mode suppress flag of the status field 2093 in the real sub-channel control block of FIG. 16 is normally "0" so that the direct I/O execution mode of that sub-channel is supported. In the dedicated sub-channel, the I/O instruction is not issued from the OS on the VM other than the occupying VM but it may be issued from the VMCP. In this case, the direct I/O execution mode suppress flag in the status field 2093 is set to "1" until the I/O of the VMCP is completed so that the I/O direct execution mode for that sub-channel is suppressed.
Accordingly, this flag is set and reset under the control of the VMCP. In the above I/O execution system, the following considerations are pointed out.
(a) The R bit of the VMS control flags 1090' (FIG. 19) may be omitted. It is not necessary if the virtual sub-channel number and the virtual interruption priority order are always translated, or if those numbers are always equal when the direct I/O execution system of the present invention is applied in the VMS.
(b) The D flag may be replaced by the H flag, but the high speed VM mode flag H cannot control the direct execution of only the I/O instruction because it also controls the direct execution of the privileged instructions other than the I/O instruction.
(c) In the I/O interrupt processing, the I/O interruption from the real interruption priority order dedicated to the VM other than the currently running VM is reflected to the VMCP, as described above. Since the VM to which it is dedicated can accept the interruption, the interruption may be reflected to the PSA of that VM and then the control may be transferred to the VMCP in a form of VMCP call. The address of the PSA of the VM can be determined from the prefix management table of FIG. 13. In this case, it is necessary to determine the PSW of the VM and information therefor is required. It may be determined based on the VM number in various ways, although it is not illustrated.
(d) The start address of the sub-channel number translation table, the start address of the interruption priority order translation table, the real interruption priority order status register 1045 and the real interruption priority order dedication status register 1049 (FIG. 21) are all initialized by the operand of the start VM instruction (see FIG. 17). Alternatively, they may be initialized by a separate instruction of the VMCP.
As described hereinabove, in accordance with the present invention, the I/O instruction issued by the OS on the VM and the I/O instruction can be directly executed so that the I/O simulation overhead of the VMCP can be substantially reduced. This is an essential function to attain a virtual machine which has a performance very close to that of a real computer.
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In a virtual machine system (VMS) capable of concurrently running at least one operating system (OS) under one real computer system and a control program (VMCP) for controlling the VMS, the object is to reduce the overhead produced for simulating VM I/Os by direct I/O execution. A VM information area of a real sub-channel control block has a status field in which a flag indicating that the sub-channel is dedicated or not is contained. When the flag is "1", it means that the sub-channel is dedicated to the VM and the sub-channel scheduling by the VMCP is not necessary. As a real interruption priority order is dedicated to a VM, only I/O interruption requests of the VM are queued into the real interruption request queue of that dedicated priority order, and the mixing of VMs in that real interruption priority order is avoided. When an interruption control mask of an interruption priority order of the OS on the VM is "0" indicating that the interruption is not acceptable by the VM, the interruption conrol mask of the corresponding dedicated real interruption priority order is also "0" and the hardware interruption does not take place. Accordingly, the interruption is retained by the hardware and the I/O interruption retention for the VM by the VMCP is avoided.
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FIELD OF THE INVENTION
The present invention relates to a system including an input-output controller such as a SCSI (Small Computer System Interface) controller, etc. and a method for detecting a failure when installing an input-output controller.
BACKGROUND OF THE INVENTION
A computer system generally comprises a number of input-output (I/O) controllers such as a LAN controller and a SCSI controller in addition to a control section (hereinafter referred to as a processor unit) including a processor that takes a central part in the system and a memory. The processor unit is connected to other units via system buses. There have been disclosed some techniques for fault detection concerned with the system bus in Japanese Patent Applications laid open No. HEI4-8147, laid open No. HEI7-168727, and laid open No. HEI8-263328.
A SCSI port is a standard interface for connecting the peripheral equipment such as a HDD (Hard Disk Drive) with the processor unit. With the SCSI port, a SCSI controller is used as an I/O controller to be a host for communicating with a magnetic disk and the like. Techniques involved with the SCSI controller have been disclosed, for example, in Japanese Patent Applications laid open No. HEI11-203239 and laid open No. HEI11-110138.
Generally, in a conventional system, I/O controllers like the SCSI controller are installed in the system when the operation of the processor unit starts. At a restart of the processor unit or when executing an instruction from a system maintainer to install an I/O controller, only a part of memory area related to the operation of the I/O controller is used and installation processing is simply carried out during the process of the installation. After completion of the installation, necessary parts of memory area are selectively used for executing respective instructions each time when I/O access occurs in operation.
In the following, a description will be given of problems in the above-mentioned conventional techniques and systems.
The first problem is that an I/O bus access fault which occurs while using an I/O controller has an impact on the whole processor system, thus causing a system failure. This is because a fault cannot be located when the fault occurs in the I/O bus access from the I/O controller to the memory.
The second problem is that the I/O controller which has caused the failure can be reinstalled when restarting the processor. This is because normal operation is performed at the stage of installation processing since only sectional I/O bus accesses may occur when installing the I/O controller.
The third problem is that in the case where an I/O controller having slave/master relationships with plural devices (slave devices), for example, the SCSI controller and disk storage units are installed and one of the slave devices has a failure, the slave device with the failure cannot be specified.
Besides, in a system adopting a disk array, etc., there is a case where an additional disk storage unit is installed in the active system in which the SCSI controller and a disk storage unit #A have been already installed. When a SCSI controller failure is detected on such occasion and failure recovery is performed for the SCSI controller while the disk storage unit #A is in use, accessing to the disk storage unit #A is interrupted, which affects a software or program running on the system.
SUMMARY OF THE INVENTION
It is therefore an object of the present invention to provide a failure detection method enabling the detection of I/O bus failure and address parity error when installing I/O controllers such as a SCSI controller, etc. connected to a system bus in a computer system, thus improving the reliability of the system.
It is another object of the present invention to provide a failure detection method enabling failure location when installing units in slave/master relationships (e.g. SCSI controller and disk storage units) and also when installing an additional slave in a computer system, thus improving the reliability of the system.
In accordance with the first aspect of the present invention, to achieve the above objects, there is provided a failure detection method for detecting a failure at a time when installing an I/O controller in a computer system, comprising the steps of executing an instruction which involves providing I/O bus access to a memory to be used by the I/O controller after installed; determining that there is no failure when predetermined results are obtained with the instruction; and installing the I/O controller in the system.
In accordance with the second aspect of the present invention, there is provided a failure detection method for detecting a failure at a time when installing an I/O controller in a computer system, comprising the steps of: executing an instruction which involves providing I/O bus access to a memory to be used by the I/O controller after installed; determining that there is no failure when predetermined results are obtained with the instruction and installing the I/O controller in the system; and notifying a host processor that there is a failure in the I/O controller when predetermined results are not obtained with the instruction so that the host processor can specify the I/O controller with the failure.
In accordance with the third aspect of the present invention, in the first or second aspect, the failure detection method further comprises the steps of executing a micro diagnostic program stored in the I/O controller; and installing the I/O controller in the system when it is verified that there is no failure by the micro diagnostic program.
In accordance with the fourth aspect of the present invention, in one of the first to third aspects, the I/O controller has slave/master relationships with a plurality of slave units, and the failure detection method further comprises the steps of: detecting a failure in the respective slave units when installing the I/O controller; and when a failure is found in any of the slave units, notifying the host processor of the slave unit having the failure.
In accordance with the fifth aspect of the present invention, in the fourth aspect, the failure detection method further comprises the steps of: executing an instruction which involves providing I/O bus access to a memory to be used by the respective slave units after installed; determining that there is no failure when predetermined results are obtained with the instruction; and notifying the host processor of the slave unit having a failure when predetermined results are not obtained with the instruction.
In accordance with the sixth aspect of the present invention, in one of the first to fifth aspects, the I/O controller is a SCSI controller.
In accordance with the seventh aspect of the present invention, in one of the first to sixth aspects, a system maintainer is informed as to the result of the installation of the I/O controller.
BRIEF DESCRIPTION OF THE DRAWINGS
The objects and features of the present invention will become more apparent from the consideration of the following detailed description taken in conjunction with the accompanying drawings in which:
FIG. 1 is a block diagram showing the configuration of the main part of a preferred computer system for illustrating an application of the present invention;
FIG. 2 is a flowchart showing the operation process according to the first embodiment of the present invention;
FIG. 3 is a block diagram showing the configuration of the main part of another preferred computer system for illustrating an application of the present invention; and
FIG. 4 is a flowchart showing the operation process according to the second embodiment of the present invention.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
Referring now to the drawings, a description of preferred embodiments of the present invention will be given in detail.
FIG. 1 is a block diagram showing the configuration of the main part of a preferred computer system for the application of the first embodiment of the present invention. With reference to FIG. 1 , the computer system comprises a processor unit 100 that operates under program control, an I/O controller 110 , a memory 120 , and an I/O bus 130 . The I/O controller 110 may be a general-purpose I/O controller such as a SCSI controller and a LAN controller.
The processor unit 100 includes an I/O controller management means 101 , an I/O driver means 102 , an I/O controller diagnostic means 103 , and a memory management means 104 .
The I/O controller management means 101 manages the condition of the I/O controller 110 . The I/O driver means 102 provides access to the I/O controller 110 . The I/O controller diagnostic means 103 verifies normal operation of the I/O controller 110 preparatory for installing the I/O controller 110 . The memory management means 104 manages accesses to the memory 120 from all units or sections. The respective means are generally realized from the execution of a program by the processor.
In the following, a detailed description will be given of the operation of the system according to the first embodiment of the present invention referring to FIGS. 1 and 2 . When the processor unit 100 is activated, the I/O controller diagnostic means 103 receives an I/O controller diagnostic request set as part of the prescribed starting up process of the processor unit 100 (step S 201 in FIG. 2 ). Subsequently, the I/O controller diagnostic means 103 sets the I/O controller management means 101 in diagnostic mode (step S 202 ). The I/O controller management means 101 issues an I/O controller installing instruction to the I/O driver means 102 (step S 203 ).
The I/O driver means 102 first hunts a memory area for control operation by the I/O controller 110 through the memory management means 104 (step S 204 ). Then, the I/O driver means 102 executes a prescribed pseudo-I/O instruction so that bidirectional access occurs between the I/O controller 110 and the memory 120 to use a part or block of the memory area for control operation hunted previously (step S 205 ).
Next, the I/O driver means 102 judges whether a specific normal response to the pseudo-I/O instruction has been obtained (step S 206 ).
If the normal response has been obtained (step S 206 /YES), the I/O driver means 102 checks whether all the memory patterns are tried, namely, all the space in the memory area for control operation has been used (step S 207 ). If unused memory area remains (step S 207 /NO), the I/O driver means 102 returns to the operation at step S 205 and executes the similar pseudo-I/O instruction to use another part or block of the memory area for control operation.
The I/O driver means 102 repeats the procedure from step S 205 to S 207 for all the memory blocks of address space necessary for I/O bus access verification.
If the normal response has not been obtained (step S 206 /NO), the I/O driver means 102 stops the instillation operation, and notifies the I/O controller diagnostic means 103 that there is a failure.
The memory 120 and I/O bus 130 are verified by the judgment on whether the specific normal response to every pseudo-I/O instruction has been obtained or not as is described above.
If the normalcy of the I/O bus 130 is verified, that is, the specific normal response to every pseudo-I/O instruction has been obtained (step S 207 /YES), the I/O driver means 102 carries out the installation operation (step S 208 ), and notifies the I/O controller diagnostic means 103 of the operation result.
The I/O controller diagnostic means 103 judges whether or not the installation operation has been normally performed (step S 209 ).
If the installation operation has been normally performed (step S 209 /YES), the I/O controller diagnostic means 103 activates a micro diagnostic program stored in the I/O controller 110 (step S 210 ), and indicates to the system maintainer the diagnostic result that the I/O controller 110 has been installed by display or the like (step S 211 ). After that the I/O controller diagnostic means 103 releases the I/O controller management means 101 from the diagnostic mode (step S 212 ).
On the other hand, if the installation operation has not been normally performed (step S 209 /NO), the I/O controller diagnostic means 103 indicates to the system maintainer the diagnostic result by display or the like (step S 211 ), and releases the I/O controller management means 101 from the diagnostic mode (step S 212 ).
In accordance with the first embodiment of the present invention, the normalcy of the I/O bus is verified when installing the I/O controller as is described above. Consequently, it is possible to detect an I/O bus failure as well as checking address parity in advance of the installation of the I/O controller, thereby preventing a failure from occurring after the installation. Thus, the reliability of the system can be improved.
In the following, the second embodiment of the present invention will be described.
FIG. 3 is a block diagram showing the configuration of the main part of a preferred computer system for the application of the second embodiment of the present invention. Referring to FIG. 3 , the computer system comprises a processor unit 300 that operates under program control, a SCSI controller 310 as an I/O controller, disk storage units 320 A and 320 B as slave units of the SCSI controller 310 , a memory 330 , and an I/O bus 340 .
The processor unit 300 includes an I/O controller management means 301 , an I/O driver means 302 , and a memory management means 303 .
The I/O controller management means 301 sends an I/O controller installing instruction to the I/O driver means 302 at a restart of the processor unit 300 or when the system maintainer gives an instruction to install an I/O controller. The memory management means 303 manages accesses to the memory 330 from all units or sections.
Having received the I/O controller installing instruction as a trigger, the I/O driver means 302 executes an instruction so that accesses occurs from the SCSI controller 310 to the memory 330 and vice versa to verify whether bidirectional access between the controller 310 and the memory 330 can be normally gained (pre-installation check).
After obtaining the verification, the I/O driver means 302 installs the SCSI controller 310 , disk storage units 320 A and 320 B in the system. Accordingly, it becomes possible for other controllers (not shown) to use the disk storage units 320 A and 320 B.
When a failure is detected by the pre-installation check, the I/O driver means 302 notifies a host processor of the failure. Thus, the host processor can specify or locate the unit with the failure.
In the following, a detailed description will be given of the operation of the system according to the second embodiment of the present invention referring to FIGS. 3 and 4 . At a start or restart of the system, the I/O controller management means 301 receives a SCSI controller installing instruction set as part of the prescribed starting up process of the processor unit 300 (step S 401 in FIG. 4 ). Incidentally, the system maintainer may input the SCSI controller installing instruction as needed while the system is in operation. The I/O controller management means 301 receives the SCSI controller installing instruction in this case as well, and conducts the same operations as follows.
Having received the SCSI controller installing instruction, the I/O controller management means 301 issues a SCSI controller installing instruction to the I/O driver means 302 (step S 402 ).
The I/O driver means 302 first hunts memory areas for the control operation of the SCSI controller 310 and the disk storage units 320 A and 320 B through the memory management means 303 (step S 403 ). Then, the I/O driver means 302 executes a pseudo-I/O instruction so that bidirectional access occurs between the SCSI controller 310 and the memory 330 to use a part or block of the memory area for the control operation of the SCSI controller 310 hunted previously (step S 404 ).
Next, the I/O driver means 302 checks whether all the space in the memory area for control operation of the SCSI controller 310 has been used (step S 405 ). If unused memory area remains (step S 405 /NO), the I/O driver means 302 returns to the operation at step S 404 and executes the similar pseudo-I/O instruction to use another part or block of the memory area for control operation of the SCSI controller 310 . The I/O driver means 302 repeats this until all the memory address space necessary for I/O bus access verification has been used.
If all the space in the memory area for control operation of the SCSI controller 310 has been used (step S 405 /YES), the I/O driver means 302 executes a pseudo-I/O instruction to use a part or block of the memory area for control operation of the disk storage units 320 A and 320 B hunted previously (step S 406 ).
Similarly, the I/O driver means 302 checks whether all the space in the memory area for control operation of the disk storage units 320 A and 320 B has been used (step S 407 ). If unused memory area remains (step S 407 /NO), the I/O driver means 302 returns to the operation at step S 406 and executes the similar pseudo-I/O instruction to use another part or block of the memory area for control operation of the disk storage units 320 A and 320 B. The I/O driver means 302 repeats this until all the memory address space for controlling the disk storage units 320 A and 320 B necessary for I/O bus access verification has been used.
If all the space in the memory area for control operation of the disk storage units 320 A and 320 B has been used (step S 407 /YES), the I/O driver means 302 judges whether the specific normal response to every pseudo-I/O instruction has been obtained to verify the normalcy of the I/O bus 340 (step S 408 ). If there is a failure, the failure can be located and the unit concerned with the failure is found out on this occasion.
Following the operation of step S 408 , the I/O driver means 302 installs the SCSI controller 310 in the system (step S 409 ), and notifies the I/O controller management means 301 of the operation result.
The I/O controller management means 301 judges whether or not the installation operation has been normally performed (step S 410 ).
If the installation operation has been normally performed (step S 410 /YES), the I/O controller management means 301 sets the SCSI controller 310 in an installed mode (step S 411 ). On the other hand, if a failure is found at step S 408 , or the installation operation has not been normally performed (step S 410 /NO), the I/O controller management means 301 indicates an error message to notify the system maintainer that maintenance is required for the SCSI controller 310 (step S 412 ).
In accordance with the second embodiment of the present invention, the normalcy of the I/O bus is verified when installing the SCSI controller as is described above. Consequently, it is possible to detect an I/O bus failure as well as checking address parity in advance of the installation of the SCSI controller, thereby preventing a failure from occurring after the installation. Thus, the reliability of the system can be improved.
Moreover, a pseudo-I/O instruction is intentionally conducted so as to let I/O bus failure occur if any and to know the unit concerned with the failure. Thus, the unit that may have the failure can be specified when installing units in slave/master relationships (e.g. SCSI controller and disk storage units).
Besides, with the conventional system that does not verify the normalcy of the I/O bus, in the case where a SCSI controller failure is detected when a disk storage unit #B is additionally installed in the active system in which the SCSI controller and a disk storage unit #A have been already installed, failure recovery is performed for the SCSI controller even when the disk storage unit #A is in use. Consequently, accessing to the disk storage unit #A is interrupted, which affects a software or program running on the system. However, according to the present invention, it is possible to avoid such inconvenience since the SCSI controller failure is detected when installed.
While the present invention has been described with reference to the particular illustrative embodiments, it is not to be restricted by the embodiments but only by the appended claims. It is to be appreciated that those skilled in the art can change or modify the embodiment without departing from the scope and spirit of the present invention.
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A failure detection method enabling the detection of I/O bus failure and address parity error when installing I/O controllers connected to a system bus in a computer system, and also enabling failure location when installing units in slave/master relationships (e.g. SCSI controller and disk storage units) and when installing an additional slave in a computer system, thus improving the reliability of the system. The failure detection method comprises the steps of executing an instruction which involves providing I/O bus access to a memory to be used by an I/O controller after installed, determining that there is no failure when predetermined results are obtained with the instruction, and installing the I/O controller in the system. When the I/O controller has slave/master relationships with a plurality of slave units, the failure detection method further comprises the steps of detecting a failure in the slave units on the occasion of the installation, and notifying the host processor of the slave unit having the failure.
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RELATED PATENT APPLICATIONS
[0001] This application claims priority to U.S. provisional patent applications Ser. No. 60/676,181 filed 29 Apr. 2005, entitled “Harmonic Linear Actuator” and Ser. No. 60/691,144 filed 16 Jun. 2005, entitled “Harmonic Linear Actuator and Flexing Splined Interlock for Harmonic Motor or Linear Actuator.”
TECHNICAL FIELD
[0002] The present invention relates to electro-mechanical actuators, and particularly to linear actuators. More particularly still, the present invention relates to the application of harmonic drives as linear actuators and the adaptation thereof for automotive applications.
BACKGROUND OF THE INVENTION
[0003] Harmonic drives have been used as motors and actuators in many electro-mechanical applications. One type of harmonic motor has a rotatable rotor and a surrounding non-rotatable stator. The rotor makes a single point of contact with the inner circumference of the stator. The single point of contact rotates around (i.e. rolls around) the inner circumference of the stator. The rotor rotates a few degrees about its longitudinal axis for each complete rotation of the single point of contact about the inner circumference of the stator. In one modification, the outer circumference of the rotor and the inner circumference of the stator have gear teeth. Such motors find use in high torque, low speed motor applications.
[0004] In one known variation, the rotatable rotor is above a non-rotatable stator, the rotatable rotor flexes or wobbles downward to make a single point of contact with the stator, the single point of contact rotates around an “inner circumference” of the stator, and the rotor rotates a few degrees about its longitudinal axis for each complete rotation of the single point of contact.
[0005] In another type of harmonic motor, a shaft is surrounded by a shaft driving member which is brought into a single point of contact with the shaft by electro-restrictive devices, wherein the rotor rotates a few degrees for each complete rotation of the single point of contact around the inner circumference of the shaft driving member.
[0006] Harmonic drive gear trains are known. In one known design, a motor rotates a “wave generator” which is an egg-shaped member, which flexes diametrically opposite portions of the surrounding flex-spline gear, which is inside an inner gear. As the diametrically opposite teeth of the flex-spline gear contact the teeth of the outer gear, the rotatable one of the gears rotates with respect to the non-rotatable one of the gears.
[0007] U.S. Pat. No. 6,664,711 to T. Baudendistel describes a harmonic motor which includes a first annular member, a second member, and a device for flexing the first annular member. One of the members is rotatable about the motor's longitudinal axis, and the other member is non-rotatable. The flexing device flexes the first annual member into at least two spaced-apart points of contact with the second member, and sequentially flexes the first annular member to rotate the at least two spaced-apart points of contact about the longitudinal axis which rotates the rotatable one of the members about the longitudinal axis.
[0008] By using at least two points of contact between the members, the rotatable one (i.e., the rotor) is being driven by at least two points of contact by the non-rotatable one (i.e. the stator or rotor driving member). Driving the motor with at least two points of contact provides a more robust and more smoothly operating motor than is otherwise provided by the prior art.
[0009] In certain applications, linear actuators are preferred to motors. For example, a brake system for a motor vehicle, and in particular an automotive vehicle, functionally reduces the speed of the vehicle or maintains the vehicle in a rest position. Various types of brake systems are commonly used in automotive vehicles, including hydraulic, anti-lock or “ABS”, and electric or “brake by wire”. For example, in a hydraulic brake system, the hydraulic fluid transfers energy from a brake pedal to a brake pad for slowing down or stopping rotation of the wheel of the vehicle. Electronic systems control the hydraulic fluid in the hydraulic brake system. In the electric brake system, the hydraulic fluid is eliminated. Instead, the application and release of the brake pad is controlled by an electric caliper.
[0010] Generally, the electric caliper includes a motor and a gear system. Typically, either a few large gears or many small gears for the gear system are needed to achieve the necessary load transfer. Also, the geometry of the motor influences its efficiency, since the preferred shape is long and thin. However, there is a limited amount of space available in the wheel for packaging the type of gears and motor necessary to obtain the same load transfer as in the hydraulic brake system. Therefore, space limitations constrain the use of an electric caliper in an automotive vehicle.
[0011] U.S. Pat. No. 6,626,270 to D. Drenner et al. describes a brake caliper which includes an electric motor having a shaft and an associated gear system including first and second planetary gears rotatable engaged with the motor shaft. At least one of the planetary gears is engaged with the shaft and a piston, and is operatively engaged with a first carrier. The other planetary gear is operatively engaged with the first stage carrier and a second carrier. A ball screw is engaged with the second stage carrier for rotation therewith, and a ball screw nut is operatively engaged with the ball screw.
[0012] Although having many advantages to mechanical brake systems, more recent prior art systems based upon hydraulic pressure behind a piston or, alternatively, an electric motor employed to turn a ballscrew to move a piston to create clamping force in a brake caliper also have drawbacks. Hydraulic brake systems employ a closed hydraulic system filled with hydraulic fluid to control the piston. This approach, although currently common in the industry, can present adverse environmental, assembly, control and safety aspects. Likewise, the electro-mechanical system approach employs multiple parts, which have certain inefficiencies, namely a motor, planetary gear set and ballscrew. These components, in addition to being expensive and difficult to assemble and maintain, also can have the disadvantage of high inertia and back-drivability resistance.
[0013] It is, therefore, a primary object of the present invention to provide an improved harmonic drive configured as a linear actuator suitable for automotive brake caliper applications in brake by wire systems, which overcomes known shortfalls of existing devices without adding to part count, manufacturing complexity, cost or reduced robustness.
SUMMARY OF THE INVENTION
[0014] Generally, the present invention fulfills the forgoing needs by providing, in one aspect thereof, a robust, compact harmonic drive linear actuator, suitable for application as a piston in the brake caliper assembly of an automotive brake by wire system. The linear actuator provides the benefits of having high force output with virtually no inertia and zero back-drivability while decreasing the component count, weight and cost in a compact, easily packagable and robust design.
[0015] The presently inventive harmonic drive actuator includes a first annular member defining a longitudinal axis which lies on a plane perpendicular to the longitudinal axis, and wherein the first annular member is relatively flexible along a direction which lies in the plane. A second member is substantially coaxially aligned with the first member and also lies on the plane. The first and second members define opposed substantially cylindrical surfaces, which are fixed for non-relative rotation about the longitudinal axis. Finally, means are provided for flexing the first annular member into at least two spaced-apart points of contact between the surfaces and for sequentially flexing the first annular member to rotate the at least two points of contact circumferentially about the longitudinal axis. The surfaces define cooperating thread-forms thereon which selectively engage to effect relative axial displacement between the first and second members in response to sequential flexure of the first annual member. This arrangement provides a high force, low cost, simple linear actuator, which is compact and easily packaged within the envelope of a traditional automotive brake caliper.
[0016] According to another aspect of the invention, the second member is relatively rigid and lies on the plane perpendicular to the longitudinal axis. This allows the cylindrical surface defined by the second member to be formed by a structural member to facilitate packaging of the linear actuator.
[0017] According to another aspect of the invention, the linear actuator further includes means to limit axial displacement of one of the annular members with respect to an adjacent grounded member. Furthermore, the other annular member defined means for urging a load in at least one direction parallel to the longitudinal axis. This feature further enhances adaptability and packaging of the inventive harmonic drive actuator.
[0018] According to still another aspect of the invention, the means for flexing the first annular member is operable to effect selective bi-directional relative longitudinal displacement between the first and second annular members. This enhances operating speed and ensures against inadvertent lock-up of an associated brake system.
[0019] According to yet another aspect of the invention, the second annular member defines a rigid, generally cup-shaped member, and the first annular member as well as the means for flexing the first annular member are disposed substantially within the second annular member. This arrangement enhances robustness by protecting the moving parts as well as miniaturization of the linear actuator.
[0020] According to still yet another aspect of the invention, the means for flexing the first annular member is responsive to an electrical control signal, and is operative to effect radial disengagement of the thread-forms in response to the absence of the control signal, whereby the first and second members are freely axially displaceable with respect to one another. This arrangement has the advantage of providing a “fail silent” operation whenever the actuator is not energized, eliminating many adverse potential failure modes.
[0021] Application of the invention is particularly advantageous for use in brake caliper assemblies for passenger vehicles. Such an apparatus comprises a brake caliper for applying a clamp load along an actuation axis, a piston slidably disposed in a bore concentric with the axis for applying the clamp load, and a harmonic drive linear actuator disposed for acting upon the piston and an opposed substantially grounded caliper surface. Preferably, elements of the linear actuator are conjoined with the piston. This arrangement provides a robust, high force compact brake actuator.
[0022] These and other features and advantages of this invention will become apparent upon reading the following specification, which, along with the drawings, describes preferred and alternative embodiments of the invention in detail.
BRIEF DESCRIPTION OF THE DRAWINGS
[0023] The present invention will now be described, by way of example, with reference to the accompanying drawings, in which:
[0024] FIG. 1 , is a broken, sectional view of the preferred embodiment of a harmonic drive linear actuator employed within a brake by wire system of an automotive vehicle;
[0025] FIG. 2 , is a cross-sectional view of the harmonic drive linear actuator of FIG. 1 , on an enlarged scale;
[0026] FIG. 3 , is a cross-sectional view taken on lines 3 - 3 of FIG. 2 ;
[0027] FIG. 4 , is a cross-sectional view taken on lines 4 - 4 of FIG. 2 ; and
[0028] FIG. 5 , is a cross-sectional view similar to that of FIG. 4 , but where the harmonic drive linear is de-activated.
[0029] Although the drawings represent embodiments of the present invention, the drawings are not necessarily to scale and certain features may be exaggerated in order to illustrate and explain the present invention. The exemplification set forth herein illustrates an embodiment of the invention, in one form, and such exemplifications are not to be construed as limiting the scope of the invention in any manner.
DESCRIPTION OF THE PREFERRED EMBODIMENT
[0030] The present invention is intended for application in varied automotive vehicle applications and will be described in that context. It is to be understood, however, that the present invention could also be successfully applied in many other applications. Accordingly, the claims herein should not be deemed limited to the specifics of the preferred embodiment of the invention described hereunder.
[0031] Referring to FIG. 1 , a preferred environment and application of the present invention within the brake system of a passenger vehicle is illustrated. A brake caliper apparatus 10 may include mounting means (not illustrated) for grounding or securing the caliper apparatus 10 to the chassis of a motor vehicle in a manner well known in the art. The caliper apparatus 10 consists of a one-piece cast iron body 12 having an actuator housing portion 14 and an integral brake pad positioning/support portion 16 . In application, the body 12 is disposed adjacent the radially outermost portions of a brake disc 18 which is mounted for rotation with an associated vehicle wheel (not illustrated).
[0032] Caliper apparatus 10 supports and positions opposed outer and inner brake pads 20 and 22 , respectively, which are positioned to straddle and selectively engage outer and inner surfaces 24 and 26 , respectively, of brake disc 18 . Outer brake pad 20 is mounted on a rightwardly facing thrust surface 28 of support portion 16 and inner brake pad 22 is mounted on a leftwardly facing thrust surface 30 of a piston 32 . Piston 32 is slip fit within a blind bore 34 formed within housing portion 16 of body 12 , opening leftwardly toward brake disc 18 .
[0033] As will be described in detail herein below, a harmonic drive linear actuator 36 is disposed within bore 34 and is operable to displace the piston 32 and inner brake pad 22 bi-directionally along a longitudinal axis designated A-A. As illustrated in FIG. 1 , brake caliper apparatus 10 is in a released or non-braking condition, wherein the brake pads 20 and 22 are axially displaced a small distance from surfaces 24 and 26 of brake disc 18 . In this condition, brake disc 18 is free to rotate about its axis of rotation (not illustrated), which is substantially parallel to actuation axis A-A.
[0034] When braking of a host vehicle is desired, a vehicle braking control system 38 applies a control signal via a line 40 to provide electrical power to linear actuator 36 . Linear actuator 36 then drives the piston 32 and brake pad 22 leftwardly along axis A-A, causing brake pads 20 and 22 to apply opposed clamping forces upon surfaces 24 and 26 , respectively, of brake disc 18 . The amount of force applied by the linear actuator 36 will translate through thrust surfaces 28 and 30 to control the frictional braking forces applied to the brake disc 18 by the brake pads 20 and 22 .
[0035] Blind bore 34 is defined by a cylindrical wall surface 42 which is concentric with axis A-A, and an end wall surface 44 which is normal to axis A-A. Piston 30 is generally cylindrical in shape and dimensioned for a precise slip-fit within bore 34 . Due to the harsh environment in which the present invention is applied, it is contemplated that a flexible seal will be provided between the piston 32 and the housing portion 14 to prevent the ingress of brake system related debris, environmental contamination or moisture.
[0036] Referring to FIGS. 1 and 2 , piston 32 and linear actuator 36 are integrally formed as a single subassembly, which, in the preferred application, is substantially entirely disposed within bore 34 of body 12 of caliper system 10 . Piston 32 is generally cup-shaped, comprising a cylindrical head portion 46 and a circumferential skirt portion 48 integrally formed therewith. The outer surface of head portion 46 forms thrust surface 30 . A keyway 50 is formed in the outer surface of skirt portion 48 , which extends the entire axial length thereof. Keyway 50 mates with a radially inwardly directed guide ridge 52 formed in wall surface 42 of bore 34 . Keyway 50 and guide ridge 52 cooperate to prevent relative rotation and limit piston 32 to axial displacement within bore 34 .
[0037] The inner surfaces of head portion 46 and skirt portion 48 of piston 32 define a rightwardly opening cylindrical cavity 54 . The inner surface 56 of skirt portion is formed as a succession of concentric, equally dimensioned V-grooves 58 , which are flat walled, and form an overall “sawtooth” configuration with a constant trough-to-trough axial dimension designated “X”. Collectively, the V-grooves are designated as a thread-form with zero pitch. The inner surface 60 of head portion 46 establishes an axial limit of travel for linear actuator 36 as will be described herein below. The entire piston 32 is constructed of machined steel or other suitable material producing a robust, substantially rigid structure.
[0038] Referring to FIGS. 2-4 , the structure and operation of linear actuator 36 are illustrated. In addition to the skirt portion 48 of piston 32 , the linear actuator 36 includes an electromagnetic actuator assembly 62 and a flexible annular member 64 disposed generally concentrically within cavity 54 of piston 32 . Electromagnetic actuator assembly 62 includes an armature body 66 fixedly mounted to a splined end of an axially elongated support member 68 . The opposite end of support member 68 is affixed to a base plate 70 . Base plate 70 is disc-shaped having an outer circumferential surface 72 dimensioned similarly to piston skirt portion 48 for slip-fit within bore 34 of brake caliper 10 ( FIG. 1 ). In application, the large leading (right-hand as viewed in FIG. 2 ) surface 74 of base plate 70 abuts end wall surface 44 of caliper bore 34 to distribute braking forces and to maintain precise axial alignment of linear actuator 36 within bore 34 . A keyway 76 is formed in circumferential surface 72 , which registers with guide ridge 52 . Thus configured, electromagnetic actuator assembly 62 , including support member 68 and base plate 70 , is grounded or fixed from relative rotation with respect to the brake caliper 10 .
[0039] Armature body 66 is generally spool-shaped, including integral leading and trailing radially outwardly extending flange portions 78 and 80 , respectively, and a reduced diameter central body portion 82 . A plurality of electrical coils or windings 84 are insulatively disposed within central body portion 82 and are each electrically in-circuit with control system 38 via lines 40 ( FIG. 1 ) to define a discrete number of circumferentially arranged poles.
[0040] Flexible annular member 64 is an open-ended cylinder, which is carried by actuator assembly 62 . Annular member 64 is a bonded composite of a thick-walled inner ring 86 formed of relatively flexible material, and a relatively thin-walled outer ring 88 having ferro-magnetic properties. Annular member 64 is dimensioned whereby its effective inner diameter is somewhat greater than that of the central body portion 82 of armature body 66 , but somewhat lesser than the effective outer diameter of flange portions 78 and 80 . Annual member is axially straddled by flange portions 78 and 80 and has an axial dimension to establish a slip-fit there between. Thus configured, annular member is captured and carried by electromagnetic actuator assembly 62 , having no relative freedom of travel in either axial direction and limited relative radial freedom of travel.
[0041] Referring to FIGS. 1 and 2 , the outer ring 88 of flexible annular member 64 has an outer surface 90 in which is defined a thread-form 92 . Thread-form 92 is illustrated as a dual helix with a constant trough-to-trough dimension designated “X”. Thus, the pitch of thread-form 92 will result in a relative axial displacement between piston 32 and flexible annular member 64 of “2X” in single 360° point of contact rotation. It is contemplated, however, that differing combinations of thread-forms 58 and 92 can be applied depending upon such variables as clamping force requirements, actuation speed, range of axial displacement, overall diameter of the piston, and the like, as will be apparent to one skilled in the art in light of the present specification.
[0042] As best viewed in FIG. 5 where annular member 64 is in a relaxed position, i.e. when none of the electrical coils 84 are electrically energized, member 64 assures a substantially round configuration. Insodoing, a radial space 94 is established between the radially innermost portion of V-grooves/thread-form 58 of surface 56 of skirt portion 48 and the radially outermost portion of thread-form 92 of outer surface 90 of annular member 60 . In this condition, the flexible annular member 64 and electromagnetic actuator assembly is entirely mechanically de-coupled from the piston 32 , and the piston is free for unrestrained axial movement within bore 34 of brake caliper 10 . This releases any brake clamping forces the caliper assembly may have been applying upon the brake disc.
[0043] Keyways 50 and 76 are continuously engaged with guide ridge 52 independent of their respective axial position within bore 34 of brake caliper. Thus, they are mutually rotatively fixed.
[0044] The outer circumferential surface of the central body portion 82 of armature body 66 defines a plurality of axially elongated, radially outwardly directed tapered cogs 96 integrally formed therewith. Likewise, the inner circumferential surface of inner ring 86 of flexible annular member 64 defines a plurality of axially elongated, radially inwardly directed tapered cogs 98 integrally formed therewith. The cogs 96 and 98 are complimentarially shaped and circumferentially distributed and interdigitated, as best illustrated in FIG. 5 . The cogs prevent relative rotation between electromagnetic actuator assembly 62 and flexible annular member 64 , while permitting the limited radial displacement there between as described herein above. The axial end surfaces of the cogs 96 and 98 also increase the effective surface area for transferring linear actuator generated axial clamping forces between the electromagnetic actuator assembly 62 and the flexible annular member 64 .
[0045] Referring to FIGS. 2-4 , the harmonic drive linear actuator functions by selectively energizing opposed coil pairs within actuator assembly 62 . For example, if an opposed pair of coils 84 a and 84 b are energized, they create a magnetic field which attracts nearby portions of the flexible annular member 64 , causing it to distend from the relaxed condition depicted in FIG. 5 into the elongated or egg-shaped configuration of FIG. 4 . In FIG. 4 , the portions of the flexible member 64 are drawn radially inwardly into intimate contact with the outer peripheral surface of central body portion 82 of armature body 66 and are rotatively locked together by the engagement of cooperating cogs 96 and 98 . Simultaneously, opposed (by 90°) portions of the flexible member 64 are deformed radially outwardly into intimate contact with inner surface 56 of skirt portion 48 of piston 32 . This engagement can be supplemented by magnetic repulsion of adjacent reverse polarized coils 84 c and 84 d.
[0046] When flexible annular member 64 is distended as illustrated in FIGS. 1-4 , opposed segments of the tread-form 92 momentarily engage adjacent segments of V-grooves/thread-form 58 to axially lock the flexible annular member 64 with the skirt portion 48 . The areas of engagement are depicted in FIG. 3 as opposed arcuate segments 100 . Whenever the coils 84 are de-energized, the flexible member 64 returns to the configuration depicted in FIG. 5 due to the resiliency of its construction.
[0047] The electrical control of harmonic motors and actuators is well known. For example, U.S. Pat. No. 6,664,711 B2 and U.S. Patent Application 2005/0253675 A1 describe harmonic motors and electrical controllers therefore which can be adopted for use with the present invention. U.S. Pat. No. 6,664,711 B2 and U.S. 2005/0253675 A1 are hereby incorporated herein by reference as an exemplary teaching of one possible approach. It is to be understood that they reflect only one of many possible control strategies. Furthermore, other methodologies for sequentially flexing the flexing member such as mechanical, electrical or electromagnetic could be implemented without departing from the spirit of the invention.
[0048] In summary, the piston 32 and linear actuator are locked together for relative non-rotation. When the electrical coils 84 are sequentially energized, the localized opposed areas of contact of the opposed thread-forms “walks around” the circumference of the linear actuator 36 , and thereby axially advancing or retracting the piston 32 with respect to the brake caliper body 10 . The inventive linear actuator therefore has very low inertia, excellent back-drivability, a lowered part count (compared to a ball-screw approach) for reliable operation and high linear force output.
[0049] The only inertia in the device is in the internal actuator employer for flexing or deforming the “flex-tube”. Preferably, this is accomplished electro-magnetically, to virtually eliminate related moving parts. This allows almost instantaneous direction reversal of the linear actuator 36 . The zero back-driveability is achieved by effecting disengagement of the piston 32 with the actuator 36 whenever power is lost, thereby allowing the piston to float.
[0050] The structure of the present invention is extremely simple, including only an actuator, a flex-tube and a piston.
[0051] The linear displacement of the actuator is effectively one thread width per revolution. The gain of the actuator can be changed simply by changing the pitch or lead angle of one or both of the thread-forms 58 and 92 .
[0052] As an analogy, the present invention operates as a “nut” and “bolt”, with the exception that they are in contact in only a limited number of opposing points. The flexible annular member 64 serves as an out-of-round “nut” which preferably contacts the mating “bolt” in only two points, which are 180° apart. The load capacity or limit is effectively reduced as a result of the reduced surface contact area between the “bolt” and out-of-round “nut”. However, this can be accommodated by thickening the “nut” in its axial dimension, i.e. increasing the number of threads and thus the number of thread segments which are engaged with the “bolt” at any given time. As a next step, the threads of the out-of-round “nut are cut as a succession of concentric grooves which are perpendicular to the axis. Assuming that the lead angle and contact circumference is compatible, if the “nut” is turned, the same axial displacement will occur. Finally, instead of spinning the “nut”, the “nut” is held stationary and deformed by changing the minor axis of orientation. In other words, the “nut” is sequentially squeezed, first at a 12 o'clock orientation, then a 1 o'clock orientation, then a 2 o'clock orientation, and so on. Because the “nut” cannot move axially or linearly, the “bolt” will be displaced axially, but without relative rotation.
[0053] It is to be understood that the invention has been described with reference to specific embodiments and variations to provide the features and advantages previously described and that the embodiments are susceptible of modification as will be apparent to those skilled in the art.
[0054] Furthermore, it is contemplated that many alternative, common inexpensive materials can be employed to construct the basic constituent components. Accordingly, the forgoing is not to be construed in a limiting sense.
[0055] The invention has been described in an illustrative manner, and it is to be understood that the terminology, which has been used is intended to be in the nature of words of description rather than of limitation.
[0056] Obviously, many modifications and variations of the present invention are possible in light of the above teachings. For example, mechanical, hydraulic or other prime movers can be employed to affect the sequenced flexure of the first annular member. It is, therefore, to be understood that within the scope of the appended claims, wherein reference numerals are merely for illustrative purposes and convenience and are not in any way limiting, the invention, which is defined by the following claims as interpreted according to the principles of patent law, including the Doctrine of Equivalents, may be practiced otherwise than is specifically described.
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A harmonic drive linear actuator includes a first annular member defining a longitudinal axis and lying on a plane, which is perpendicular to the longitudinal axis. The first member is relatively flexible along a direction parallel to the plane. A second member is substantially coaxially aligned with the first member to define opposed substantially cylindrical surfaces and are fixed for non-relative rotation about the longitudinal axis. An actuator is provided for flexing the first annular member into at least two spaced-apart points of contact between the opposed surfaces and for sequentially flexing the first member to rotate the at least two points of contact circumferentially about the axis. The first and second surfaces define cooperating thread-forms thereon, which selectively engage to effect controlled, bidirectional relative axial displacement between the members in response to sequential flexure of the first member. The linear actuator can be conjoined with an actuator piston of a vehicle brake caliper assembly.
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CROSS REFERENCE TO RELATED APPLICATION
[0001] This application is a continuation of International Application No. PCT/EP2006/060903, filed Mar. 21, 2006, which is incorporated by reference as if fully set forth.
FIELD OF INVENTION
[0002] The invention relates to a heat shield for the local separation of a flow channel within a turbine engine, in particular a gas turbine plant, with respect to a stator housing radially surrounding the flow channel, with two axially opposite joining contours which each can be brought into engagement with two components which are axially adjacent along the flow channel and which each provide a complementary reception contour for the joining contours, of which reception contours at least one reception contour has an axial clearance, along which the joining contour joined in it is mounted axially displaceably, at least one seal being provided between the axially displaceable joining contour and the reception contour.
BACKGROUND
[0003] Heat shields of the generic type designated above are part of axial-throughflow turbine engines, through which gaseous working media flow for compression or controlled expansion and, because of their high process temperatures, those plant components which are acted upon directly by the hot working media are subject to high thermal loads. Particularly in the turbine stages of gas turbine plants, the rotating blades and guide vanes, arranged axially one behind the other in rotating blade and guide vane rows, are acted upon directly by the hot combustion gases occurring in the combustion chamber. In order to prevent the situation where the hot gases flowing through the flow channel subject to thermal load those regions within the turbine engine which are provided in stator regions facing away from the flow channel, heat shields, as they are known, which are provided on the stator side in each case between two guide vane rows arranged axially adjacently to one another, ensure as gastight a bridge-like sealing as possible between two guide vane rows arranged axially adjacently. Correspondingly designed heat shields may also be provided along the rotor unit, which are in each case mounted on the rotor side between two axially adjacent rotating blade rows, in order to protect corotating rotor components from the introduction of an excessive amount of heat.
[0004] Although the following statements refer solely to heat shields which are arranged between two guide vane rows and to that extent can separate and correspondingly protect the stator-side housing and the components connected to it with respect to the heat-loaded flow channel, it is also conceivable to provide the following measures on a heat shield which serves for protecting corotating rotor components and which can be introduced between two rotating blade rows arranged axially adjacently to one another.
[0005] FIG. 2 a illustrates a diagrammatic longitudinal section through a gas turbine stage, into the flow channel of which project radially from outside guide vanes 1 connected to a stator housing S, the special configuration of which has no further significance in what follows.
[0006] A rotating blade 2 , connected to a rotor unit, not illustrated, projects between two guide vanes 1 arranged adjacently in guide vane rows and is spaced apart radially on the end face with respect to a heat shield 3 which with the guide vane 2 encloses as small a free intermediate gap 4 as possible, in order as far as possible to avoid leakage losses of flow fractions of the hot gas stream through the intermediate gap 4 . For this purpose, the rotating blade tip has sealing structures 5 which are arranged so as to rotate freely with respect to what are known as abrasion elements 6 .
[0007] In order to avoid the situation where hot combustion gases in the region of the heat shield 3 , which in a bridge-like manner spans the interspace between two guide vanes 1 , 1 ′ arranged axially adjacently to one another, may penetrate into that region of the heat shield 3 which faces radially away from the flow channel, the heat shield 3 provides two axially opposite joining contours 7 , 8 which extend axially into corresponding reception contours 9 , 10 within the guide vane roots.
[0008] The reception contour 9 corresponds to a groove-shaped recess which is designed to be complementary with an exact fit to the joining contour 7 and which is incorporated in the root region of the guide vane 1 . The axially opposite joining contour 8 of the heat shield 3 is likewise inserted into a reception contour 10 which is designed to be correspondingly complementary to the outer contour of the joining contour 8 and which is introduced in the root region of the guide vane 1 ′. However, the reception contour 10 has an axial clearance 11 , so that the joining contour 8 is mounted axially slideably in the event of a corresponding operationally induced thermal expansion of the heat shield 3 .
[0009] For the fluidtight sealing of the heat shield 3 with respect to the respective reception contours 9 , 10 in the root regions of the guide vanes 1 , 1 ′, seals 12 , 13 are provided between the joining contours 7 , 8 and the associated reception contours 9 , 10 . The seals 12 , 13 are located each in a groove-shaped recess 14 within the joining contours 7 , 8 (see also the illustration of a detail according to FIG. 2 b of the joining region between the joining contour 8 and the reception contour 10 ). The seals 12 , 13 are preferably manufactured from an elastic sealing material in the form of a round bar, project partially beyond the radially outer boundary surface 16 and fit flush, at least along a joining line, against the surface region 17 of the reception contour 10 .
[0010] As a result of the sealing action of the seals 12 , 13 , it is possible, on the one hand, to avoid the situation where hot gases from the flow channel penetrate into the regions facing radially away from the flow channel, to the heat shield 3 , and the situation is likewise prevented where cooling air L fed in on the stator side may pass through corresponding leakage points into the flow channel. As already explained initially, the clearance 11 provided in the recess 10 serves for a thermally induced material expansion along the heat shield 3 , with the result that the joining contour 8 , together with the seal 12 provided in it, is displaced into a position on the right, evident in the illustration. When, by contrast, the gas turbine stage is shut down and the individual components cool down, the joining contour 8 , together with the seal 12 provided in it, returns to the original initial position. It is obvious that, due to the thermally induced relative movements between the reception contour 8 and the surface region 17 , the seal 12 is subject to material abrasion phenomena which, when a maximum permissible tolerance limit is exceeded, lead to a wear-induced reduction in the sealing function of the seal, so that cooling air L can escape through the intermediate gaps which occur or are already present between the joining contour 8 and reception contour 10 . This not only leads to a considerable loss of cooling air, with the result that the cooling action is drastically reduced, but there is also the risk that hot gases may also enter regions which face away from the flow channel with respect to the heat shield 3 . In addition, usually seal are used which consist of a fabric material which may be thinned out under excessive mechanical frictional stress, with the result that the sealing action of the seal decreases with increasing operating time.
SUMMARY
[0011] The object on which the invention is based is to provide a heat shield for the location separation of a flow channel within a turbine engine, in particular a gas turbine plant, with respect to a stator housing radially surrounding the flow channel, with two axially opposite joining contours which can each be brought into engagement with two components which are axially adjacent along the flow channel and which each provide a complementary reception contour for the joining contours, of which reception contours at least one reception contour has an axial clearance, along which the joining contour joined in it is mounted axially displaceably, at least one seal being provided between the axially displaceable joining contour and the reception contour, in such a way that the seal is to reduce or considerably lower abrasion caused by relative movements between the joining contour and the reception contour which are brought about by the thermally induced material expansions and shrinkages.
[0012] In particular, it is appropriate to take measures which considerably reduce the wear of the seals, although the measures to be taken here are to be executable as simply as possible in structural terms. Finally, it is appropriate decisively to prolong the maintenance cycles of the maintenance-subject components on the heat shield, thus with particular regard to the seals, and to improve their operating reliability.
[0013] The present invention is a heat shield arrangement for local separation of a flow channel within a turbine engine, with respect to a stator housing radially surrounding the flow channel. The heat shield includes two axially opposite joining contours which are each engageable with two components which are axially adjacent along the flow channel. Each provides a complementary reception contour for the joining contours. At least one of the reception contours has an axial clearance, in which the associated joining contour is axially displaceably mounted. At least one seal is provided between the axially displaceable joining contour and the reception contour. The seal is mounted movably within the reception contour or the joining contour in such a way that the seal is deflectable against a surface region of the reception contour or of the joining contour.
BRIEF DESCRIPTION OF THE DRAWINGS
[0014] The invention is described below by way of example, without any restriction of the general idea of the invention, by means of exemplary embodiments, with reference to the drawings in which:
[0015] FIG. 1 a shows a diagrammatic partial longitudinal sectional illustration through a joining region between a heat shield and an axially adjacent guide vane,
[0016] FIG. 1 b shows a perspective illustration of the sealing element with a spring element in a vertical projection above a recess within the joining contour,
[0017] FIGS. 2 a, b show a partial longitudinal sectional illustration through a heat shield with axially adjacent guide vanes and an illustration of a detail relating to this according to the prior art.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
Introduction to the Embodiments
[0018] According to the solution, a heat shield is designed, according to the features of the preamble of claim 1 , in such a way that the seal is mounted movably within the reception contour or the joining contour in such a way that the seal can be deflected by the action of force against a surface region of the reception contour or of the joining contour.
[0019] According to the present invention, the seal, which preferably consists of a metallic material, preferably of an incompressible material, is introduced within a recess along the reception contour or joining contour, but is additionally deflected or pressed against a surface region of the reception contour or joining contour by the action of force, preferably by the action of spring force. The following considerations provide for integrating the seal into the joining contour of the heat shield, so that the seal is pressed by the action of spring force against a surface region of the reception contour. It is likewise also possible, however, to integrate the seal in a corresponding recess provided within the reception contour, so that the seal is pressed against a surface region of the joining contour. The choice of mounting of the seal will be governed by the respective structural conditions of the joining connection between the heat shield and the axially following component of the gas turbine plant. Without any restriction to the general idea of the invention, the seal design according to the invention will be described below as an integral constituent of the joining contour of the heat shield. In this regard, reference is made to the exemplary embodiment described in the Figures.
DETAILED DESCRIPTION
[0020] FIG. 1 a shows a partial view of a longitudinal section through a heat shield 103 in the region of the joining contour 108 which issues into a corresponding groove-shaped reception contour 110 of an axially adjacent root of a guide vane 101 ′. The axial depth of the reception contour 110 is dimensioned, in such a way that, in the case of a thermally induced material expansion of the heat shield 103 , the joining contour 108 is mounted slideably along the axially oriented clearance 111 . The joining contour 108 consequently executes a translational movement indicated by the direction of the arrow E′. In the exemplary embodiment illustrated in FIG. 1 a , the joining contour 108 has a radially outer joining face 116 in which a groove-shaped recess 114 is incorporated. The depth of the groove-shaped recess 114 , measured from the joining face 116 , corresponds at least to the maximum radial extent of the seal 112 , the shape of which is adapted to the inner contour of the groove-shaped recess 114 , so that the seal 112 can be pushed completely into the recess 114 . Furthermore, within the groove-shaped recess 114 , a spring element 118 is provided which is introduced between the groove bottom of the recess 114 and the seal 112 , so that the spring element 118 can drive the seal 112 radially upward. For a supplementary overview of the design of the seal 112 , of the spring element 118 and of the groove-shaped recess 114 within the joining contour 108 , reference is made to the perspective illustration according to FIG. 1 b , which is to be considered below together with FIG. 1 a.
[0021] The seal 112 is designed in the form of a rod in the way illustrated in perspective in FIG. 1 b and is preferably manufactured from an incompressible metallic material which has essentially no abrasion properties. The seal 112 has centrally a rectangularly formed protrusion 119 which engages into a correspondingly rectangularly formed recess 120 in the inserted state within the groove-shaped recess 114 . The seal 112 is positively guided linearly in the radial direction by the protrusion 119 , so that the seal 112 is prevented from slipping out of place in the circumferential direction along the groove-shaped recess 114 . Between the seal 112 and the bottom of the groove-shaped recess 114 , a spring element 118 of curved form is introduced, which can press the seal 112 radially upward by the action of spring force. In order to prevent the spring element 118 from slipping out of place in the circumferential direction along the groove-shaped recess 114 , the curved spring element portion 118 ′ facing the groove bottom issues into a corresponding recess disposed in the groove bottom.
[0022] The boundary wall 121 , axially opposite the rectangularly formed recess 120 , within the groove-shaped recess 114 is manufactured from a sealing material and can thereby come into fluidtight contact with the seal 112 .
[0023] FIG. 1 a illustrates the inserted state of the joining contour 108 within the reception contour 110 , it being evident in the longitudinal sectional illustration illustrated that the spring element 118 presses the seal 112 radially outward against a surface region 117 of the reception contour 110 and therefore presses the heat shield 103 in a fluidtight manner against the reception contour 110 within the root of the guide vane 101 ′. In order to ensure that the seal 112 is pressed by the action of force both against the surface region 117 and at the rear against the boundary wall 121 , the radially lower side edge of the seal 112 is of obliquely inclined design, so that the spring element 118 can also press the seal 112 axially against the rear boundary face 121 in a fluidtight manner.
[0024] In order to improve the sealing action of the seal 112 against the surface region 117 of the reception contour 110 , the side edge of the seal which faces the surface region 117 is designed to be contour-true with respect to the surface region 117 .
[0025] Although the sealing system designed according to the present invention cannot avoid the axial longitudinal movements of the heat shield 103 caused by the thermal material expansion or shrinkage, nevertheless, with a suitable choice of the seal material, material abrasion becomes entirely irrelevant, especially since the seal 112 is selected from an incompressible wear-free preferably metallic material which ensures fluidtight sealing on account of the pressure caused by the action of spring force.
[0026] It is likewise conceivable to provide the seal arrangement acted upon by spring force alternatively in the region of the reception contour 110 , such as, for example, in the region of the boundary face, instead of within the joining contour 108 in the way indicated in FIGS. 1 a and 1 b.
[0027] Furthermore, the cooling air L′ flowing in under high pressure can exert a high pressure force on the axially directed face 123 of the protrusion 119 within the cooling volume V′ enclosed by the heat shield 103 , so that, in addition to the spring force component, the seal is pressed in the axial direction against the boundary side 121 consisting of sealing material.
[0028] In addition to the actual embodiment of the spring element 118 which is illustrated in FIGS. 1 a and 1 b , further spring element designs may also be envisaged, such as, for example, a multiplicity of individual helical spring elements helically shaped or coiled spring elements and suitably shaped flat springs.
[0029] Moreover, for the sake of completeness, it is pointed out that the heat shield illustrated in FIGS. 1 a and 1 b delimits in a ring-like multiple arrangement the entire circumferential region between two guide vane rows arranged adjacently to one another. For this purpose, two heat shields arranged adjacently to one another in the circumferential direction are in engagement via a common strip band seal 124 , by means of which a possible loss of cooling air along two heat shields contiguous to one another in the circumferential direction can be avoided.
[0030] The sealing arrangement according to the invention thus affords the following advantages:
[0031] The leaktightness of the cooling air volume which is separated from the flow channel by the heat shield is considerably improved by virtue of the wear-free seal, especially since the sealing action is ensured, despite thermal expansion and shrinkage phenomena, by the seal being pressed by the action of spring force against the respective surface region lying opposite the seal.
[0032] Regardless of predetermined tolerance dimensions in terms of the design of the reception contour or of the joining contour, the pressing of the seal caused by spring force ensures at any time a sealing of the joining region with respect to its radially upper and lower boundary faces, especially since the radially upper seal 112 , by virtue of the counterforce exerted on the joining region, can also press the radially lower boundary face of the joining region against the boundary face of the reception contour 110 in a fluidtight manner. Should the seal be provided in the region of the boundary face, the same applies accordingly.
[0033] Due to the pressing action of the seal 112 against the surface region 116 of the reception contour 110 by the action of spring force, the spring element 118 , because of its inherent elasticity, contributes to a certain capacity for the absorption of shocks or vibrations, so that mechanical vibrations occurring within the joining region can be absorbed by the spring element 118 and therefore do not subject the joining region to excessively high mechanical stress.
[0000]
LIST OF REFERENCE SYMBOLS
1, 1', 101'
Guide vane
2
Rotating blade
3, 103
Heat shield
4
Intermediate gap
5
Ribs
6
Abrasion elements
7, 8, 108
Joining contour
9, 10, 110
Reception contour
11, 111
Axial clearance
12, 13, 112
Seal
114
Groove-shaped recess
15
N/A
16, 116
Joining face
17, 117
Surface region
118
Spring element
118'
Part region of the spring element
119
Protrusion
120
Recess
121
Boundary face
123
Radial side face of the protrusion
124
Strip band seal
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A heat shield arrangement for local separation of a flow channel within a turbine engine, with respect to a stator housing radially surrounding the flow channel is provided. The heat shield includes two axially opposite joining contours which are each engageable with two components which are axially adjacent along the flow channel. Each provides a complementary reception contour for the joining contours. At least one of the reception contours has an axial clearance, in which the associated joining contour is axially displaceably mounted. At least one seal is provided between the axially displaceable joining contour and the reception contour. The seal is mounted movably within the reception contour or the joining contour in such a way that the seal is deflectable against a surface region of the reception contour or of the joining contour.
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TECHNICAL FIELD
This invention relates to a method of preparation of battery cells, and in particular to battery cells having a support layer to support the edges and corners of electrodes during packaging of the cells.
BACKGROUND OF THE INVENTION
Cells and batteries are energy storage devices well known in the art. Cells typically comprise electrodes and an ion conducting electrolyte therebetween. For example, the rechargeable lithium ion cell, known as a rocking chair type lithium ion battery, typically comprises essentially two electrodes, an anode and a cathode, and a non-aqueous lithium ion conducting electrolyte therebetween. The anode (negative electrode) is a carbonaceous electrode that is capable of intercalating lithium ions. The cathode (positive electrode), a lithium retentive electrode, is also capable of intercalating lithium ions. The carbon anode comprises any of the various types of carbon (e.g., graphite, coke, carbon fiber, etc.) which are capable of reversibly storing lithium species, and which are bonded to an electrochemically conductive current collector (e.g., copper foil) by means of a suitable organic binder (e.g., polyvinylidine fluoride, PVdF).
The cathode comprises such materials as transition metals and chalcogenides that are bonded to an electrochemically conducted current collector (e.g., aluminum foil) by a suitable organic binder. Chalcogenide compounds include oxides, sulfides, selenides, and tellurides of such metals as vanadium, titanium, chromium, copper, molybdenum, niobium, iron, nickel, cobalt, and manganese. Lithiated transition metal oxides are, at present, the preferred positive electrode intercalation compounds. Examples of suitable cathode materials include LiMnO 2 , LiCoO 2 , LiNiO 2 , and LiFePO 4 , their solid solutions and/or their combination with other metal oxides and dopant elements, e.g., titanium, magnesium, aluminum, boron, etc.
The electrolyte in such lithium ion cells comprises a lithium salt dissolved in a non-aqueous solvent which may be (1) completely liquid, (2) an immobilized liquid (e.g., gelled or entrapped in a polymer matrix), or (3) a pure polymer. Known polymer matrices for entrapping the electrolyte include polyacrylates, polyurethanes, polydialkylsiloxanes, polymethacrylates, polyphosphazenes, polyethers, polyvinylidine fluorides, polyolefins such as polypropylene and polyethylene, and polycarbonates, and may be polymerized in situ in the presence of the electrolyte to trap the electrolyte therein as the polymerization occurs. Known polymers for pure polymer electrolyte systems include polyethylene oxide (PEO), polymethylene-polyethylene oxide (MPEO), or polyphosphazenes (PPE). Known lithium salts for this purpose include, for example, LiPF 6 , LiClO 4 , LiSCN, LiAlCl 4 , LiBF 4 , LiN(CF 3 SO 2 ) 2 , LiCF 3 SO 3 , LiC(SO 2 CF 3 ) 3 , LiO 3 SCF 2 CF 3 , LiC 6 F 5 SO 3 , LiCF 3 CO 2 , LiAsF 6 , and LiSbF 6 . Known organic solvents for the lithium salts include, for example, alkyl carbonates (e.g., propylene carbonate and ethylene carbonate), dialkyl carbonates, cyclic ethers, cyclic esters, glymes, lactones, formates, esters, sulfones, nitrates, and oxazoladinones. The electrolyte is incorporated into pores in a separator layer between the anode and the cathode. The separator layer may be either a microporous polyolefin membrane or a polymeric material containing a suitable ceramic or ceramic/polymer material. Silica is a typical main component of this latter type of separator layer.
Lithium ion battery cells, as are most cells, are often made by adhering, e.g., by laminating, thin films of the anode, cathode, and the electrolyte/separator layers together wherein the electrolyte/separator layer is sandwiched between the anode and cathode layers to form an individual cell. A plurality of such cells are generally bundled together, in what is typically known as a cell stack or winding, and packaged to form a higher energy/voltage battery. Packaging of the cell or cell stack generally involves a vacuum seal lamination process requiring complex packaging equipment. During packaging, the pressures and forces are exerted upon the individual cell layers, which may cause vulnerable edges and corners of the electrode layers in each cell to be bent, crushed or otherwise damaged. This damage often decreases the overall life and power of the cell. Specifically, damage to the electrode films results in non-uniform utilization of the active materials, which in turn, can lead to lithium plating and loss of life. In addition, the pressure exerted on the electrode layers may cause the separator to split thereby posing possible risks of shorting within the battery.
Thus, there is a need to develop a cell construct and method of assembly to produce a more robust battery cell having longer life and increased activity, and which is less prone to developing shorts.
SUMMARY OF THE INVENTION
The present invention provides a robust battery cell, and in particular, a robust lithium ion battery cell, having long cell life and high activity with minimal risk of shorting. The battery cell comprises a support layer surrounding at least a portion of the outer edge, referred to as edge perimeter, of the smaller of the anode and cathode electrode layers and adjacent to the electrolyte/separator layer. The support layer provides support and strength primarily to the larger of the anode and cathode electrode layers as well as to the electrolyte/separator layer therebetween during vacuum sealing and exposure to other associated cell-packaging pressures. The support layer thus provides added rigidity and resistance to crushing during manufacture and packaging of the battery cell.
In an exemplary embodiment, the support layer may generally be in the shape of a frame having an edge perimeter and an open central portion. The support layer frame is positioned around the smaller electrode such that the smaller electrode lies within the open central portion allowing the edge perimeter of the support layer to provide support to the larger electrode, in particular the edges of the larger electrode, when the two electrodes are assembled and packaged together. The support layer may extend outwardly in the horizontal plane of the smaller electrode and beyond the edge perimeter of the larger electrode, but optimally the extension should be substantially equal to the edge perimeter of the larger electrode. The support layer of the present invention advantageously comprises polymers, including homopolymers, copolymers, or mixtures thereof.
The present invention also provides a method of preparing the battery cell including the support layer described above. The method comprises joining at least one anode, at least one cathode, at least one support layer positioned in surrounding relation to at least a portion of the smaller of the anode or cathode, and at least one electrode/separator layer sandwiched between the anode and cathode to form at least a single cell. Similarly, a plurality of single cells may be joined to form a battery. Multiple cells may be arranged as a cell stack or winding with support layers placed around each of the smaller of the anode or cathode in each cell. The anodes, cathodes, electrolyte/separator layers, and support layers in the cell stack may be sealed together to form the battery.
In constructing or assembling the cell, the support layer may be first placed adjacent to the surface of the electrolyte/separator layer followed by placement of the smaller electrode inside the open central portion of the support layer. Alternatively, the support layer may be placed around the smaller electrode prior to placement adjacent the separator layer. The smaller electrode, the support layer, the larger electrode and the electrolyte/separator layer are then joined to form a battery cell. Joining is typically accomplished by conventional packaging equipment, such as vacuum sealing or laminating equipment, to seal or enclose the cell or cell stack to form a battery. By virtue of the support layer, the edges of the larger electrode resist bending and crushing during the joining process.
BRIEF DESCRIPTION OF THE DRAWINGS
The present invention will now be described, by way of example, with reference to the accompanying drawings, in which:
FIG. 1 is an exploded view of a battery cell.
FIG. 2 is a cross-sectional view of a packaged battery cell.
FIG. 3 is an exploded view of a battery cell stack having two cells.
DETAILED DESCRIPTION
The invention is hereinafter described with general reference to a lithium ion battery cell, however, it may also be applied to other non-lithium ion conducting battery cells. As shown in FIG. 1 , an embodiment of a battery cell 10 comprises a first electrode 14 and a second electrode 22 separated by an electrolyte/separator layer 30 , referred to simply as separator layer 30 . Either of the first electrode 14 or the second electrode 22 may be an anode, with the other being a cathode in the cell 10 . The first electrode 14 has an outer edge or an edge perimeter 16 defining a surface area 15 . Similarly, the second electrode 22 has an edge perimeter 24 defining a surface area 23 . Surface area 23 is larger than surface area 15 . Thus, first electrode 14 is a smaller electrode than second electrode 22 . A support layer 18 having an edge perimeter 20 and an open central portion 9 is positioned around at least a portion of the first electrode 14 . Advantageously, the support layer 18 is positioned around the entire first electrode 14 . The open central portion 19 defines area which is generally equal to or larger than the surface area 15 of the first electrode 14 . Preferably, the area defined by central portion 19 can be substantially equal to surface area 15 to maximize support for the electrodes in the cell. In constructing the cell, edge perimeter 20 in positioned to surround the first electrode 14 generally in substantially the same plane in which first electrode 14 lies, whereby first electrode 14 occupies central portion 19 of support layer 18 . As shown in FIGS. 1 and 2 , first electrode 14 and second electrode 22 are assembled together with separator layer 30 therebetween to form cell 10 , which is di packaged with laminate material 11 a using laminating equipment to form seal 11 . Vacuum sealing is preferably used to form seal 11 . Support layer 18 provides beneficial support to the larger second electrode 22 during packaging of the cell 10 by adding strength and rigidity to the edges and corners of second electrode 22 , for example, to reduce or prevent the edges and corners from being bent or crushed under packaging pressures.
The edge perimeter 20 of support layer 18 generally determines the level of support provided to second electrode 22 . Edge perimeter 20 defines an area 21 which includes the area defined by open central portion 19 . Area 21 may be larger than the surface area 23 of second electrode 22 . In other words, the edge perimeter 20 of the support layer 18 may extend outwardly beyond the edges and corners of edge perimeter 24 of second electrode layer 22 . Alternatively, support layer 18 may have an area 21 substantially equal to the surface area 23 of larger second electrode 22 thereby having an edge perimeter 20 substantially equal to the edge perimeter 24 of the second electrode 22 to provide adequate support. Such a support layer 18 would absorb pressures, for example, including air pressure and vacuum pressure, exerted on cell 10 during packaging thereby relieving second electrode 22 from exposure to the total pressure of packaging. Such a relief in pressure coupled with the support provided to second electrode 22 to withstand packaging pressures significantly reduces or may even prevent bending or crushing the otherwise vulnerable corners and edges of second electrode 22 .
While support layer 18 is illustrated and described as a frame-like structure surrounding the entire first electrode 14 , the present invention is not so limited. Persons of ordinary skill in the art will readily understand that the benefits of the support layer 18 may be available in instances where the support layer 18 only surrounds a portion of the first electrode 14 . For example, the support layer 18 may be provided to support only two opposing edges of first electrode 14 leaving the other edges free. Advantageously, the support layer 18 will be provided for and surround at least those portions of the first electrode 14 which are vulnerable to pressures during packaging of the battery cell 10 .
The support layer 18 may be any material compatible for use in a battery cell 10 . Ideally, the support layer 18 may comprise a polymeric material. This polymeric material may be the same material used in the binder of either the first electrode 14 or the second electrode 22 , or it may be different. Examples of polymeric materials suitable for the present invention include but are not limited to, homopolymers, copolymers, or mixtures of polymers such as vinylidine fluoride, vinylidine chloride fluoride, vinylidine chloride, vinylchloride, acrylonitrile fluoroethylene, fluoropropylene, chlorofluoroethylene, chlorofluoropropylene, chloroethylene, chloropropylene, ethylene, propylene, vinylalcohol, glycol, acetate, ester, acrylate, carbonate, ethylene oxide, propylene oxide, acrylic acid modified olefins, maleic acid modified olefins, cellulose, nylon, urethane, terephthalate, and styrene.
As shown in FIGS. 1 and 2 , a separator layer 30 , which includes an electrolyte, is placed between the first electrode 14 and the second electrode 22 to provide a medium for cell activity and ultimate conduction of electricity. Separator layer 30 may be any size necessary for optimal cell activity. For example, the separator layer 30 shown in FIGS. 1 and 2 generally has a surface area 31 larger than surface areas 15 and 23 of first and second electrodes 14 and 22 , respectively. Alternatively, surface area 31 may be substantially equal to area 21 defined by edge perimeter 20 of support layer 18 or substantially equal to surface area 23 of second electrode 22 .
The first electrode 14 , second electrode 22 , and separator layer 30 , typically comprise polymeric materials. The first electrode 14 and the second electrode 22 generally include an organic binder containing the polymeric material. By way of example only, and not limitation, suitable polymeric materials include homopolymers, copolymers, or mixtures of polymers such as polyvinylidine fluoride, polyvinylidine chloride fluoride, polyvinylidine chloride, polyvinylchloride, polyvinylchloride acetates, polyacrylonitriles, polyfluoroethylenes, and polyolefins such as polypropylene and polyethylene, acrylic or maleic acid modified polyethylene or polypropylene, polyvinylalcohols, polyglycols, and the like. These materials may be obtained from commercial sources as is known to one skilled in the art.
Lithium ion and other non-lithium ion batteries may comprise a plurality of the individual cells 10 illustrated in FIG. 1 , each formed from individual small first and large second electrodes separated by a separator layer. The cells are generally arranged in a cell stack and packaged to from a battery. In such a battery, at least a portion of one or more of the first electrodes 14 , having a surface area 15 smaller than that of the counter second electrode 22 , may be surrounded by a support layer 18 . One embodiment of the present invention, shown in FIG. 3 , is a cell stack 12 containing two cells sharing a single small first electrode 14 . The first electrode 14 has opposing surfaces 14 a , 14 b and a first edge perimeter 16 defining a first surface area 15 . A support layer 18 defining an open central portion 19 and an edge perimeter 20 is placed in surrounding relation to the first electrode 14 . Two separator layers 30 and 32 are placed adjacent to and in contact with opposing surfaces 14 a , 14 b , respectively, of the first electrode 14 . The individual sizes and polymeric materials of the two separator layers 30 and 32 may be the same or different as determined by the user and generally depends upon the voltage requirements and cost of the battery. As shown in FIG. 3 , the surface area 33 of separator layer 32 is substantially equal to the surface area 31 of separator layer 30 . Adjacent to and contacting the surfaces 30 a and 32 a , respectively, of separator layers 30 and 32 opposing the first electrode 14 are second electrode 22 and third electrode 26 , respectively. Adjacent to and contacting the surface 30 b of separator layer 30 is support layer 18 . Second electrode 22 and third electrode 26 have surface areas 23 and 27 , respectively, defined by edge perimeters 24 and 28 , which may be substantially equal to the area 21 defined by the edge perimeter 20 of the support layer 18 . The surface areas 23 and 27 of electrodes 22 and 26 , respectively, may be equal or different in size. Advantageously, the surface areas 23 and 27 are substantially equal to the area 21 of support layer 18 . In this fashion, the support layer 18 maximizes support to both larger second and third electrodes 22 and 26 by maintaining a uniform outer edge surface of cell stack 12 without allowing the edges and corners of electrodes 22 and 26 from becoming vulnerable to pressures exerted during packaging and internal pressures maintained during the lifetime of the vacuum sealed dual-cell battery.
The present invention also provides a method of constructing or assembling a battery cell, such as a lithium ion battery cell, having a support layer. Referring again to FIG. 1 , the method comprises providing at least one anode and at least one cathode wherein either of the anode or the cathode is the first electrode 14 having a surface area 15 that is smaller relative to the larger surface area 23 of the other of the anode or the cathode, i.e., second electrode 22 . A support layer 18 is provided in surrounding contact with at least a portion of the first electrode 14 whereby the support layer 18 is adapted to provide reinforcing support to the larger second electrode 22 . Optimally, every first electrode 14 in a cell stack is surrounded by a support layer 18 during subsequent packaging in a multi-cell battery. Between each first electrode 14 and second electrode 22 in sequence, a separator layer 30 is placed, and first electrode 14 , support layer 18 , second electrode 22 , and separator layer 30 are joined to form a battery cell 10 .
Joining may involve vacuum sealing or other lamination methods to package the cell. As shown in FIG. 2 , seal 11 of cell 10 encloses the cell 10 and its components, first electrode 14 , support layer 18 , second electrode 22 , and separator layer 30 under vacuum. Vacuum and air pressures exerted on the cell 10 by packaging equipment conventionally used to package batteries vary depending on equipment. Conventional techniques known in the art to join components of a battery cell are suitable in the method of the present invention.
Other aspects of the present method include placing support layer 18 adjacent to the separator layer 30 prior to adding the first electrode 14 and joining the layers together to provide a joined battery cell 10 . Upon joining cell 10 would have the support layer 18 in a surrounding relation with at least a portion of the edge perimeter 16 of the smaller surface area 15 of first electrode 14 , i.e., either the anode or the cathode. Alternatively, battery cell 10 may be assembled such that the support layer 18 is independently provided in a surrounding relation with the edge perimeter 16 of smaller first electrode 14 prior to joining the layers together to form the cell 10 .
Accordingly, the support layer of the present invention provides sufficient support for larger electrode layers during packaging to eliminate the need for more complex and expensive packaging equipment, materials and processes, such as pre-formed or rigid packaging processes, for the manufacture and packaging of battery cells. Consequently, a capital cost savings, including equipment, materials and fabrication process savings together with battery cells having longer lifetimes and fewer shorts, may be realized during production.
While the present invention has been illustrated by the description of one or more embodiments thereof, and while the embodiments have been described in considerable detail, they are not intended to restrict or in any way limit the scope of the appended claims to such detail. Additional advantages and modifications will readily appear to those skilled in the art. The invention in its broader aspects is therefore not limited to the specific details, representative apparatus and method and illustrative examples shown and described. Accordingly, departures may be made from such details without departing from the scope or spirit of Applicants' general inventive concept.
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The present invention, a cell layer edge support, provides longer battery cell life while minimizing the possibility of shorts within the cell. More specifically, an edge support layer is positioned around at least a portion of the smaller electrode, either the anode or the cathode, in the cell to define a supporting perimeter comparable to the perimeter of the larger electrode. The support layer generally comprises a polymeric material which helps to absorb pressures exerted on the cell layers during packaging. The anode, cathode, support layer and a separator layer placed between the anode and the cathode may be joined to form a battery. Preferably, a plurality of cells having the support layer may be joined to form a higher energy, longer life battery.
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FIELD OF THE INVENTION
[0001] This invention relates a golf putter and a golf putting training apparatus which resides at a first end proximal and in contact with the golfer's neck with the putting swing correctly completed when the apparatus first end continues proximal and in contact with the neck at the conclusion of the swing. The invention, more particularly demonstrates an incorrect swing when the apparatus first end swings away from the neck toward the golfer's shoulder as the swing concludes.
BACKGROUND OF THE INVENTION
[0002] Different putter structures and methods are shown in the prior art. Included are the following U.S. Patents: U.S. Pat. No. 5,209,474 to Voyer; U.S. Pat. No. 5,342,055 to Diley; U.S. Pat. No. 5,529,306 to Staats et al.; U.S. Pat. No. 5,893,803 to Leadbetter et al.; U.S. Pat. No. 6,595,865 to Stitz; U.S. Pat. No. 5,465,971 to Tischler; U.S. Pat. No. 5,520,392 to Foresi et al.; U.S. Pat. No. 5,649,870 to Harrison; U.S. Pat. No. 6,572,486 to Sweinhart; U.S. Pat. No. 6,533,676 to D'Angelo et al.; U.S. Pat. No. 6,491,591 to Schuster; U.S. Pat. No. 6,350,207 to Arcuri; U.S. Pat. No. 5,665,007 to Tatum; U.S. Pat. No. 5,584,768 to Lee; and U.S. Pat. No. 4,461,479 to Mitchell.
[0003] The patents referred to herein are provided herewith in an Information Disclosure Statement in accordance with 37 CFR 1.97.
SUMMARY OF THE INVENTION
[0004] Prior art reveal many golf putters including the “long putter” and putters with a handle portion residing in the arm pit, stomach or chest during the putting swing.
[0005] The putter and putter training apparatus disclosed herein is a “neck putter” used such that the putter shaft, distal from the putter head, remains gently pressed against the golfer's neck during the execution of a proper putting stroke. The position of the putter shaft, distal from the golf club head, gives immediate feedback to the golfer on performing the “correct” and “incorrect” putting stroke before the ball is struck. Movement of the putter shaft, distal from the putter head and proximal and gently pressed against the golfer's neck, away from the neck and toward the shoulder signals the golfer that the golfer's wrists have improperly broker resulting in the putter shaft falling away from the neck, or in falling off the neck during the putting stroke. The golfer be trained, by use of the putter and or the putting training apparatus to stop making an “incorrect” putting stroke, which results in a bad putt, and to make a “correct” stroke.
[0006] The “neck putter” is longer than the “long putter” expected to be in the 60″ to 72″ length range. The training apparatus, the preferred embodiment of the invention, is an alternate to the putter and is used for training in addition to the putter. The training apparatus is an attachment, generally measuring approximately 36″ in length, which, in the preferred embodiment is received at the grip clip means by an existing putter shaft, slipped up the shaft such that the grip clip means is affixed by a friction fit at the golf putter grip. Alternative means to the grip clip means illustrated will be recognized by those of ordinary skills in the attaching and affixing arts for the temporary attachment of the training apparatus at the putter grip by connecting the grip clip or connecting means to a putter primarily at the putter grip.
[0007] The “neck putter” and training apparatus train the golfer to perform a more effective putting stroke achieved from muscle memory accomplished through repetition. Additionally, the “neck putter” principle is defined by keeping the putter pressed gently against the neck at all times during application of the putting stroke. This provides the user with an effective tool for enhancing the Stability, Tempo, and Pace (STP) required for an overall improved putting stroke.
BRIEF DESCRIPTION OF THE DRAWINGS
[0008] The foregoing and other features and advantages of the present invention will become more readily appreciated as the same become better understood by reference to the following detailed description of the preferred embodiment of the invention when taken in conjunction with the accompanying drawings, wherein:
[0009] FIG. 1 is a perspective drawing showing the golf apparatus and golf putter in combination where the apparatus first end is in contact with the golfer's neck and the grip clip means ( 40 ) is affixed by affixing means at the golf putter grip.
[0010] FIG. 2 illustrates the golf apparatus ( 5 ) showing the grip clip means ( 40 ).
[0011] FIG. 3 is a detail from FIG. 2 illustrating the grip clip ( 40 ) showing the grip clip first end ( 50 ), grip clip first end dimension D 1 ( 52 ), grip clip second end ( 60 ), grip clip slot ( 65 ) and grip clip slot dimension D 5 ( 66 ).
[0012] FIG. 4 illustrates the grip clip ( 40 ), as seen in FIG. 3 , viewing from the Grip clip second end ( 60 ).
[0013] FIG. 5 illustrates the process of interconnecting the golf apparatus ( 5 ) with a golf putter ( 70 ) where the grip clip slot dimension D 5 ( 66 ) is greater than the putter shaft dimension D 4 ( 54 ) allowing the tubular grip clip ( 40 ) to receive the putter shaft ( 72 ). The apparatus ( 5 ) and the tubular grip clip ( 40 ) slides on the putter shaft ( 72 ) toward the golf putter first end ( 80 ) and is affixed by a grip affixing means at the golf putter grip ( 75 ) or alternatively the grip clip means ( 40 ) is placed and affixed by clip affixing means at the golf putter grip ( 75 ).
[0014] FIG. 6 illustrates the grip clip ( 40 ) showing a hinge means ( 42 ) affixed by hinge affixing means to the apparatus shaft ( 10 ) at the apparatus second end ( 30 ).
[0015] FIG. 7 illustrates the neck putter ( 200 ) in position against the golfer's neck in preparation for the putter stroke.
[0016] FIG. 8 is a front elevation of the neck putter ( 200 ) showing the neck putter shaft length adjustment means ( 250 ).
[0017] FIG. 9 is a side elevation of the neck putter ( 200 ).
[0018] FIG. 10 illustrates a golfer utilizing the apparatus and golf putter in combination ( 1 ).
[0019] FIG. 11 shows the golfer utilizing the neck putter ( 200 ) where the apparatus has moved away from the golfer's neck indicating an incorrect golf putting stroke.
[0020] FIG. 12 shows the apparatus and golf putter in combination ( 1 ) demonstrating the grip clip ( 40 ) at the putter grip ( 80 ) in position for use by the golfer.
[0021] FIG. 13 shows the neck putter ( 200 ) with a neck putter grip ( 230 ).
DETAILED DESCRIPTION
[0022] The training apparatus with putter ( 1 ) and the apparatus ( 5 ), illustrated at FIGS. 1 through 6 , 10 and 12 show apparatus upper shaft ( 10 ), the apparatus upper shaft first end ( 20 ), the counter weight ( 22 ), the apparatus upper shaft second end ( 30 ), grip clip means ( 40 ) with hinge means ( 42 ). Seen at the grip clip means ( 40 ) is the grip clip first end ( 50 ) having a grip clip first end dimension D 1 ( 52 ), a grip clip second end ( 60 ) having a grip clip second end dimension D 2 ( 62 ) and a grip clip slot ( 65 ) having a grip clip slot dimension D 5 ( 66 ). Seen in FIGS. 1, 5 and 10 is a golf putter ( 70 ) having a golf putter shaft ( 72 ), a golf putter first end ( 80 ), a golf putter second end ( 90 ) and a golf putter head ( 100 ). The golf putter shaft ( 72 ) has a putter shaft dimension D 3 ( 54 ).
[0023] The preferred embodiment of the invention is the training apparatus and golf putter ( 1 ) comprising an apparatus ( 5 ) having an apparatus upper shaft ( 10 ). The apparatus upper shaft ( 10 ) having an apparatus upper shaft first end ( 20 ) and an apparatus upper shaft second end ( 30 ). Grip clip means ( 40 ) affixed to the apparatus upper shaft ( 10 ) at the apparatus upper shaft second end ( 30 ) by hinge means ( 42 ). A golf putter ( 70 ) having a golf putter lower shaft ( 72 ). The golf putter ( 70 ) having a golf putter lower shaft first end ( 80 ) and a golf putter lower shaft second end ( 90 ). A golf putter head ( 100 ) affixed by golf club head affixing means at the golf putter lower shaft second end ( 90 ). A golf putter grip ( 75 ) is received at the golf putter lower shaft first end ( 80 ). The golf putter grip ( 75 ) having a dimension D 4 ( 64 ) greater than a putter lower shaft ( 72 ) dimension D 3 ( 54 ). Dimensions are generally inside or outside diameters where the structures are generally tubular and circular in cross section. However, where not circular in cross section and where the structure is tubular, the dimension(s) will interrelate in illustrating the movement of the grip clip ( 40 ), generally tubular in structure, from a lower portion of the golf putter lower shaft ( 72 ) toward and in contact with the golf putter grip ( 75 ). It will be recognized that golf club tubular shafts are generally tapered from a smaller outside diameter proximal the golf club head to a greater outside diameter proximal the golf club grip ( 75 ) and that the golf club grip ( 75 ) will generally have a greater outside diameter or dimension, where not circular in cross section, than the golf putter lower shaft ( 72 ).
[0024] The apparatus upper shaft ( 10 ), golf putter lower shaft and golf putter grip ( 75 ) are generally tubular having a variety of cross sections. The grip clip means ( 40 ) generally comprises a tubular member means ( 42 ) having a grip clip first end ( 50 ) and a grip clip second end ( 60 ). The tubular member means ( 42 ) having a hinge means ( 42 ) affixed by hinge affixing means intermediate the grip clip first end ( 50 ) and the grip clip second end ( 60 ) at the tubular member means wall ( 43 ) at the outer surface ( 44 ). The hinge means ( 42 ) affixed by hinge affixing means at the apparatus second end ( 30 ) providing hinge interaction between the apparatus shaft ( 10 ) and the grip clip means ( 40 ). Hinge affixing means may be by formation of hinge leaves via injection molding or metal formation from rigid materials including plastics, metals and other equivalent materials; hinge means regarding the rotation of one hinge leaf relative to another hinge leaf may be by a bolt received via apertures in the hinge leaf aligned with apertures in the apparatus upper shaft ( 10 ) proximal the apparatus second end ( 30 ) and secured by a nut or by a leaf structure formed in a generally tubular form which is received by the apparatus second end ( 30 ) and which has hinge interconnection means relative to a second leaf structure illustrated here generally as a grip clip ( 40 ). Shaft means, in all embodiments, are generally a rigid material, tubular in structure formed from plastics, composite materials, metals and other equivalent materials.
[0025] A grip clip slot ( 65 ) in the wall ( 43 ) from the grip clip first end ( 20 ) to the grip clip second end ( 30 ) wherein the slot ( 65 ) has a grip clip slot dimension D 5 ( 66 ) which is greater than a putter shaft dimension D 3 ( 54 ) and which is sized to receive a golf putter shaft ( 72 ) intermediate the golf putter head ( 100 ) and the golf putter grip ( 75 ). The grip clip slot dimension D 5 ( 66 ) has a dimension less than the dimension of the golf putter grip dimension D 4 ( 64 ). The grip clip first end dimension D 1 ( 52 ) is less than the grip clip second end dimension D 2 ( 62 ). The grip clip first end dimension D 1 ( 52 ) and the grip clip second end dimension D 2 ( 62 ) is sized to receive the golf putter grip ( 75 ) and to be affixed by grip affixing means at the golf putter grip ( 75 ). The grip affixing means to affix the grip clip means ( 40 ) includes friction fitting by the fact of the grip clip first end dimension D 1 ( 52 ) being less than the grip clip second end dimension D 2 ( 62 ) and the golf putter grip dimension D 4 ( 64 ), proximal the apparatus first end ( 20 ) being greater than the grip clip second end dimension D 2 ( 62 ). The grip affixing means to affix the grip clip means ( 40 ) also includes other forms of gripping including a spring secured clam shell structure allowing the grip clip means ( 40 ) to be opened to allow the grip clip slot ( 65 ) to receive a golf putter grip ( 75 ). Other similar friction affixing, clamp affixing structures and other strictures will be viewed by those of ordinary skill in the art as equivalent. The apparatus ( 5 ) at the grip clip slot ( 65 ) will receive either the apparatus shaft ( 10 ) to slide up the apparatus shaft ( 10 ) toward the apparatus first end ( 20 ) and receive and be affixed at the golf putter grip ( 75 ) or the grip clip slot ( 65 ) will receive the golf putter grip ( 75 ) and be affixed by affixing means for use in putting. The apparatus ( 5 ) at the apparatus first end ( 20 ) will be placed by the golfer against the golfer's neck ( 21 ). The golfer will detect the position of the apparatus first end ( 20 ) relative to the golfer's neck ( 21 ) and when sensing that the apparatus first end ( 20 ) has moved away from the neck ( 21 ) and toward the golfer's shoulder ( 22 ) will realize that the golf stroke has been incorrectly executed. In the alternative, the golfer, in realizing that the apparatus first end ( 20 ) has remained in contact with the golfer's neck ( 21 ) throughout the putting stroke, will realize that the golf stroke has been correctly executed.
[0026] An embodiment of the invention is a neck putter ( 200 ) having an upper putter shaft ( 205 ) having an upper putter shaft terminus ( 206 ) and a lower putter shaft ( 207 ). The upper putter shaft ( 205 ) and lower putter shaft ( 207 ) are, in the preferred embodiment, comprised of tubular means but may be comprised of shaft means including plastics, composite materials, metals and other shaft materials recognized by those of ordinary skills in the golfing arts regarding golf shafts. The upper putter shaft ( 205 ) has an upper putter shaft first end ( 210 ) and an upper putter shaft second end ( 211 ). The lower putter shaft ( 207 ) has a lower putter shaft first end ( 212 ) and a lower putter shaft second end ( 220 ). A neck putter head ( 240 ) is affixed by golf putter and golf head affixing means at the lower putter shaft second end ( 220 ). The neck upper putter shaft first end ( 210 ) is distal from the upper putter shaft second end ( 211 ). A neck putter grip ( 230 ) means, generally tubular, is received by the upper putter shaft ( 205 ) at the upper putter shaft second end ( 211 ) and by the lower putter shaft ( 207 ) at the lower putter shaft first end ( 212 ). A neck putter second grip ( 235 ) means may be received by the upper putter shaft ( 205 ) intermediate the upper putter shaft first end ( 210 ) and the putter grip ( 230 ). Grip means ( 230 ) and ( 235 ) comprises a covering, generally tubular, or surface which is grasped by the golfer in operating the putter and in performing the golf stroke and may be composed of plastic, leather, foams and other materials commonly used in forming golf club grips.
[0027] The lower shaft ( 207 ) may be formed in two pieces comprising a lower shaft upper portion ( 208 ) and a lower shaft lower portion ( 209 ) for the purpose of allowing the lower putter shaft ( 207 ) to be adjusted in length by the lower shaft upper portion ( 208 ) to be received into or to receive the lower shaft lower portion ( 209 ) to allow adjustment of the length of the lower shaft ( 207 ) by use of a neck putter shaft length adjustment means ( 250 ). Neck putter lower shaft length adjustment means ( 250 ) may be comprised of allen screw asserting force from the lower shaft upper potion ( 208 ) against the lower shaft lower portion ( 209 ), a screw coupling received by threaded means at the lower shaft upper portion terminus ( 206 ) or the lower putter shaft ( 207 ) distal from the neck putter second end ( 220 ) which compresses either the lower shaft upper portion ( 208 ) proximal the lower shaft upper portion terminus ( 206 ) or the lower shaft lower portion ( 209 ) against the other. Other putter shaft length adjustment means ( 250 ) will be recognized by those of ordinary skills in the affixing arts to be the equivalent to those recited.
[0028] It will be recognized that rules of golf club construction will observed including, but not limited to, the angle of presentation between the golf putter head and the lower putter shaft ( 207 ) and that the moveable portions of the indicated structure including the putter shaft length adjustment means ( 250 ) will be fixed by a means which will make adjustment during play difficult. The neck putter second grip ( 235 ) is provided to allow the golfer an alternative means of holding the neck putter during the putter stroke. The neck putter ( 200 ) is adjusted to a length such that the upper putter shaft ( 205 ) proximal the neck putter first end ( 210 ) will be positioned proximal to and touching the golfer's neck during the putting stroke. A counter weight ( 202 ) may form or be placed within the upper putter shaft ( 205 ) proximal the neck putter first end ( 210 ).
[0029] While a preferred embodiment of the present invention has been shown and described, it will be apparent to those skilled in the art that many changes and modifications may be made without departing from the invention in its broader aspects. The appended claims are therefore intended to cover all such changes and modifications as fall within the true spirit and scope of the invention.
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A golf putter and a golf putting training apparatus are disclosed which resides at a first end proximal and in contact with the golfer's neck with the putting swing correctly completed when the apparatus first end continues proximal and in contact with the neck at the conclusion of the swing. An incorrect swing is demonstrated when the apparatus first end swings away from the neck toward the golfer's shoulder as the swing concludes.
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BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates, in general, to testing techniques and, more particularly, to a method for testing a plurality of functional circuit blocks, wherein each of the functional circuit blocks is designed as an existing semiconductor integrated circuit.
This claims priority under 35 USC §119 to Japanese patent application Serial Number 371925/2001, filed Dec. 5, 2001, the subject matter of which is incorporated herein by reference in its entirely for all purposes.
2. Description of the Related Art
In recent years, a system LSI comprises many functional circuit blocks. The functional circuit block which is a core of the system LSI, is called as intellectual property (IP), macro cell or so on. The IP is a block which is designed in the state of hardware or software and executes a specific operation.
A conventional method for testing the functional circuit blocks in the system LSI sets a plurality of test groups each comprising a plurality of the functional circuit blocks to be tested simultaneously, using a combination of a parallel access method and a serial access method. The conventional method tests the test groups in turn. The concept of the parallel access method is shown in FIG. 14 . As shown in FIG. 14 , each of the input and output terminals of each of IP 1401 and 1402 connects with the outer terminals of the system LSI 1400 with one-one relation. The parallel access method tests a plurality of IP parallel using the outer terminals of the system LSI, by inputting a signal to IP from the outer terminals directly and observing an output signal output by the outer terminals directly. The concept of the serial access method is shown in FIG. 15 . As shown in FIG. 15 , there are a serial-parallel converter 1501 and a parallel-serial converter 1502 between the outer terminals of the system LSI 1500 and the input and output terminals of IP 1503 and 1504 . The serial access method tests a plurality of IP serially using the outer terminals of the system LSI, by inputting a signal to IP from the outer terminals through the serial-parallel converter 1501 and observing an output signal output by the outer terminals through the parallel-serial converter 1502 .
An operation of the conventional method for testing the functional circuits in the system LSI will be described with reference to FIG. 16 . The vertical axis shows the range of the number of pins of the system LSI necessary for testing. The horizontal axis shows test time necessary for testing. Six functional circuit blocks IP(A)–IP(F) are shown in FIG. 16 . A vertical length of each functional circuit block is indicative of the number of pins of the system LSI necessary for testing. A horizontal length of each functional circuit block is indicative of test time necessary for testing.
The conventional test method divides the functional circuit blocks into a plurality of test groups. In FIG. 16 , the functional circuit blocks are divided into four test groups. A first test group comprises the functional circuit blocks IP(A) and IP(B). A second test group comprises the functional circuit blocks IP(C) and IP(D). A third test group comprises the functional circuit block IP(E). A fourth test group comprises the functional circuit block IP(F).
The conventional test method tests the functional circuit blocks by test groups. First, the first test group is tested. Next, the second test group is tested, after the test in the first test group is finished. Correspondingly, the third test group is tested, after the test in the second test group is finished. The fourth test group is tested, after the test in the third test group is finished.
However, each of the functional circuit blocks in each test group does not always have the same test time as the other functional circuit blocks in the corresponding test group. The test time of the functional circuit block IP(A) is longer than that of the functional circuit block IP(B). The non-used pins of the system LSI for testing exist uselessly, from the time of finishing the test in the functional circuit block IP(A) until finishing the test in the functional circuit block IP(B). The testing of the second test group can not start immediately after the test of the functional circuit block IP(B) is finished, because the test in the functional circuit block IP(A) has not been finished yet. Therefore, the conventional test method does not use the non-used pins of the system LSI effectively.
SUMMARY OF THE INVENTION
According to one aspect of the present invention, there is provided a method for testing a plurality of the functional circuit blocks in the system LSI, the method comprising dividing a plurality of the functional circuit blocks into at least a first test group and a second test group, wherein the first test group is tested before the second test group, and starting testing of one functional circuit block in the second test group immediately after one functional circuit block in the first test group is finished being tested.
The novel features of the invention will more fully appear from the following detailed description, appended claims and the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is an operational diagram showing a method for testing functional circuit blocks according to a first preferred embodiment of the present invention.
FIG. 2 is a block diagram showing the number of LSI pins and testing time according to the first preferred embodiment of the present invention.
FIG. 3 is a block diagram showing a test circuit according to the first preferred embodiment of the present invention.
FIG. 4 is a timing chart showing necessary time for testing each functional circuit block shown in FIG. 2 .
FIG. 5 is an operational diagram showing a method for testing functional circuit blocks according to a second preferred embodiment of the present invention.
FIG. 6 is a block diagram showing the number of LSI pins and testing time according to the second preferred embodiment of the present invention.
FIG. 7 is a block diagram showing a test circuit according to the second preferred embodiment of the present invention.
FIG. 8 is a timing chart showing necessary time for testing each functional circuit block shown in FIG. 6 .
FIG. 9 is an operational diagram showing a method for testing functional circuit blocks according to a third preferred embodiment of the present invention.
FIG. 10 is a block diagram showing the number of LSI pins and testing time according to the third preferred embodiment of the present invention.
FIG. 11 is a block diagram showing a test circuit according to the third preferred embodiment of the present invention.
FIG. 12 is a timing chart showing necessary time for testing each functional circuit block shown in FIG. 10 .
FIG. 13 is an operational diagram showing a method for testing functional circuit blocks according to a fourth preferred embodiment of the present invention.
FIG. 14 is a block diagram for describing a parallel access method.
FIG. 15 is a block diagram for describing a serial access method.
FIG. 16 is a block diagram showing the number of LSI pins and testing time according to a conventional method for testing functional circuit blocks.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
A method for testing functional circuit blocks of the present invention will be explained with reference to the preferred embodiments of the present invention. Moreover, not all the combinations of the characteristics of the present invention described in the embodiments are essential to the problem solving means of the present invention.
A method for testing the functional circuit blocks according to a first preferred embodiment of the present invention will be described with reference to FIGS. 1–4 . FIG. 1 is an operational diagram showing the method for testing the functional circuit blocks according to the first preferred embodiment of the present invention. FIG. 2 is a block diagram showing the number of LSI pins and testing time according to the first preferred embodiment of the present invention. FIG. 3 is a block diagram showing a test circuit according to the first preferred embodiment of the present invention. FIG. 4 is a timing chart showing time necessary for testing each functional circuit block shown in FIG. 2 .
First, an operation of the method for testing the functional circuit blocks according to the first preferred embodiment of the present invention will be explained with reference to FIGS. 1 and 2 . In FIG. 2 , the vertical axis P shows the range of the number of pins of the system LSI which are available for testing the functional circuit blocks. The horizontal axis T shows test time to finish testing in the functional circuit blocks. The functional circuit blocks are shown as IP(i). IP(i)t shows test time necessary for testing the functional circuit block IP(i) and IP(i)p shows the number of pins of the system LSI necessary for testing.
In step S 101 , each test time necessary for testing each functional circuit block and each of the number of pins of the system LSI necessary for testing each functional circuit blocks, are determined. In FIG. 2 , each test time IP(A)t–IP(F)t and each of the number of pins IP(A)p–IP(F)p are determined. In addition, in step S 101 , the functional circuit block having the longest test time among the functional circuit blocks, is selected. In FIG. 2 , the functional circuit block IP(A) having test time IP(A)t is selected. As shown in FIG. 2 , test time IP(A)t has the longest horizontal length.
In step S 102 , one of the functional circuit blocks is selected from among the non-selected functional circuit blocks of step S 101 in consideration of the number of pins of the system LSI which are available for starting testing in parallel with the functional circuit block selected in step S 101 . In FIG. 2 , the functional circuit block IP(B) is selected. The following relationship is considered:
P=IP ( A ) p+IP ( B ) p+ΔP 1 [1],
wherein ΔP1 is the number of unused pins of the LSI when the functional circuit blocks IP(A) and IP(B) are simultaneously tested. The smaller the value ΔP1 is, the more efficient the method for testing becomes. The other functional circuit blocks IP(C)–IP(F) are not selected, because testing of the other functional circuit blocks IP(C)–IP(F) can not be started with the functional circuit block IP(A) at the same time out of consideration of the number of pins of the system LSI. Also, if for example the functional circuit block IP(D) is selected instead of the functional circuit block IP(B), ΔP2 (=P−IP(A)p−IP(D)p) is larger than ΔP1. The method for testing becomes inefficient if the functional circuit block IP(D) is selected in step S 102 instead of functional circuit block IP(B).
In step S 103 , the functional circuit blocks selected in steps S 102 and S 103 are set as one test group. These set functional circuit blocks can be tested by the parallel access method at the same time. In FIG. 2 , the functional circuit blocks IP(A) and IP(B) are set as one test group (1st test group).
In step S 104 , it is determined whether there is a non-selected functional circuit block or not. If there is a non-selected functional circuit block, steps S 101 –S 103 are repeated. If not, step S 105 is executed. In FIG. 2 , the functional circuit blocks IP(C) and IP(D) are set as one test group (2nd test group). The functional circuit block IP(E) is set as one test group (3rd test group) and the functional circuit block IP(F) is set as one test group (4th test group). In FIG. 2 , there are four test groups.
By the way, in the 1st test group, test time IP(B)t is shorter than test time IP(A)t. So, the test process for the functional circuit block IP(B) is finished faster than the test process for the functional circuit block IP(A). When the test process for the functional circuit block IP(B) is finished, the number of non-used pins ΔP3 (=P−IP(A)p)>ΔP1 exists until the test process for the functional circuit block IP(A) is finished.
So, in step S 105 , it is determined whether there is a functional circuit block among the next test group which is available as a pretest group for starting to test using the non-used pins of the system LSI during the test process of the first test group. If such a functional circuit block is determined as available in step S 105 , step S 106 is executed, and if not, step S 107 is executed. In more detail with reference to FIG. 2 , according to the relationship between the 1 st test group and the 2nd test group, the functional circuit block IP(D) in the 2nd test group is available for starting to test using the non-used pins of the system LSI during the test process for the 1st test group. So, the functional circuit block IP(D) is selected out of consideration for the test time. Usually, the functional circuit block having the longest test time is selected.
In step S 106 , the functional circuit block which is selected in step S 105 , is added to the pre-test-group. Therefore, immediately after the test process for one functional circuit block in the first test group is finished, the test process for the functional circuit block which is selected in step S 105 in the pretest group is started. In FIG. 2 , the functional circuit block IP(D) is selected as in the pretest group and is thus added to the 1st test group. Therefore, immediately after the test process for the functional circuit block IP(B) is finished, the test process for the functional circuit block IP(D) is started.
In step S 107 , it is determined whether there is a non-selected test group or not. If there is a non-selected test group, steps S 105 and S 106 are executed. If not, step S 108 is executed. In FIG. 2 , there are a 3rd test group and a 4th test group. Steps S 105 and S 106 are executed for the 3rd test group and 4th test group.
In step S 108 , a test circuit is provided for each test group as shown in FIG. 3 . The test circuit has a test control circuit 310 and the functional circuit blocks 320 – 370 . The test control circuit 310 and the functional circuit blocks 320 – 370 are connected to each other by the control bus. Each of the functional circuit blocks 320 – 370 is controlled through the control bus by the test control circuit 310 . In addition, the test control circuit 310 has a test access circuit and so on. As shown in FIG. 3 , each functional circuit block is tested by the parallel access method. Returning to FIG. 3 , the test process for the functional circuit blocks is executed.
In FIG. 4 , each wave form shows the testing status of each functional circuit block. The rising part of the wave form shows the status of being tested. The falling part of the wave shows the status of not being tested. As shown in FIG. 4 , the test process for the functional circuit blocks IP(A) and IP(B) are started at the same time. Next, immediately after the test process for the functional circuit block IP(B) is finished, the test process for the functional circuit block IP(D) is started. Next, immediately after the test process for the functional circuit block IP(A) is finished, the test process for the functional circuit block IP(C) is started. Next, immediately after the test process for the functional circuit blocks IP(C) and IP(D) is finished, the test process for the functional circuit block IP(E) is started. Next, immediately after the test process for the functional circuit block IP(E) is finished, the test process for the functional circuit block IP(F) is started. Therefore, total test time is the sum of IP(B)t, IP(D)t, IP(E)t and IP(F)t. On the other hand, total test time of the conventional test method is the sum of IP(A)t, IP(D)t, IP(E)t and IP(F)t. Thus, total test time of the first preferred embodiment of the present invention is shorter than total test time of the conventional test method by the difference between IP(A)t and IP(B)t.
The method for testing the functional circuit blocks according to the first preferred embodiment of the present invention starts to test next test group without waiting for finishing all of test processes of the previous test group. The method for testing the functional circuit blocks according to the first preferred embodiment of the present invention saves the time necessary for finishing all of the test processes of the previous test group. Therefore, the method for testing the functional circuit blocks according to the first preferred embodiment of the present invention reduces test time for the functional circuit blocks of the system LSI in comparison with the conventional method.
A method for testing the functional circuit blocks according to a second preferred embodiment of the present invention will be described with reference to FIGS. 5–8 . FIG. 5 is an operational diagram showing the method for testing the functional circuit blocks according to the second preferred embodiment of the present invention. FIG. 6 is a block diagram showing the number of LSI pins and testing time according to the second preferred embodiment of the present invention. FIG. 7 is a block diagram showing a test circuit according to the second preferred embodiment of the present invention. FIG. 8 is a timing chart showing necessary time for testing each functional circuit block shown in FIG. 6 . Like elements are given like or corresponding reference numerals in the first and second preferred embodiments. Thus, dual explanations of the same elements are avoided.
First, an operation of the method for testing the functional circuit blocks according to the second preferred embodiment of the present invention will be explained with reference to FIG. 5 . The steps S 501 –S 505 shown in FIG. 5 are added between step S 107 and step S 108 shown in FIG. 1 .
In step S 501 , it is determined whether a test group comprises only one functional circuit block or not. If a test group comprises only one functional circuit block, step S 502 is executed, and if not, step S 505 is executed.
In step S 502 , whether or not the functional circuit block can be tested in parallel with test processes of another test group by the serial access method is determined, based on consideration of the number of pins of the system LSI. If it can be tested, step S 503 is executed. If not, step S 505 is executed.
In step S 503 , it is determined whether test time of the functional circuit block to be tested by the serial access method is shorter than total test time of the other test groups or not. If it is, step S 504 is executed. If not, step S 505 is executed. In step S 504 , the functional circuit block is added to another test group. Then, step S 505 is executed.
In step S 505 , it is determined whether additional test groups exist or not. If so, step S 501 is executed again. If not, step S 108 is executed.
Next, an operation of the method for testing the functional circuit blocks according to the second preferred embodiment of the present invention will be explained with reference to FIG. 6 concretely.
In step S 501 , first, the 1st test group is checked. The 1st test group comprises two functional circuit blocks IP(A) and IP(B), so step S 505 is executed. In step S 505 , additional test groups (2nd, 3rd, 4th test groups) exist, so step S 501 is executed again. The process of the 2nd test group is omitted for the same reason as the 1st test group. In step S 501 again, the 3rd test group is checked. The 3rd test group comprises only one functional circuit block IP(E), so step S 502 is executed. It is determined that the 3rd test group can be tested by the serial access method in parallel with other test groups, so step S 503 is executed. Test time of the functional circuit block IP(E) of the 3rd test group to be tested by the serial access method is shorter than total test time of the other test groups, so step S 504 is executed. In step S 504 , the functional circuit block IP(E) of the 3rd test group is added to other test groups (1st, 2nd and 4th test groups) and is shown as IP(E 1 ) in FIG. 6 . In step S 505 , the 4th test group is checked, the 4th test group is checked in step S 501 again. The 4th test group comprises only one functional circuit block IP(F), so step S 502 is executed. In step S 502 , it is determined that the 4th test group can not be tested in parallel with another test groups, so step S 505 is executed. In step S 505 , additional test group do not exist, so step S 108 is executed.
In step S 108 , a test circuit is provided for each test group as shown in FIG. 7 . The test circuit has a test control circuit 710 and the functional circuit blocks 720 – 770 . The test control circuit 710 and the functional circuit blocks 720 – 770 are connected to each other by the control bus. Each functional circuit block 720 – 770 is controlled through the control bus by the test control circuit 710 . In addition, the test control circuit 710 has a test access circuit and so on. As shown in FIG. 7 , all functional circuit blocks except for the functional circuit block IP(E 1 ) are tested by the parallel access method, the functional circuit block IP(E 1 ) is tested by the serial access method. Returning to FIG. 7 , the test process for the functional circuit blocks is executed.
In FIG. 8 , each wave form shows the testing status of each functional circuit block. The rising part of the wave form shows the status of being tested. The falling part of the wave shows the status of not being tested. As shown in FIG. 8 , the test process for the functional circuit blocks IP(A), IP(B) and IP(E 1 ) are started at the same time. Next, immediately after the test process for the functional circuit block IP(B) is finished, the test process for the functional circuit block IP(D) is started. Next, immediately after the test process for the functional circuit block IP(A) is finished, the test process for the functional circuit block IP(C) is started. Next, immediately after the test process for the functional circuit blocks IP(C) and IP(D) is finished, the test process for the functional circuit block IP(F) is started. Therefore, total test time is the sum of IP(B)t, IP(D)t and IP(F)t. On the other hand, total test time of the conventional test method is the sum of IP(A)t, IP(D)t, IP(E)t and IP(F)t. Thus, total test time of the second preferred embodiment of the present invention is shorter than total test time of the conventional test method by the difference IP(A)t+IP(E)t−IP(B)t. In addition, total test time of the first preferred embodiment of the present invention is the sum of IP(B)t, IP(D)t, IP(E)t and IP(F)t. Therefore, total test time of the second preferred embodiment of the present invention is shorter than total test time of the first preferred embodiment by the difference IP(E)t.
As the method for testing the functional circuit blocks according the first preferred embodiment of the present invention, the method for testing the functional circuit blocks according to the second preferred embodiment of the present invention can start to test next test group without waiting for finishing all of test processes of previous test group. The method for testing the functional circuit blocks according to the second preferred embodiment of the present invention saves the time necessary for finishing all of the test processes of the previous test group. Therefore, the method for testing the functional circuit blocks according to the second preferred embodiment of the present invention reduces test time for the functional circuit blocks of the system LSI in comparison with the conventional method.
Furthermore, the method for testing the functional circuit blocks according to the second preferred embodiment of the present invention tests the functional circuit blocks using a combination of the parallel access method and the serial access method. Therefore, the method for testing the functional circuit blocks according to the second preferred embodiment of the present invention reduces test time for the functional circuit blocks of the system LSI in comparison with the method according to the first preferred embodiment of the present invention.
A method for testing the functional circuit blocks according to a third preferred embodiment of the present invention will be described with reference to FIGS. 9–12 . FIG. 9 is an operational diagram showing the method for testing the functional circuit blocks according to the third preferred embodiment of the present invention. FIG. 10 is a block diagram showing the number of LSI pins and testing time according to the third preferred embodiment of the present invention. FIG. 11 is a block diagram showing a test circuit according to the third preferred embodiment of the present invention. FIG. 12 is a timing chart showing necessary time for testing each functional circuit block shown in FIG. 10 . Like elements are given like or corresponding reference numerals in the above preferred embodiments. Thus, dual explanations of the same elements are avoided.
First, an operation of the method for testing the functional circuit blocks according to the third preferred embodiment of the present invention will be explained with reference to FIG. 9 . The steps S 901 –S 905 shown in FIG. 9 are added between step S 505 and step S 108 shown in FIG. 5 .
In step S 901 , it is determined whether a test group comprises only one functional circuit block or not. If the test group has only one functional circuit block, step S 902 is executed. If not, step S 905 is executed.
In step S 902 , whether or not the functional circuit block can be tested in parallel with test processes of another test group by a parallel/serial combination access method is determined, based on consideration of the number of pins of the system LSI. If it can be tested, step S 903 is executed. If not, step S 905 is executed.
In step S 903 , it is determined whether or not test time of the functional circuit block to be tested by the parallel/serial combination access method is shorter than total test time of the other test groups. If it is, step S 904 is executed. If not, step S 905 is executed. In step S 904 , the functional circuit block is added to other test groups. Then, step S 905 is executed.
In step S 905 , it is determined whether additional test groups exist or not. If additional test groups exist, step S 901 is executed again. If not, step S 108 is executed.
Next, an operation of the method for testing the functional circuit blocks according to the third preferred embodiment of the present invention will be explained with reference to FIG. 10 concretely.
In step S 901 , first, the 1st test group is checked. The 1st test group is comprised with two functional circuit blocks IP(A) and IP(B), so step S 905 is executed. In step S 905 , the additional test groups (2nd, 3rd, 4th test groups) exist, so step S 901 is executed again. The process of the 2nd test group is omitted for the same reason as the 1st test group. In step S 901 again, the 3rd test group is checked. The 3rd test group is comprised with only one functional circuit block IP(E 1 ), so step S 902 is executed. As explained above in the preferred embodiment, the 3rd test group is decided to be tested by the serial access method, so step S 905 is executed. After step S 905 , in step S 901 again, the 4th test group is checked. The 4th test group is comprised with only one functional circuit block IP(F), so step S 902 is executed. It is determined that the 4th test group can be tested by the parallel/serial combination access method in parallel with other test groups, so step S 903 is executed. Test time of the functional circuit block IP(F) of 4th test group to be tested by the parallel/serial combination access method is shorter than total test time of the other test groups, so step S 904 is executed. In step S 904 , the functional circuit block IP(F) of 4th test group is added to other test groups (1st, 2nd and 3rd test groups) and is shown as IP(F 1 ) in FIG. 10 . In step S 905 , the additional test groups do not exist, so step S 108 is executed.
In step S 108 , a test circuit is provided for each test group as shown in FIG. 11 . The test circuit has a test control circuit 1101 and the functional circuit blocks 1102 – 1107 . The test control circuit 1101 and the functional circuit blocks 1102 – 1107 are connected with the control bus to each other. Each functional circuit block 1102 – 1107 is controlled through the control bus by the test control circuit 1101 . In addition, the test control circuit 1101 has a test access circuit and so on. As shown in FIG. 11 , the functional circuit blocks IP(A)–IP(D) are tested by the parallel access method, the functional circuit block IP(E 1 ) is tested by the serial access method and the functional circuit block IP(F 1 ) is tested by the parallel/serial combination method. Then, the test process for the functional circuit blocks is executed.
In FIG. 12 , each wave form shows the testing status of each functional circuit block. The rising part of the wave form shows the status of being tested. The falling part of the wave shows the status of not being tested. As shown in FIG. 12 , the test process for the functional circuit blocks IP(A), IP(B), IP(E 1 ) and IP(F 1 ) are started at the same time. Next, immediately after the test process for the functional circuit block IP(B) is finished, the test process for the functional circuit block IP(D) is started. Next, immediately after the test process for the functional circuit block IP(A) is finished, the test process for the functional circuit block IP(C) is started. Therefore, total test time is the sum IP(E 1 )t of IP(B)t, IP(D) and Δα. On the other hand, total test time of the conventional test method is the sum of IP(A)t, IP(D)t, IP(E)t and IP(F)t. Thus, total test time of the third preferred embodiment of the present invention is shorter than total test time of the conventional test method by the difference IP(A)t+IP(E)t+IP(F)t−IP(B)−Δα. In addition, total test time of the first preferred embodiment of the present invention is the sum of IP(B)t, IP(D)t, IP(E)t and IP(F)t. Therefore, total test time of the third preferred embodiment of the present invention is shorter than total test time of the first preferred embodiment by the difference IP(E)t+IP(F)t−Δα. Furthermore, total test time of the second preferred embodiment of the present invention is the sum of IP(B)t, IP(D)t and IP(F)t. Therefore, total test time of the third preferred embodiment of the present invention is shorter than total test time of the second preferred embodiment by the difference IP(F)t−Δα.
As the method for testing the functional circuit blocks according the first and second preferred embodiments of the present invention, the method for testing the functional circuit blocks according to the third preferred embodiment of the present invention starts to test next test group without waiting for finishing all of test processes of previous test group. The method for testing the functional circuit blocks according to the third preferred embodiment of the present invention saves the time needed to wait for finishing all of test processes of previous test group. Therefore, the method for testing the functional circuit blocks according to the third preferred embodiment of the present invention reduces test time for the functional circuit blocks of the system LSI in comparison with the conventional method.
Furthermore, the method for the method for testing the functional circuit blocks according to the third preferred embodiment of the present invention tests the functional circuit blocks using a combination of the parallel access method, the serial access method and parallel/serial combination access method. Therefore, the method for testing the functional circuit blocks according to the third preferred embodiment of the present invention reduces test time for the functional circuit blocks of the system LSI in comparison with the method according to the first and second preferred embodiments of the present invention.
A method for testing the functional circuit blocks according to a fourth preferred embodiment of the present invention will be described with reference to FIG. 13 . FIG. 13 is an operational diagram showing the method for testing the functional circuit blocks according to the fourth preferred embodiment of the present invention. The method for testing the functional circuit blocks according to the fourth preferred embodiment of the present invention provides an improvement of the first preferred embodiment. The method for testing the functional circuit blocks according to the first preferred embodiment of the present invention decides all test groups and then adjusts the relationship among the test groups. However, the method for testing the functional circuit blocks according to the fourth preferred embodiment of the present invention adjusts the relationship between predecided test group and newly decided test groups every newly decided test group.
An operation of the method for testing the functional circuit blocks according to the fourth preferred embodiment of the present invention will be explained with reference to FIG. 13 .
In step S 1301 , test time necessary for testing each functional circuit block and the number of pins of the system LSI necessary for testing each functional circuit block are calculated.
In step S 1302 , the functional circuit block of which test time is the longest test time among all functional circuit blocks, is selected.
In step S 1303 , it is determined whether or not there is a functional circuit block which can be tested in parallel with the functional circuit block selected in step S 1302 among the non-selected functional circuit blocks out of consideration for the number of pins of the system LSI. If there is, step S 1304 is executed, and the functional circuit block is selected. Steps S 1303 and S 1304 are repeated until there is no functional circuit block which can be tested in parallel with the functional circuit block selected in step S 1302 . If the decision in step S 1303 is no, step S 1305 is executed and the functional circuit blocks selected in steps S 1302 –S 1304 are set as one test group. Next, step S 1306 is executed.
In step S 1306 , it is determined whether or not there is a non-selected functional circuit block. If there is, step S 1307 is executed. If not, step S 1309 is executed.
In step S 1307 , it is determined whether or not there is a functional circuit block among the non-selected functional circuit blocks which is available for starting to test using the non-used pins of the system LSI at test process for a predecided test group. If there is, step S 1308 is executed. If not, step S 1303 is executed.
In step S 1308 , the functional circuit block is added to the predecided test group. Therefore, immediately after the test process for one functional circuit block in the predecided test group is finished, the test process for the added functional circuit block is started. Next, step S 1306 is executed.
Step S 1309 is equal to step S 108 . In step S 1309 , a test circuit is provided for each test group.
As the method for testing the functional circuit blocks according the first preferred embodiments of the present invention, a method for testing the functional circuit blocks according to a fourth preferred embodiment of the present invention starts to test a next test group without waiting for finishing all of test processes of previous test group. The method for testing the functional circuit blocks according to the fourth preferred embodiment of the present invention saves the time needed to wait for finishing all of test processes of previous test group. Therefore, the method for testing the functional circuit blocks according to the fourth preferred embodiment of the present invention reduces test time for the functional circuit blocks of the system LSI in comparison with the conventional method.
Furthermore, the method for testing the functional circuit blocks according to the fourth preferred embodiment of the present invention adjusts the relationship between predecided test group and newly decided test group for every newly decided test group.
While the preferred form of the present invention has been described, it is to be understood that modifications will be apparent to those skilled in the art without departing from the spirit of the invention.
The scope of the invention, therefore, is to be determined solely by the following claims.
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A method for testing a plurality of functional circuit blocks of a system LSI, including dividing the plurality of functional circuit blocks into at least a first test group and a second test group, wherein the first test group is tested before the second test group and wherein testing of a functional circuit block in the second test group is started immediately after testing of a functional circuit block in the first test group is finished.
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This is a division, of application Ser. No. 593,367 filed July 7, 1975.
BACKGROUND OF THE INVENTION
In previous devices the adjustments of the backstops to the length of the sheets discharged from the sheet making device were performed manually and the inaccuracy of such adjustments affected unfavorably the uniformity of the stacks formed at the discharge end of the stacker; furthermore the snubber mechanism must be properly adjusted both at the delivery end of the take-off conveyor and at the receiving end of the adjacent stacker device for proper transmittal of the bundles of sheets formed on the take-off conveyor.
The object of this invention is to provide accurate control for the positioning of the back-up device and also to facilitate the adjustment of the snubbers for the accurate arrangement and transmission of the bundles of sheets for stacking.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a perspective view of the conveyor system indicating the location of the improved devices thereon.
FIG. 2 is an end view of the take-off conveyor showing one end of the support for the back-up device and its connection for the adjustment of the spacing of the back-up abutments.
FIG. 3 is a fragmental end view of the dial and switch control and indicator for the back-up adjustment on a larger scale.
FIG. 4 is a sectional view of the adjustment control device, the section being taken substantially on 4--4 of FIG. 3.
FIG. 5 is a developed view of the adjustment control device and the switch actuated by the dial and reductor transmission.
FIG. 6 is a fragmental perspective view showing the relation of the indicator for the back-up support to the snubber support at the discharge end of the take-off conveyor.
FIG. 7 is a fragmental view showing the guard and guide for the sheets at the delivery to the take-off conveyor.
FIG. 8 is a fragmental view showing the adjustable mounting for the snubbers at the discharge end of the conveyor.
FIG. 9 is a partly sectional view on a larger scale of the adjustable mounting ahd support of the snubbers.
FIG. 10 is the support in relation to the discharge end of the take-off conveyor above the layboy.
FIG. 11 is a fragmental perspective view of the anchoring of the adjusting chain for the snubber support at the receiving end of the layboy.
FIG. 12 is a side view of the adjustable assembly for the snubber rollers at the receiving end of the layboy.
FIG. 13 is a partially sectional view of the guiding of the supporting bracket of the snubber assembly at the layboy.
FIG. 14 is a partially sectional view of the adjusting and clamping device for one of the brackets of the snubber assembly at the layboy.
FIG. 15 is a fragmental perspective view showing part of the adjusting device for the snubbers at the layboy.
FIG. 16 is a developed view of the clamping device to clamp and hold the bracket of the snubber assembly in adjusted position.
FIG. 17 is a diagram of the circuits for adjusting the back-up device.
DETAILED DESCRIPTION
The overall conveyor system includes a delivery conveyor 1 which delivers the sheets from the sheet making machines such as a cutting machine 2. The sheets from the delivery conveyor 1 are dropped onto a take-off conveyor 3 which latter consists of a plurality of rollers 4 driven in the manner described in the aforementioned patent. Rollers 6 at the discharge end of the take-off conveyor are driven at an accelerated rate of speed whereby the sheets are delivered onto the layboy conveyors 7 of the stacker device 8 of the type described in Martin U.S. Pat. No. 3,321,202. The ratio of speed of the various conveyors, as described in the first mentioned patent, is such that the sheets are advanced on the take-off conveyor a distance equal to the width of one sheet at the rate of the cutting of the sheets by the cutting machine 2 whereby the rows of sheets passing upon the take-off conveyor 3 ultimately are stacked in bundles equivalent to the number of multiple cuts by the cutting machine 2.
For the proper alignment of the sheets on the take-off conveyor 3 the sheets delivered thereon are aligned by a back-up device 11. The bundles of sheets 12 are suitably held together on the accelerated speed rollers 6 by a row of snubbers 13. The bundles are then transferred to the intake end of the layboy conveyors 7 and then to a stacker device 8. In the present illustration the layboy conveyors 7 are on a rocking layboy frame 14 and are held together in bundles by snubbers 16. The pivoted portion 17 of the stacker device 8 rises and lowers and operates in the manner described in said Martin U.S. Pat. No. 3,321,202.
The back-up device 11 includes a bracket 18 at each end of the take-off conveyor 3. A shaft 19 is extended between the brackets. On the shaft 19 are a plurality of levers 21, as shown in FIGS. 2 and 6. Each lever 21 has a hub 22 rotatable on the shaft 19. On the lower end of each lever 21 is an abutment member 23 which tapers parallel with the adjacent rollers 4 toward the receiving side of said take-off conveyor 3. An arm 24 extends from each hub 22 and on each arm 24 there is a counter-weight 26 slidable on the respective arm 24 for the selected balance or play required to accommodate the sheets in the respective bundles travelling along the take-off conveyor 3. A deflector plate 27 is secured to slanting edges 28 of the brackets 18 facing toward the receiving side of the take-off conveyor 3 and diverging from the rollers 4 upwardly and toward the receiving side of the take-off conveyor 3 thereby to deflect the sheets thrown off the delivery conveyor 1 downwardly below the tapered abutment members 23, thereby to accurately register and align the edges of the sheets as they are bundled and travel on the take-off conveyor 3.
In order to accurately adjust the positions of the abutment members 23 to the length of the sheets 12 delivered onto the take-off conveyor 3, the back-up device 11 is adjustable. Each bracket 18 has a pair of wheels 30 thereon which ride on an adjacent rail 29 as shown in FIG. 2. From the bottom edge of each bracket 18 extend a pair of ears 31 and on each ear is anchored the end of a chain 32. Each chain 32 is on a suitable sprocket 33 at each end thereof, which latter are journalled near the respective ends of the rail 29. One of the sprockets 33 is driven by a chain and sprocket drive 34. A suitable reduction gearing 36 driven by an electric motor 37 drives the chain and sprocket drive 34 in selected directions. The sprockets 33 farthest from the chain and sprocket drive 34 are keyed on a cross shaft 35 for simultaneously adjusting the position of the brackets 18 to the length of the sheets 12 delivered to the take-off conveyor 3. Another electric motor 38 or other suitable power source drives through a belt and pulley transmission 39 the rollers 6 in the manner described in said first mentioned Martin Patent.
The controls for the adjustment of the back-up device 11 are illustrated in FIGS. 2, 3, 4, 5, and 6. On a fixed bracket 41 on one side of frame member 42 of the take-off conveyor 3 is mounted a suitable reduction gearing 43 which is connected by a flexible cable 44 to a gear transmission 46 on the cross shaft 35. A drive shaft 47 extends from the reduction gearing 43 and is keyed to a bearing hub 48. This bearing hub 48 is formed with an enlarged boss 49 and a disc 51. On the enlarged bearing boss 49 is rotatable a dial disc 52 with scale graduations 53 thereon. From the disc 51 extends a radial pin 54. Limit pins 56 extend from the dial disc 52 and are so spaced so as to limit the rotating motion of the dial disc 52 within the range of the graduations 53. On the boss 49 is a pointer disc 57 with a pointer mark 58 on its edge. A clamping disc 59 is fixedly secured to the boss 49 by screws 61. The pointer disc 57 is connected to the clamping disc 59 by a pin 62 extending from the clamping disc 59 into the pointer disc 57 as shown in FIG. 4. A screw 63 is threaded through the clamping disc 59 and bears against the pointer disc 57 so as to press the same tightly against the dial disc 52 and thereby to rotate the dial disc 52 with the pointer disc 57. By loosening the thumb screw 63 the dial disc 52 is freed for independent rotary adjustment.
The dial disc 52 has a recess 64 in its periphery. A two-circuit spring return switch 66 has an arm 67 with a roller 68 on its end in engagement with the recess 64, in the initial position of the dial disc 52, as shown in FIG. 5 The graduations 53 on the dial disc 52 are on a scale proportionate to the sheet lengths and correspond to the ratio of the reduction gearing 43 to the rate of rotation of the sprocket shaft 35 and corresponding to the unit of movement of the back-up device 11. When the dial disc 52 is loosened it is turned to the graduation indicating the selected length of sheet, and the roller 68 is pushed out of the recess 64 into circuit closing position of the switch 66. Then the pointer disc 57 is tightly clamped against the dial disc 52 so that its pointer mark 58 points to the graduation of the selected sheet length. The adjusting motion of the back-up device 11 is converted by the gear transmission 46, the flexible cable 44 and the reduction gearing 43 into rotation of the dial disc 52 of the control unit proportionate to the adjusting movement of the back-up device 11, so that when the back-up device 11 reaches the selected spaced position, the dial disc 52 is returned to its initial position and the switch roller 68 is again nesting in the recess 64 thereby opening the two-circuit switch 66. The pointer mark 58 remains pointing to the graduation indicating the sheet length to which the back-up device is adjusted.
The electrical circuit for controlling the adjustment of the back-up device is illustrated in FIG. 17. Terminals 71, 72, 73 and 74 in the switch 66 are for the circuits for adjustments in opposite directions. Terminals 71 and 72 are for operating the electric motor in a direction to move the back-up device away from the delivery conveyor 1 thereby to provide for longer sheets and this circuit is herein referred to as for "longer" adjustment. The terminals 73 and 74 are connected in a circuit for rotating the motor 37 in the opposite direction, thereby to move the back-up device closer to the delivery conveyor 1 to adjust for shorter sheets and this second circuit is herein referred to as for the "shorter" adjustment.
The terminals 71 and 73 are both connected to a line 75. For the longer adjustment, the switch 66 is shifted by rotating the dial disc 52 in the direction to connect the bridge 76 for closing the circuit through terminals 71 and 72 into the longer adjustment circuit. Thus line 75 then is connected to line 77 which is connected to one of the terminals 78 of a spring return switch 79 which latter initiates the operation of the motor by its bridge 81 bridging terminals 78 and 82 to line 83. For purposes hereinafter described, line 83 passes through terminals 84 and 86 of a spring return button switch hereinafter called "jog longer" button switch 87 and then to line 88 through the terminals 89 of a "jog shorter" spring return button switch for purposes to be hereinafter described, and then to a line 92 to the eletromagnet of an electromagnetic switch 93, thereby to energize the electromagnetic switch 93 and close the circuit of the electric motor 37 to rotate in a direction to move the back-up device away from the delivery conveyor 1 for longer sheets.
The button switch 79 operates momentarily and is spring-returned into open position so that when the button switch 79 is closed and the circuit is closed from line 77 to line 83, it energizes an auxiliary electromagnetic switch 94 which keeps the circuit between line 77 and line 83 closed as long as the switch 66 is in circuit closing position. Whenever the switch 66 is spring returned to the opening position then the auxiliary electromagnetic switch 94 is de-energized.
When the dial disc 52 is turned in the direction opposite to the previous turning then the terminals 73 and 74 are bridged by the switch 66 and connect the supply line 75 with line 96, and through the terminals 97 of the spring return button switch 79 when the latter is closed, and then through line 98 and through terminals 99 of the normally closed jog shorter button switch 91 and line 101 and terminals 102 of the normally closed jog longer button swith 87 to line 103 and to the electromagnet of the shorter switch 72 to operate the motor 37 in the opposite direction thereby to shorten the distance between the back-up device and the delivery conveyor 1. When the button switch 79 closes the bridge 81, it energizes the auxiliary electromagnetic switch 94 which remains energized as long as the switch 66 keeps the line closed between terminals 73 and 74.
The jog shorter and jog longer button switches 91 and 87 are normally in circuit closing position. For the purpose of more minute adjustments in either direction terminals 102 can be bridged by a bridge 105 by pressing the jog shorter button switch 91 whereupon the current is closed from line 85 to line 101 and terminals 102 to line 103 to the shorter electromagnetic switch 72. By pressing the jog longer button switch 87 its bridge 106 closes the circuit between terminals 104 between the supply line 75 to terminals 104 to line 88 and through terminals 89 to line 92 and to the longer electromagnetic switch 93 so as to operate the motor 37 in the opposite direction. Thus, even when the switch 66 is in the neutral position accurate adjustments can be made either to shorten or to lengthen the distance between the back-up device and the delivery conveyor 1.
The snubber assembly 13 is near the delivery end of the take-off conveyor 3 and as shown in FIGS. 6, 8, 9, and 10 it is supported on brackets 41 which are secured to the opposite side frames 42 adjacent the accelerating rollers 6. A cross-shaft 113 extends between the brackets 41 above the adjacent rollers 6. A tubular cross-bar 114 of rectangular cross section has its solid ends journalled on the shaft 113. On the cross bar 114 are spaced lugs 116 from which lugs extend snubber arms 117. On the free or lower end of each snubber arm 117 is a snubber roller 118. The cross-bar 114 has at each end thereof a perpendicular ear 119 extending both from its top and bottom thereof. Set screws 121 are threaded into plates 122 on one of the brackets 41 and bear against the adjacent ears 119 respectively. By adjusting the screws 121 as illustrated in full and in dotted lines in FIG. 9 the position of the cross bar 114 can be tilted to selected angles thereby to raise or lower the snubber rollers 118 according to the thickness of the bundle on the take-off conveyor rollers 6. In this manner the bundles are held together in spite of the accelerated movement on the rollers 6. The face of the cross-bar 114 facing toward the delivery end of the take-off conveyor 3 is provided with sheet length graduations 123 as shown in FIG. 2. A finger 124 extended from the back-up device bracket 18 adjacent said accelerated roller 6 has a pointer 125 thereon adjacent the graduations 123 to indicate the measurement to which the back-up device is adjusted.
The manner in which the snubber arms 117 are supported on the lugs 116 is illustrated in FIGS. 8 and 9. A shaft 127 is extended through the lugs 116 and a sleeve 128 is rotatable on the shaft 127 and each arm 117 is connected to one of the sleeves 128. Each sleeve 128 has a flange 129 extended upwardly and around the adjacent face of the cross bar 114 so as to limit the downward movement of the arm 117 and the snubber roller 118. Upward movement of the roller 118 and the arm 117 is permitted when the thickness of the bundle passing so requires but the weight of the roller 118 is such that it will hold the sheets bundled together.
The second snubber device 16 is above the intake end of the layboy 7 as shown in FIG. 1. The function of this second snubber device 16 is to hold the sheets in the bundle and prevent their irregular spreading while the layboy 7 is rocked to follow the rising or lowering stacker device 8.
From the stacker device base 131 extend brackets 132 from each of which extends a horizontal bar 133. Each snubber bracket 134 has a clamping device 136 whereby the bracket 134 is held stationary on the bar 133 in adjusted positions. On the inside face of each snubber bracket 134 are mounted a pair of spaced rollers 137. The side frame 138 of the layboy 7 has a guide bar 139 thereon travelling between the rollers 137 as shown in FIGS. 13 and 14. A cross-bar 141 connects the opposite snubber brackets 134 at the upper ends thereof. Adjacent the cross-bar 141 and parallel therewith is an adjusting shaft 142 which is journaled in lugs 143 extended from the cross-bar 141. The snubber arms 144 have a sleeve 146 rotatable on the shaft 142. Each snubber arm 144 has a snubber roller 147 suitably journaled at its free end for engagement with the bundles of paper passing onto the layboy conveyors 14. Adjacent each end of the adjusting shaft 142 at the adjacent snubber bracket 134 is an adjusting sprocket 148. Around each sprocket 148 is an adjusting chain 149 which chain passes over a pair of spaced sprockets 151 in opposite directions as shown in broken lines in FIG. 12. Along each adjacent face of the adjacent side frame 152 of the layboy 7 are spaced anchors 153 spaced oppositely from the respective adjacent bracket 134. The ends of the adjusting chain 149 are anchored on the respective anchors 153. As shown in FIGS. 1 and 10 the side frame 152 of the layboy 7 rides on rollers 154 on brackets 154 supported on the base of the stacker base frame. As the layboy 7 reciprocates the chain 149 idles around and with the top sprocket 148 and with the lower guide sprockets 151. The upper sprockets 148 are pinned or keyed on a cross shaft 142 which is journalled in the opposite brackets 134. On one end of the cross shaft 142 is a head 154 and on the other end of the cross-shaft 142 outside of the adjacent bracket 134 is a handle wheel 156. The position of the snubber brackets 134 is adjusted by turning the handle wheel 156 in the desired direction and then, through the chain 149 and sprockets 148 and 151, the snubber brackets 134 travel on the guide bars 139 to locate the snubber 147 in the desired position.
Each bracket 134 is tightly clamped on the bar 133 in the adjusted position by clamping means 136. The clamping means are illustrated in detail in FIG. 16. In the clamping means a U-shaped block 157 has its cavity slidably fitting on the horizontal bar 133. A cover block 158 is screwed on the legs of the U-shaped block 157 by screws 159. The cover block 158 has a threaded hole 161 therethrough. A handle 162 is provided with a set screw 163 which fits into the hole 161 so that when the set screw 163 is tightened it bears against the bar 133 and fastens the U-shaped block 157 on the bar 133. The bracket 134 has a hole therethrough fitting over a boss 166 on the back of the U-shaped block 157. A clamping washer 167 is pressed against the bracket 134 by a set screw 168 extended through the washer 167 and through the boss 166 and threaded into the hole 164 so as to tightly fasten the assembly together. In order to adjust the position of the snubber assembly 16 the clamps on both sides are loosened and the handle wheel 156 is turned which through the shaft 142 also rotates the sprocket 148 on the other side of the machine so that both chains 149 travel in unison and advance both brackets 134 in alignment whereupon the handle 162 is tightened to hold the brackets 134 in adjusted position. As shown in FIG. 1 the conveyors 14 of the layboy 7 are located in part under the accelerating rollers 6 so that the accelerating rollers 6 throw the bundles of sheets on the conveyors 14 of the layboy 7. It is important that the snubber rollers 147 engage the sheets at about the leading edges thereof. As shown in FIG. 1 the adjustment is for the narrowest board, and as illustrated in FIG. 12 the snubbers 16 are adjusted to the widest possible board or sheet.
A guard 169 is supported on brackets 171 on the side frame of the takeoff conveyor in registry with the lower of the sandwich conveyors 1. The guard 169 is inclined downwardly over the rollers 4 of the take-off conveyor 3 so as to guide the sheet toward the back-up device 11. A scraper flange 172 along the edge of the guard 169 adjacent the delivery conveyor 1 extends downwardly to scrape off material that may adhere to the adjacent lower conveyor.
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This invention pertains to the type of apparatus for handling sheets shown in U.S. Pat. No. 3,658,322 and particularly to the take-off conveyor on such apparatus on which the direction of the sheets issued from the sheet making machine is changed toward a stacker. The improvements pertain to the accurate adjustment of the back-up means on the take-off conveyor to correspond to the length of the sheets delivered from the sheet making machine thereby to allow accurate stacking of the bundles of sheets on the take-off conveyor; the adjustability is accomplished through a suitable selector dial on circuit control device which is calibrated for the length of the sheets and which when set to the particular length then through an electric circuit and driving mechanism moves the back-up abutments to that selected measurement accurately and automatically; another improvement is the adjustability of the snubber device at the discharge end of the take-off conveyor for adjustment to the thickness of the bundles of sheets; a further improvement includes adjustable snubbers on the layboy at the intake of the stacker device for adjustment to the width of the sheets for the proper transmittal of the sheets to the stacker conveyor.
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This is a continuation of application Ser. No. 752,270, filed Dec. 14, 1976, now abandoned.
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to the isomerization of dehydrolinalol (3,7-dimethyl-oct-6-en-3-olyne) of formula ##STR1## to citral (3,7-dimethyl-octa-2,6-dienal) of formula ##STR2##
2. Description of the Prior Art
U.S. Pat. No. 3,920,751 describes the isomerization of acetylenic alcohols to ethylenic carbonyl compounds in the presence of catalysts based on metals selected from the group consisting of V, Mo, W, Nb and Re. This same patent also discloses the possibility of using small amounts of co-catalysts, in particular alcohols, cyclohexanol being the compound most commonly used.
U.S. Pat. No. 3,912,250 also deals with a similar isomerization in the presence of silanyl vanadates combined with large quantities of solvents (paraffins, nitrobenzene, silicone oil and mesitylene).
Further, U.S. Pat. No. 3,912,656 discloses the same isomerization by means of silanyl vanadate combined with rather large quantities of silanol.
SUMMARY OF THE INVENTION
It is a primary object of the present invention to provide a process for the isomerization of dehydrolinalol to citral which is improved in its performance.
Another object of the invention is to provide an industrially economical process for the isomerization of dehydrolinalol.
Another object of the invention is to provide a process for the isomerization of dehydrolinalol which gives citral in improved yield.
Another object of the invention is to provide a process for the isomerization of dehydrolinalol which makes it possible to avoid the use of large amounts of solvents, which can greatly decrease the productivity of an apparatus of a given size, the productivity being the amount of reaction product obtained per unit time and per unit volume of the reactor.
Another object of the invention is to provide an isomerization process which avoids the use of relatively expensive co-catalysts, such as the silanols.
It has now been found that these objects can readily be achieved by a process which forms the subject of the present invention. This process for the preparation of citral from dehydrolinalol comprises, in its broader aspect, heating dehydrolinalol in the presence of a catalyst based on a vanadium compound and in the presence of an alkanol of 12 to 18 carbon atoms in which the alkyl moiety may be straight or branched chain, the numerical ratio ##EQU1## being between 3 and 500 and preferably between 6 and 150.
According to a narrower preferred aspect of the invention, a second co-catalyst is also present, which consists of an alkanol or cycloalkanol (optionally an alkylcycloalkanol) of from 7 to 11 carbon atoms. This second co-catalyst is present in such amounts that the numerical ratio ##EQU2## is within the limits indicated for the amount of the first co-catalyst.
DETAILED DESCRIPTION OF THE INVENTION
The catalysts based on a vanadium compound which can be used in accordance with the present invention are vanadium compounds, such as those mentioned in U.S. Pat. No. 3,920,751, the disclosure of which is incorporated herein by reference. The preferred catalysts are oxygen-containing compounds containing a group having one of the following formulae:
--V═O --O--V═O --V←O═--O--V←O═,
wherein the atom V can be joined to other atoms by ionic or covalent bonds. As the catalyst, particularly advantageous compounds are the vanadates, which may be salts or esters derived from alcohols or from silanols. The esters are often more advantageous for use than the salts. Furthermore, since dehydrolinalol and citral are known to have a tendency to instability, both in a basic and in an acid medium, it is obvious that it is advantageous to work under conditions which avoid the reaction mixture assuming an acid or basic character.
As suitable catalysts, there may be mentioned alkyl vanadates, such as methyl vanadate, ethyl vanadate, propyl vanadate, hexyl vanadate, decyl vanadate, lauryl vanadate, octadecyl vanadate, tetrahydrolinalyl vanadate; other aliphatic vanadates such as dehydrolinalyl vanadate, triethanolamine vanadate; cycloaliphatic vanadates, such as cyclohexyl vanadate; aryl vanadates, such as phenyl vandate; and silyl vanadates, such as triphenylsilyl vanadate.
The amount of catalyst is such that the weight of vanadium (in the combined state) is between 0.0001% and 5% of the weight of the dehydrolinalol and preferably between 0.01 and 2%.
As with the known processes, the process according to the invention can be carried out in the presence or absence of a solvent. If a solvent is used, it should be substantially inert so as not to react chemically with the catalyst or the reactants. In particular, they can be chlorinated or non-chlorinated aliphatic, cycloaliphatic or aromatic hydrocarbons, nitrated aromatic hydrocarbons, ethers or amides.
As the first co-catalyst suitable for use in the practice of the process according to the invention, there may be mentioned lauryl alcohol, myristyl alcohol, palmityl alcohol and stearyl alcohol, also referred to as n-dodecan-1-ol, n-tetradecan-1-ol, n-hexadecan-1-ol and n-octadecan-ol, respectively, and alkanepolyols (preferably diols).
As the second co-catalyst which may be used, there may be mentioned n-octan-1-ol, n-heptan-1-ol, n-decan-1-ol, 2-ethyl-cyclohexanol and 2-ethyl-hexan-1-ol.
The reaction temperature is generally between 50° and 300° C. and preferably between 120° and 220° C.
When the reaction is complete, the reaction product is isolated by any conventional means, generally by distillation. In the practice of the invention, it is preferred to distill the unreacted dehydrolinalol, the citral and, when present, the second more volatile co-catalyst, leaving the catalyst and the first less volatile co-catalyst as a residue which can be directly re-used for fresh isomerizations. According to a preferred technique, a flash distillation is first carried out, which gives a distillate containing the unreacted dehydrolinalol, the citral and, when used, the volatile co-catalyst, and then, in a second stage, this mixture is subjected to a fractional distillation to separate the dehydrolinalol from the citral and, when present, from the second co-catalyst.
In addition to the advantages already mentioned, the process of the invention makes it possible to obtain good yields of citral and a high degree of conversion of the dehydrolinalol (DHL).
The examples which follow are set forth to illustrate the invention. The alkanols mentioned in these examples are primary alkanols with a non-branched carbon chain but this is not to be considered as limiting the invention.
EXAMPLE 1
0.56 g of cyclohexyl orthovanadate, 20.16 g of octadecanol and 50 g of dehydrolinalol are introduced into a 125 cm 3 three-neck flask equipped with a nitrogen inlet and a distillation column. The mixture is rapidly heated to 160° C., with stirring and is then maintained at this temperature for 25 minutes, after which it is cooled to 60° C. and distilled under a reduced pressure of 0.3 mm Hg, while heating the reactor to 130° C. The process is repeated twice, each time introducing 50 g of DHL into the distillation residue and then heating at 160° C. for 25 minutes, and then seven more times, each time introducing 50 g of DHL into the residue of the preceding distillation and heating at 165° C. for 25 minutes. The amount of dehydrolinalol and citral present in the distillate is determined in each instance.
The following table in which DC denotes the degree of conversion of the dehydrolinalol and Y denotes the yield of citral relative to the dehydrolinalol converted shows the results obtained in each operation:
TABLE 1______________________________________Operation No. Temperature DC Y______________________________________1 160° C. 14% 96%2 160° C. 15% 98%3 160° C. 16% 91%4 165° C. 24% 99%5 165° C. 21% 97%6 165° C. 24% 96%7 165° C. 26% 96%8 165° C. 23% 91%9 165° C. 24% 100%10 165° C. 23% 96%______________________________________
EXAMPLE 2
1.28 go of octadecyl orthovanadate, 19.13 g of octadecanol and 50 g of dehydrolinalol are introduced into a 125 cm 3 three-neck flask equipped with a nitrogen inlet and a distillation column. The mixture is rapidly heated to 165° C., with stirring and is then maintained at this temperature for 25 minutes, after which it is cooled to 60° C. and distilled under a reduced pressure of 0.3 mm Hg, while heating the reactor to 130° C. The dehydrolinalol and the citral are determined in the distillates.
The process is repeated several times, under varying conditions of reaction temperature and time. The results obtained in accordance with this example are reported in the following table:
TABLE II______________________________________ Reaction Duration ofOperation No. temperature the reaction DC Y______________________________________1 165° C. 25 mins. 19% 94%2 165° C. 40 mins. 29% 96%3 165° C. 25 mins. 19% 96%4 175° C. 25 mins. 37% 93%5 175° C. 30 mins. 46% 90%6 165° C. l hr. 33% 96%______________________________________
EXAMPLE 3
0.53 g of cyclohexyl orthovanadate, 6.72 g of octadecanol, 50 g of dehydrolinalol, and 10 cm 3 of paraffin oil of high boiling point are introduced into a 125 cm 3 three-neck flask equipped with a nitrogen inlet and a distillation column. The mixture is rapidly heated to 150° C., with stirring and is then maintained at this temperature for 25 minutes, after which it is cooled to 60° C. and distilled under a reduced pressure of 0.3 mm Hg, while heating the reactor to 130° C. The process is repeated four times by introducing a further 50 g of DHL into the preceding distillation residue and then heating at 160° C. for 30 minutes. The dehydrolinalol and the citral are determined in each of the distillates.
The results of this example are set forth in the following table:
TABLE III______________________________________Operation No. Temperature DC Y______________________________________1 150° C. 10% 89%2 160° C. 21% 95%3 160° C. 23% 91%4 160° C. 21% 91%5 160° C. 25% 90%______________________________________
EXAMPLE 4
Operating as described in Example 3 but using 0.53 g of cyclohexyl orthovanadate and 10.6 of tetradecanol, results are obtained as set forth in the following table:
TABLE IV______________________________________ Reaction Duration ofOperation No. temperature the reaction DC Y______________________________________1 160° C. 25 mins. 19% 92%2 160° C. 25 mins. 22% 94%3 160° C. 25 mins. 22% 95%4 160° C. 25 mins. 22% 95%5 160° C. 33 mins. 28% 94%______________________________________
EXAMPLE 5
1.28 g of octadecyl orthovanadate and 20.16 g of octadecanol are introduced into a 100 cm 3 flask which is equipped with a dropping funnel, an argon inlet, a distillation column and a stirrer, with provision for connection with a vacuum pump, and the mixture is then heated at 180° C. while reducing the pressure to 150 mm Hg. A first quantity of 20.32 g of dehydrolinalol is run in over 1 hour 15 minutes and, at the same time, the volatile products are distilled. The reactor is then heated to 200° C. under a reduced pressure of 100 mm Hg, after which a second quantity of 20.46 g of dehydrolinalol is run in over 1 hour and 20 minutes and, at the same time, the volatile products are distilled. Thereafter the reactor is cooled and volatile products are then removed at 140° C. under a reduced pressure of 0.1 mm Hg. Analyses carried out on the distillate showed that the degree of conversion of the dehydrolinalol (DC) is 30% and the yield (Y) of citral is 82%. 5.01 g of DHL are introduced into the distillation residue and the whole is heated to 200° C. for 25 minutes and then cooled. The volatile product is removed by distillation carried out at 100° C. to 140° C. under a reduced pressure of 0.1 mm Hg. The degree of conversion (DC) of the dehydrolinalol is 94% and the yield of citral (Y) is 92%. The same operation is carried out a second time, introducing 5.12 g of dehydrolinalol, and the degree of conversion of the dehydrolinalol is found to be 95% and the yield of citral 82%. On introducing a further 5.08 g of dehydrolinalol and heating at 200° C. for 15 minutes, the degree of conversion of the dehydrolinalol is found to be 78%, and the yield of citral 93%.
EXAMPLE 6
0.56 g (1.54×10 -3 mols) of cyclohexyl orthovanadate, 4.65 g of dodecanol and 50.02 g of dehydrolinalol are introduced into a 125 ml three-neck flask equipped with a nitrogen inlet and a distillation column. The mixture is rapidly heated to 160° C., with stirring, and is kept at this temperature for 25 minutes. It is then cooled to 30° C. and the volatile products are distilled under a pressure reduced to 0.5 mm Hg. The distillate (49.56 g) is analyzed and found to contain 41.0 g of dehydrolinalol and 8.2 g of citral. The degree of conversion of the dehydrolinalol is 18% and the yield of citral relative to the dehydrolinalol which has disappeared is 91%.
EXAMPLE 7
1.27 g (1.45×10 -3 mols) of octadecyl orthovanadate, 1.18 g (4.35×10 -3 mols) of octadecanol, 7.34 g (5.7×10 3 ) mols) of octanol and about 50 g of dehydrolinalol are introduced into a 125 cm -3 three-neck flask equipped with a nitrogen inlet and a distillation column. The mixture is rapidly heated to 160° C. and is kept at this temperature for 25 minutes. It is then cooled to 60° C. and the volatile products are distilled under a pressure reduced to 0.3 mm Hg; the distillation residue is heated to 130° C. and then cooled. About 7.4 g of octanol and about 50 g of dehydrolinalol are again introduced and the operation is repeated four times.
The dehydrolinalol and the citral are determined in the distillates, and the following table shows the results obtained:
TABLE V______________________________________ DHL OctanolOperation No. introduced introduced DC Y______________________________________1 49.91 g 7.34 g 14% 93%2 50.10 g 7.43 g 15% 93%3 50.11 g 7.30 g 15% 95%4 50.18 g 7.28 g 17% 93%______________________________________
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Citral is prepared by heating dehydrolinalol in the presence of a vanadium compound as catalyst and an alkanol of 12 to 18 carbon atoms as co-catalyst, whereby isomerization is effected. There may also be present an alkanol or cycloalkanol of 7 to 11 carbon atoms as co-catalyst.
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The invention relates to a device and method for controlling and/or monitoring a yarn processing system.
BACKGROUND OF THE INVENTION
When controlling and/or monitoring a yarn processing system a plurality of actively initiated or spontaneous actions or reactions, so-called events, takes place at and/or in different components or functional units which events are triggered and carried out by differing signals and/or which are confirmed by differing signals, respectively. An optimum course of the performance of the yarn processing system only results from a functional co-action between and with a correct timewise sequence of the events.
The main control of the textile machine and at least the control devices of the feeding devices are interconnected by a communication network having the form of a serial communication field bus system comprising one or several field buses for the transmission of signals built into messages. In this case the network can be formed with so-called T-connectors or like a “daisy-chain”. Since prioritised events exist, e.g. time critical and/or time specific events, and secondary, less time critical and/or less time specific events, the communication in the field bus system is carried out e.g. by messages which are prioritised by special message types, in order to carry out and/or to confirm the prioritised events without delay. The immense data flood within a complex yarn processing system may lead to the disadvantage that prioritised events cannot be carried out and/or confirmed at the right time with the field bus system.
In earlier known yarn processing systems in which the components or at least a majority of the components were interlinked functionally with each other, a separate signal line was provided for each type of signal. This resulted in complicated cabling and in considerable efforts when processing and/or conditioning the signals.
SUMMARY OF THE INVENTION
It is an object of the present invention to provide a device and a method as mentioned which allow to optimise the definition and the safety for the transmission times of time specific and/or time critical messages or signals in yarn processing systems, and to simplify the synchronisation between the different functional units and the components within the system. In the case of an air jet weaving machine constituting the textile machine of the yarn processing systems such time critical signals would e.g. be the trig signals sent from the weaving machine to the yarn stopping accessory device of each yarn measuring feeding device, or the so-called yarn winding pulses which are to be transmitted to the weaving machine from a winding sensor monitoring the withdrawal of the yarn from the yarn measuring feeding device. In the case of a rapier weaving machine or a projectile weaving machine, respectively, constituting the textile machine, e.g. time critical messages or signals would be the trig signals for controlling the respective controlled yarn tensioning accessory devices provided at the exit sides of the yarn feeding devices.
Summarised, it is an object of the present invention to provide a device and a method as mentioned above allowing to optimally operate even complex yarn processing systems to which a field bus system is associated in view to working speed and to the reliability of the operation with a simple cabling only and so that time critical and/or time specific events are carried out and/or confirmed at the correct time during the operation and for all operation conditions, i.e. also in case of an otherwise extremely large data flood occurring in the communication network.
According to the invention, the event signals are transmitted in real time via the at least one separate event line. The event signals may be simple, fast and short signal pulses. This at least largely excludes the danger of a mutual collision of event signals or the delay of an event signal, respectively. The event line has to transmit only the event signals at the right time and as rapidly as possible from at least one respective sender to at least on respective receiver. The event specific characteristic which belongs to the event signal is transmitted in advance within the field bus system to at least one participant in the communication system in order to define the per se anonymous event signal for the one or several concerned participants in an evaluative fashion. The definition is made by software. Since the event signal and its event specific characteristic are transmitted along separate paths and first are combined at the addressed participants into a meaningful signal, into a command or into a confirmation, the yarn processing system can be controlled and/or monitored optimally. There is sufficient time available for the transmission of the event specific characteristic which is provided in advance within the field bus system in order not to overload the field bus system even in case of a large data flood. The transmission of the event signals along the event lines is not affected in case of a large data flood within the field bus system. The field bus system communicates essentially on a continuous time basis, while events signals are individually transmitted in real time. By means of the different messages communicating within the field bus system, so to speak, the function of the event line is continuously reconfigured or changed during the operation of the textile machine. Although there is essentially only one event line this event line fulfils in this way the task of many signal lines which were needed otherwise for each sort of the events.
This is possible, because there is at least one or there are several specific event lines in addition to the field bus system as the function of a bidirectional digital signal transmission between the textile machine and at least the yarn feeding devices, in which case the transmitted event signals are messages having a time critical or time specific character, so-called event synchronous signals. This may e.g. be trig signals for initiating or carrying out certain and predetermined functions in the yarn feeding devices and the accessory devices of the yarn feeding devices, or in respective accessory devices of the textile machine. These event synchronous signals even may be feedback signals e.g. for confirming initiated and carried out events or indications of the status of specific conditions, functions or components within the yarn processing system, etc.
In a preferred embodiment of the device according to the invention the actual function of the at least one event synchronous line may be defined or configured in relation to time, expediently on a continuous time basis. This is done by means of information of a serial type. This information is sent within the at least one serial field bus which interlinks the textile machine, the yarn feeding devices, and in some case, the accessory devices as provided. The actual function of the event synchronous line is meant to be its intended function at a certain point in time or during a certain time period. This function e.g. may consist of information on the actual type of the next event which is associated to the event signal sent in the at least one event line, and of address information related to the next event signal, i.e. to which or from which node or to which and from which node of the yarn feeding devices/accessory devices the next event signal has to go or has to come.
In other words the field bus system is used to associate a certain function to the at least one event line. The field bus system is apt to continuously vary or subsequently actualise this association of the function in an easily controlled fashion by means of the at least one field bus. The consequence of these capabilities is that the event line continuously is prepared to transmit each occurring time critical and/or time specific event signal precisely and directly at the moment at which it is needed. In this way a completely time-safe control of the yarn processing system can be achieved.
The at least one event line in the yarn processing system is a bidirectional, direct digital line having the purpose of transmitting pulses which indicate events. These pulses indicating an event will be defined in the preferred embodiment by a serial information communication via the field bus system. Bidirectional has the meaning that each node within the system is allowed to use the event line in order to both send or receive event signals (and to read the same).
The function of the event line which, as mentioned, varies in time, is defined or configured by means or via the serial communication field bus system which e.g. has a CAN-bus operating with a CAN-protocol. The field bus of the field bus system contains serial type information related to the type of an upcoming event which will show up in the form of the next event signal on the event line, and also information for which specific node or specific nodes this special event signal is intended, or from which node or nodes it may come. The field bus even may indicate a number of such events such that then this number will be considered by one or by several of the nodes, or the field bus may define a number of events which will happen during a subsequent certain period of time, or until a new definition of the function takes place, which then will erase or substitute the preceding definition of the function.
The structure of the communication system according to the invention allows to configure and vary the function of the event line during the operation of the textile machine. A possible delay time for the consideration of the event signal or for carrying out the event after the transmission of the event signal may even be defined and pre-calculated as soon as the function is defined.
The connecting structure of the at least one event line either is a so-called point-to-point-structure or a multi-drop-structure. In terms of hardware a point-to-point-structure means that e.g. only one event line intended for several events extends to each yarn feeding device. In this single event line an individual event signal driver is provided. Within the multi-drop-structure a single event signal driver is needed only, since there is only one event line to which all yarn feeding devices or other participants are connected.
Within a yarn processing system comprising an air jet weaving machine it will be important time critical events for the weaving machine to start the yarn withdrawal in the respective correct moment, to monitor the number of the yarn windings withdrawn from the respective yarn feeding device, and, finally, to terminate the yarn withdrawal at the respective yarn feeding device. According to the invention this may be realised as follows:
1. At first the weaving machine sends via the field bus, e.g. a CAN-bus, a message which associates the function for a trig signal to the event line. This means that the next following event signal transmitted in the event line has to be a trig signal for a certain event.
2. In the next moment the next following sent CAN-message defines a specific yarn feeding device within the yarn processing system in order to instruct the magnet provided in the yarn stopping accessory device of this yarn feeding device to lift the yarn stopping pin after the expiration of a number of x milliseconds which will be counted upon the transmission of the next following event signal in the event line. This event signal then will be the trig signal according to 1.
3. As soon as the event signal or the trig signal, respectively, is transmitted in the event line the event (the lifting of the yarn stopping pin) will be carried out then when the number x in milliseconds has been counted or when the corresponding period of time has expired.
4. The next following CAN-message gives the same event line the function for the yarn winding pulses of a specific yarn feeding device which yarn winding pulses represent the number of the windings withdrawn. Then the yarn feeding device uses the event line to send these yarn winding pulses which will be monitored and considered by the main control of the weaving machine thanks to the definition given beforehand.
5. After the correct number of the yarn winding off pulses stemming from the selected yarn feeding device has been considered, a further CAN-message again gives the event line the function for a trig signal.
6. The next following CAN-message defines the event which has to be carried out for the related yarn feeding device which is the returning or closing of the yarn stopping pin after the expiration of a number of y milliseconds which will be counted upon occurrence of the next following event signal in the event line (this event signal will be a trig signal according to 5.).
7. In the same moment the feeding device control device of the related yarn feeding device is reading the event signal or trig signal occurring in the event line such that the yarn withdrawal is terminated in accordance with the conditions as defined in 6., i.e., as soon as after the transmission of the event signal the number of y milliseconds has expired. One cycle of a weft yarn insertion (one pick) now has taken place in a correct and time-safe fashion.
The core of the invention is to use for different events only at least one event line in order to transmit the event signals in the simplest form and as rapidly as possible, and to define in advance and by software the event line or the respective event signal, respectively, via the field bus system in order to allow to use it for the respective participant. By a definition in advance of the respective expected event signal which definition in advance varies during the operation of the yarn processing system, the event signals related to differing events can be transmitted on the same event line because they will be specifically identified by the addressed participants in the communication systems due to the definition in advance. The field bus system is well adapted for this identification and has sufficient time for the identification, because it is kept free from the task to transmit the event signals at the correct time or in real time.
Expediently an individual point-to-point-event line for different events is provided between the textile machine and at least each yarn feeding device, preferably with one event signal driver per event line. The event signals will be transmitted along each of these event lines which only then will be associated by the definition via the field bus system to the different events.
Alternatively only a single, common multi-drop-event line is provided between the textile machine and at least the yarn feeding devices, preferably having one common event signal driver.
In the case that at least one accessory device is associated to at least one yarn feeding device, which accessory device can be controlled and/or monitored by the feeding device control, then the accessory device directly may be connected to the event line, or indirectly via the feeding device control. In the case that, to the contrary, at least one accessory device is associated to at least one yarn feeding device, which accessory device has an electronic accessory device control and/or accessory device monitoring, then the accessory device directly may be connected to the event line, or indirectly via the feeding device control. The connection of the accessory device to the field bus system may be made analogously direct or indirect.
In the case that at least one accessory device is associated to the textile machine which accessory device can be controlled or monitored either from the main control or from an individual electronic accessory device control, then the accessory device also may be connected directly to the event line, or indirectly via the main control.
The respective event signal is at least one signal pulse. The events signals for different events may be identical among themselves since they receive their respective meaning first by the definition via the field bus system.
Expediently, the participants of the communication are connected to nodes having addresses. Alternatively, the communication participants may have individual addresses in the field bus system. This simplifies the respective definition in advance of each event signal for the communication participants.
Expediently, the characteristic of the event signal by which the event signal will respectively be defined in advance, may be transmitted for each transmission direction in the event line in each communication direction within the field bus system.
The following characteristics may be defined individually or in combination within the field bus system. Only a selection of different possibilities will be explained:
the type of the event represented by the event signal, the address and/or node address of at least one sender and/or receiver of the event signal among the communication participants, the expected point in time of the event and/or a time window and/or a time period for the event or until the event will happen, the number of events to be expected at one or at several nodes, and a delay time duration which is to be considered respectively between the transmission of the event signal and the initiation and/or confirmation of the event, the consequence of the one or the several event signals which are transmitted at a certain point in time and/or within a determined time window from or to a determined address, and the like.
The signal types which are associated to the event in the yarn processing system (not limiting, only an exemplary listing) may be:
an actuating or de-activating trig signal for a yarn stopping accessory device of a yarn feeding device, a yarn winding count signal of a counting accessory device of a yarn feeding device, a trig signal for actuating or de-activating a yarn stretching accessory device of a yarn feeding device located at an exit of the yarn feeding device, a trig signal for activating, de-activating or adjusting a controlled yarn braking accessory device within the yarn path, a signal of a weft yarn detector accessory device or a yarn breakage detector accessory device along the yarn path which is to be expected at a predefined point in time or within a predefined time window, an event confirmation signal, an event inhibition signal, a status signal of at least one communication participant which is to be expected or which is to be asked for at a predetermined point in time or within a predetermined time window, etc.
According to the method the respective event signal may be defined such that it can be used from at least one addressed communication participant, even if the event signal is transmitted on the event line to several participants. When defining the event signal the addressed communication participant is informed which event is meant by the next following event signal. Alternatively, the communication participant is informed about an expectation point in time or a time period or a time window, and, in some cases, about at least one sender address belonging to the event signals.
BRIEF DESCRIPTION OF THE DRAWINGS
Embodiments of the invention will be described with the help of the drawings, in which:
FIG. 1 is a schematic illustration of a yarn processing system, and
FIG. 2 is a detailed schematic illustration of a yarn processing system.
DETAILED DESCRIPTION
In the following yarn processing systems will be described having a respective weaving machine as a textile machine and also having weft yarn feeding devices as feeding devices. However, the invention also can be employed for other yarn processing systems such as e.g. a knitting machine and knitting yarn feeding devices.
A yarn processing system S in FIG. 1 includes a textile machine M having an electronic main control MCU and several yarn feeding devices F 1 , F 2 , F 3 to Fn. Furthermore, a field bus system FBS is provided including at least one field bus FB which interconnects the main control MCU and the yarn feeding devices F 1 to Fn, the latter expediently via yarn feeding device controls FC. At least one field bus driver FBD for a bidirectional serial data transmission is provided within the field bus system FBS. Separate from the field bus system FBS an event line EL is provided to which all yarn feeding devices F 1 to Fn and the main control MCU are connected either directly or via the field bus FB. An event signal driver ELD is provided for the event line EL. As indicated by arrows in the respective blocks the event line EL serves for signal transmissions in each transmission direction.
The method for controlling and/or monitoring the yarn processing system S in FIG. 1 is explained with the assumption that the textile machine M is an air jet weaving machine and that the associated yarn feeding devices F 1 to Fn are so-called weft yarn measuring feeding devices, each having a yarn stopping accessory device. Furthermore, a further accessory device in the form of a so-called winding count sensor (not shown) is arranged at each yarn feeding device which sensor counts during each insertion a withdrawn yarn winding and generates at least one signal then. A magnet is arranged within the yarn stopping accessory device for lifting a not shown yarn stopping pin out of the yarn path. The stopping pin can be returned from the lifted position again into the lowered position by spring load or by the magnet, respectively. In the lowered position of the yarn stopping pin the yarn withdrawal is interrupted. In the lifted position of the yarn stopping pin the yarn windings are withdrawn one by one by the air jet weaving machine.
An insertion in the yarn channel occupied by the yarn feeding device F 3 is controlled and monitored as follows:
1. The air jet weaving machine sends a message via the field bus FB (e.g. a CAN-bus) which associates the function for a trig signal to the event line EL. This means that the subsequent event signal will be a trig signal for a certain event, namely for lifting the yarn stopping pin in the yarn feeding device F 3 .
2. In the next moment the next sent e.g. CAN-message defines the yarn feeding device F 3 in the yarn processing system. The message gives the order that the magnet has to lift the yarn stopping pin x milliseconds after the occurrence of the subsequent event signal in the event line. Consequently, this event signal will be the trig signal according to 1.
3. As soon as the event signal is transmitted via the event line EL, the event or the function according to 2, will be carried out, as soon as x milliseconds have expired.
4. The next e.g. CAN-message associates winding counting pulses from the yarn feeding device F 3 to the event line EL. During withdrawal of the yarn the winding count accessory device generates yarn minding pulses which are sent by the yarn feeding device F 3 into the event line EL. These yarn winding pulses are monitored and registered by the main control MCU of the air jet weaving machine.
5. After a predetermined, correct number of yarn winding off pulses originating from the yarn feeding device F 3 have been monitored and counted, a new sent e.g. CAN-message will associate the event line EL again to a trig signal.
6. The next following e.g. CAN-message defines for the yarn feeding device F 3 that the accessory device of the yarn feeding device F 3 has to lower or close of the yarn stopping pin y milliseconds after the occurrence of the next following event signal in the event line as the event. This event then will be the trig signal according to 5.
7. Immediately after this point in time the yarn feeding control FC in the yarn feeding device F 3 reads the incoming event signal in the event line EL as a trig signal. The yarn withdrawal is terminated in accordance with the condition defined in 6, i.e., as soon as y milliseconds have expired upon occurrence of the event signal. One cycle of the weft yarn insertion (one pick) then has taken place in the correct fashion and with a proper timing.
In the yarn processing system in FIG. 2 an air jet weaving machine is indicated as the textile machine M to which at least two yarn feeding devices F 1 , Fn are associated in separated yarn channels. The air jet weaving machine has a weaving shed 1 , an insertion and yarn selecting assembly 2 , and a main shaft 3 , of which the rotational angle ranges or rotational angles are monitored in coded fashion by the main control MCU. Furthermore, e.g. at the side of the weaving shed remote from the yarn feeding devices an accessory device A in the form of an arrival sensor is provided which confirms the arrival of the free weft yarn tip e.g. by an okay signal and/or which generates a fault signal in case that the free tip of the weft yarn has not arrived at a predetermined point in time or within a predetermined time window, respectively.
Each yarn feeding device F 1 , Fn is a so-called weft yarn measuring feeding device which measures the weft yarn length for each insertion. A housing 4 supports a storage drum 5 . Furthermore, at the inlet side an accessory device E in the form of a yarn breakage detector or yarn run detector is provided and connected to the yarn feeding device control FC. Furthermore, a yarn stopping accessory device D is provided and connected to the yarn feeding device control FC. Finally, even an accessory device B in the form of a yarn winding count sensor may be oriented the storage drum 5 which sensor generates at least one count signal for each withdrawn winding and transmits the count signals to the yarn feeding device control FC. The accessory device D has at least one magnet by which a yarn stopping pin can be lifted from a lowered stopping position (stopping the yarn against withdrawal) into a release position (releasing the yarn for withdrawal), and which then can be returned.
At the withdrawal side of the yarn feeding device an accessory device G in the form of a yarn stretcher may be provided which, in some cases, may be connected to the yarn feeding device control FC. In the further course of the yarn path an accessory device H in the form of a controlled yarn brake having an individual accessory device control AC may be provided. Furthermore, a weft yarn monitor may be arranged as an accessory device K within the yarn path.
Each yarn feeding device F 1 to Fn pulls off yarn from a storage bobbin 7 provided in a storage bobbin stand 6 . At the stand, as well, accessory devices (not shown) may be provided for monitoring and/or controlling certain functions.
A serial communication system in the form of a field bus system FBS interconnects the main control MCU and the yarn feeding devices F 1 , Fn by means of at least one field bus FB. The yarn feeding device controls FC either are connected directly to the field bus FB (not shown), or, as shown, via a so-called yarn feeding device control box FCB. Even the stand 6 , the accessory devices H, K and in some cases the accessory device A may be connected to the field bus FB. For such purposes nodes are provided which have predefined addresses.
Accessory devices associated to at least one respective yarn feeding device may be connected to the respective yarn feeding device control FC. Accessory devices associated to the textile machine, to the contrary, may be connected to the main control MCU. The field bus system FBS contains at least one common field bus driver FBD by which the transmission of messages NES is carried out in both transmission directions within the field bus system FBS.
Separate from the field bus system FBS one event line EL is arranged in a multi-drop structure, to which different communication participants of the field bus system FBS are connected. The event line EL serves for the transmission of event signals ES at the correct time or in real time, respectively, and selectively in each transmission direction. In this case the event signals ES may be relatively simple signal pulses. The feeding device controls FC are directly connected to the event line EL, while the accessory devices E, D, B, G are connected to the event line EL via the feeding device controls FC. Differently, the accessory devices H, K, A and also the main control MCU, are directly connected to the event line EL. Even not shown accessory devices at the stand 6 may be connected to the event line EL.
In a not shown alternative individual point-to-point-event lines may be provided to the respective communication participants in the field bus system FBS. Then each event line is equipped with an individual event signal driver ELD.
An insertion cycle for one weft yarn of the yarn feeding device F 1 is controlled and monitored in the fashion as explained with the help of FIG. 1 . The further accessory devices are controlled and/or monitored in analogous fashion.
The indirect definition of an event signal which will be generated in the form of a fault signal from the accessory device A (arrival sensor) in case of a not arriving weft yarn is carried out e.g. in the following way:
The main control MCU is informed by the yarn winding count pulses about the movement of the weft yarn through the weaving shed. The point in time of or a time window for the arrival of the free weft yarn tip at the accessory device A is known. By a corresponding message NES in the field bus system FBS e.g. after receipt of the first yarn winding count pulse it is defined that an event signal transmitted at the predefined point in time or within the predefined time window will be a fault signal from the accessory device A and will have the consequence that the weaving machine has to be switched off. In case that the event signal is transmitted at the predefined point in time or within the predefined time window, the main control MCU will switch off the weaving machine.
In a similar way an event signal transmitted during an insertion cycle from a weft yarn monitor (accessory device K) will be recognised as representing the event of a yarn breakage or a yarn stop caused by a fault and will be registered such that at least the weaving machine will be switched off.
In this case e.g. the signal of the weft yarn monitor upon start of the yarn within a time window will be defined via the field bus system as an expected event signal from the node addressed to the main control MCU. Furthermore, the consequence of the receipt of this event signal will defined. In case that the event signal will be received as an okay signal, nothing will be done. In case that the event signal does not arrive, a determination is made that a yarn breakage has occurred, and the machine will be switched off. As a definition also an inquiry for at least one event signal may be carried out at the predetermined point in time or within a time window, respectively.
The activation or deactivation or adjustment of the accessory device H e.g. is made by communicating the message via the field bus system FBS that the next following event signal is intended for the node address of the accessory device H only and has to be ignored by all other communication participants.
In a very complex system a point-to-point-structure of several event lines may be more expedient in order to allow to handle as many as possible event signals at the appropriate time.
In the case of a rapier weaving machine as the textile machine of the yarn processing system, e.g. the controlled yarn brake is actuated as the accessory device by defining by the node address of the yarn feeding device control of the operating yarn channel or by the node address of the controlled yarn brake in the field bus system at which point in time the respective event signal for the activation will arrive and at which point in time the event signal for the deactivation of the controlled yarn brake will arrive. In this case the points in time or the time windows e.g. are associated to the rotational angle of the main shaft of the weaving machine by calculations or the like and also the event signals will be transmitted depending therefrom. In this way it is assured that the yarn tension will be increased accordingly when the bringer gripper grips the yarn, so that then the yarn tension will be decreased, so that the yarn tension again will be increased, as soon as the bringer gripper transfers the yarn to the taker gripper, and so that the yarn tension again will be decreased after the transfer.
In case of a projectile weaving machine the controlled yarn brake similarly will be activated and deactivated by using respective event signals. In this case the purpose and the point in time or the time window of the event signals are transmitted in advance to the respective correct addresses by messages within the field bus system.
In a similar way also in other yarn processing systems which e.g. include a knitting machine and knitting yarn feeding devices associated to the knitting machine and, in some cases, accessory devices, may be controlled and/or monitored with event signals the meaning of which will be respectively defined via the field bus system.
Although a particular preferred embodiment of the invention has been disclosed in detail for illustrative purposes, it will be recognized that variations or modifications of the disclosed apparatus, including the rearrangement of parts, lie within the scope of the present invention.
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A device for controlling and monitoring a yarn processing system, which comprises an electronic main control unit and at least one yarn feeding unit, and inside of which a serial communications field bus system is provided with at least one field bus for carrying out communication. At least one bi-directional event line is provided outside the field bus system in order to transmit a time critical and/or time-specific, digital and anonymous event signal for carrying out and/or confirming events. For at least one communication participant connected to the field bus system, an event specific characteristic feature of respective event signal can be defined by the software side configuration inside the field bus system.
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BACKGROUND OF THE INVENTION
The invention relates to a receiver for receiving data from a differential data bus with two lines which can detect a positive and a negative level on the bus lines.
Such receivers usually have two resistive input branches, which are used to weaken the input signals from the data bus. According to solutions in the state of the art, two voltage sources in combination with two comparators are used for detecting the two levels. The exact detection levels are mainly defined by the voltage sources. If the voltage sources do not deliver exactly the same voltage, witch can easily occur in practice, the positive and negative detection levels are not equal, which should be avoided.
It is an object of the invention to provide a receiver for a differential data bus which ensures symmetrical detection levels of positive and negative signals.
This object is achieved by the receiver having the features according to claim 1 :
Receiver for a differential data bus with two resistive branches, with a differential amplifier with two transistors, with a resistor, and with a control logic that controls a switch with which a current from a current source is switchable to either side of the resistor, which resistor couples the two transistors, and with two operational amplifiers which are coupled to the two transistors of the differential amplifier with opposite poles, in which receiver the control logic detects from the output signals of the two operational amplifiers whether a “0” or a “1” is expected on the bus and which receiver sets the switch accordingly so that a comparison with the received bus signal is made.
The receiver according to the invention uses only one voltage source instead of two in order to avoid level mismatches. This one voltage source is realized with one current source and one resistor. By switching the resistor between two branches of a differential amplifier this voltage source can be used for detecting a positive level on one line and a negative level on the other line, or vice versa. This ensures an absolutely symmetrical detection of levels of the two polarities, which has the consequence of a very low jitter.
The control logic puts the switch with which the current is switched on either side of the differential amplifier in accordance with the falling edge last received.
According to the advantageous measures of claim 2 , two transistors can be used as the differential amplifier, thus providing a simple circuitry.
BRIEF DESCRIPTION OF THE DRAWINGS
The invention will be further described with reference to the drawings, in which:
FIG. 1 is a schematic block diagram of an embodiment of a receiver according to the invention with only one voltage source used for the detection of positive as well as negative levels, and
FIG. 2 is a timing diagram of the receiver according to FIG. 1 with several bits received from the data bus.
DETAILED DESCRIPTION
The schematic block diagram of FIG. 1 shows a receiver for a differential data bus with two lines bm and bp. As this bus works with differential signals, the signals always have opposite polarities, if the bus is not disturbed. The bus may be, for example, one according to the FlexRay standard.
FIG. 1 shows that the input stage of the receiver is provided with two branches with resistive dividers, which are used to accommodate high common input voltages.
The first divider comprises three resistors 4 , 5 and 6 in series. Resistor 4 is coupled to the line bp of the bus. The second divider comprises three resistors 1 , 2 and 3 , also in series, of which resistor 1 is coupled to the other line bm of the data bus.
The connection between resistor 1 and resistor 2 is coupled to the input of an inverter 7 , whose output is coupled to a connection between resistors 3 and 6 . In the same way a second inverter 8 is coupled to the connection between resistors 4 and 5 and the connection between the last transistors 3 and 6 of the dividers.
The connection between the resistors 5 and 6 is coupled to the base of a first bipolar npn-transistor 9 , while the connection between the transistors 2 and 3 is coupled to the base of a second bipolar npn-transistor 10 .
The collectors of the transistors 9 and 10 are coupled via current sources 11 and 12 to a power source V+ with positive voltage.
The emitters of the two transistors 9 and 10 are coupled via a resistor 13 which, together with a current source 14 , forms a voltage source which is used for detecting positive and negative levels, as will be explained below. The two transistors 9 and 10 and the resistor 13 form a differential amplifier.
The current source 14 can be switched to either side of the resistor 13 by a switch 15 , which is controlled by a control logic 16 .
The data outputs are realized by a second comparator 17 and a first comparator 18 , which deliver the output signals RXD 1 and RXD 0 .
The negative input of the second comparator 17 and the positive input of the first comparator 18 are coupled to the collector of the second transistor 10 , while the positive input of comparator 17 and the negative input of comparator 18 are coupled to the collector of the first transistor 9 .
As already mentioned, instead of using two separate voltage sources, one voltage source is formed with one resistor 13 and one current source 14 . The switch 15 serves to determine whether a positive or a negative differential voltage has to be detected.
The control logic 16 detects only the falling edges of the output signals RXD 0 and RXD 1 . A falling edge of RXD 0 causes the control logic 16 to set the switch 15 to a second position, in which the current source 14 is coupled to the emitter of transistor 10 , whereas a falling edge of RXD 1 causes the control logic 16 to set the switch 15 to a first position, in which the current source 14 is coupled to the emitter of transistor 9 .
With reference to the timing diagram in FIG. 2 , it will now be explained how the receiver according to FIG. 1 works when data bits appear on the bus. The timing diagram shows the voltages of several signals in the receiver.
The first two signals in FIG. 2 are the bus signals bm and bp on the bus lines. As this is a differential bus, for example a bus according to the FlexRay-standard, the signals bm and bp have opposite polarities.
The next two signals in the diagram are the signals V 1 and V 2 . These are bus signals bm and bp which have been weakened by input dividers formed by the resistors 1 to 6 . The signals V 1 and V 2 are applied to the bases of the transistors 9 and 10 , respectively.
The next two signals show the voltages at the collectors of the transistors 9 and 10 .
The last two signals are the output signals RXD 1 and RXD 0 of the comparators 17 and 18 and of the receiver.
In the timing diagram of FIG. 2 , RXD 0 first is negative, so that a falling edge (not shown) must have appeared in this signal last. That is why the control logic had set the switch 15 in the second position. Now a falling edge appears in bm and a rising edge in signal bp. Consequently, the same edges appear in the weakened versions V 1 and V 2 of these signals. As V 2 is coupled to the base of the transistor 9 , this transistor switches and the potential at its collector falls, as can be seen in the timing diagram. At the same time V 1 shows a falling edge, so that transistor 10 closes and the potential at its collector shows a rising edge. This has the consequence that the level of the output signal RXD 1 changes from high to low, whereas the output signal RXD 0 goes from low to high.
The fact that the signal RXD 1 shows a falling edge causes the control logic to set the switch 15 to the first position, in which the current source 14 is coupled to the emitter of the second transistor 9 , as now a falling edge in the signal bm is expected.
The timing diagram shows that in fact at the next transition the signal bp changes from high to low and that signal bm from low to high. This time, the transistors 9 and 10 are switched to the opposite positions, so that the potential at the collector of transistor 9 goes up and that at the collector of transistor 10 goes down. Consequently, the signal RXD 1 shows a rising edge and RXD 0 shows a falling edge this time, so that the control logic 16 switches the switch 15 to its second position, in which the current source is coupled to the emitter of transistor 10 .
Now a falling edge in the signal bp is expected next and the process is repeated as described above.
The switching process of the two transistors will be explained in detail below:
The outputs of the bipolar transistors 9 and 10 switch at the point where the currents through the emitters are equal. So, at this moment the emitter currents are I/2, wherein I is the tail current of the differential pair formed by the current source 14 . At this moment the current through the resistor 13 is I/2. It can thus be calculated that: V 1 −Vbe−½I*R=V 2 −Vbe. Now the collector of transistor 10 goes down and the collector of the transistor 9 goes up. Output RXD 0 goes from 1 to 0 and output RXD 1 goes from 0 to 1. The falling edge of RXD 0 causes the control logic to switch the switch 15 to the other side of the resistor (The control logic only reacts to negative edges of RXD 0 and RXD 1 , positive edges are of no influence). After this, the differential pair switches its outputs again when the point is reached where: V 2 −Vbe−½*I*R=V 1 −Vbe. RXD 1 goes from 1 to 0, RXD 0 goes from 0 to 1, and the control logic switches the tail current back to the other side of the resistor.
In the example of FIG. 2 , the bus lines were already high or low at the beginning. However, this may not be the case when starting up a data bus. This means no differential voltage on the bus for a specified time. When the idle state is detected, the switch 15 is set to the first (default) position. In this position the receiver is ready to detect a “0”, as, for example according to the FlexRay-standard, a “0” is always the first bit after idle. A “0” means that RXD 0 will have a falling edge and on this edge the switch position will be set to the second position so that the receiver is ready to detect a “1”. Now the receiver and the switching position are in the normal routine as described above.
If for some reason the first bit after idle is not a “0” but a “1”, it would seem that the first bit will be missed by the system. This, however, is not the case for the following reason: the falling edges of RXD 0 and RXD 1 are translated into an RXD signal. So a negative edge on RXD 0 makes RXD “0” and a negative edge on RXD 1 makes RXD “1”. Most protocols require that RXD is high when the bus is idle, so if the first bit is “1” no negative edge will arise on RXD 1 , RXD will stay high, and the comparator will still wait for a “0” (which should come after the previous “1”). So, the system will still work in this case.
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The invention relates to a receiver for a differential data bus with two resistive branches ( 1, 2, 3; 4, 5, 6 ), with a differential amplifier with two transistors ( 9, 10 ), with a resistor ( 13 ), and with a control logic ( 16 ) that controls a switch ( 15 ) with which a current from a current source ( 14 ) is switchable to either side of the resistor ( 13 ), which resistor couples the two transistors ( 9, 10 ), and with two operational amplifiers ( 17, 18 ) which are coupled to the two transistors ( 9,10 ) of the differential amplifier with opposite poles, in which receiver the control logic detects from the output signals of the two operational amplifiers ( 17,18 ) whether a “0” or a “1” is expected on the bus and which receiver sets the switch ( 25 ) accordingly so that a comparison with the received bus signal is made.
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TECHNICAL FIELD OF THE INVENTION
[0001] The present invention relates to a system that implements instance based learning for effective behavior profiling and detection of intrusion anomalies.
BACKGROUND OF THE INVENTION
[0002] Intrusion into a system such as an information system can be defined as one or more unauthorized activities that violate the security policy applicable to the system. The detection of an intrusion is the act of tracing those unauthorized activities (or users) in the system. Intrusion detection relies on the belief that an intruder's behavior will be noticeably different from that of a legitimate user and that unauthorized actions, therefore, are detectable. Thus, intrusion detection should provide an in-depth defense against intrusion into the system by checking and rechecking the effectiveness of other access control mechanisms of the system.
[0003] The main goal of intrusion detection is to effectively monitor the events occurring in a host machine or network for signs of intrusion and to report the signs of intrusion to a system administrator so that the system administrator can take appropriate remedial and/or preventative actions.
[0004] Generally, the detection of intrusions can be classified into two categories, misuse detection and anomaly detection, depending on how the monitored data is evaluated. In misuse detection, information about previous attacks is used to generate attack signatures that can be compared to current activity data in order to determine if the current activity data indicates an intrusion. In anomaly detection, the normal behavior of the system is learned, and any activity that strongly deviates from the learned normal behavioral profile is considered an intrusion.
[0005] One of the problems with anomaly intrusion detection is that it is difficult to learn intrusion behavior from discrete data. Unfortunately, the success of an intrusion detection is mainly dependent on how efficiently the audited data can be analyzed for traces of intrusion.
[0006] An instance based learning model can be used to classify query data (i.e., query instance) according to the relationship between the query instance and stored exemplar instances. Instance based learning requires a notion of how the similarity between two discrete data sequences can be measured in order to classify the query instance.
[0007] The similarity measure proposed by Lane and Brodley in “Temporal Sequence Learning and Data Reduction for Anomaly Detection,” Proceedings of the 5 th Conference on Computer and Communication Security, ACM Press, New York, N.Y., is a useful similarity metric. According to this similarity metric, the similarity between two discrete valued sequences X and Y of fixed length n defined as X=(x 0 , x 1 , . . . , x n−1 ) and Y=(y 0 , y 1 , . . . , y n−1 ) is given by the following pair of functions:
W ( X , Y , k ) = { 0 if k < 0 or x k ≠ y k 1 + W ( X , Y , k - 1 ) if x k = y k
and
SIM ( X , Y ) = ∑ k = 0 n - 1 W ( X , Y , k )
[0008] As can be seen from the above functions, the similarity score between two instances X and Y that are exactly the same is a maximum and has a value of n(n+1)/2. This maximum similarity score is denoted Sim max . A lower bound on the similarity score when there is exactly one unmatched position between any pair of instances X and Y is given by the following function:
Lb n 1 = { ( ⌈ n - 1 2 ⌉ ) 2 if n is even n 2 - 1 4 if n is odd
[0009] The converse measurement, i.e., distance, between the sequences X and Y is given by Dist(X,Y)=Sim max −Sim(X,Y).
[0010] In the context of anomaly detection, user behavior or system behavior is profiled. However, these behavioral profiles can, potentially, grow without bound. Therefore, data reduction is important because the size of the profile directly impacts the time required for classification of a test instance as normal or an anomaly. The behavioral profile of the user/network is required to be present in main memory for real time detection of intrusive activities to be possible. Accordingly, a major challenge in designing an intrusion detection system is to make sure that these behavioral profiles do not consume huge amounts of space in the primary memory, or otherwise normal activities of the user/network will be impaired.
[0011] The present invention is directed to an intrusion detection system that detects anomalies and that addresses one or more of these or other problems.
SUMMARY OF THE INVENTION
[0012] In accordance with one aspect of the present invention, a computer implemented method for detecting intruders into a computer comprises the following: capturing historical data input into the computer by a user during a training mode; profiling the historical data during the training mode to identify normal behavior; capturing test data input by the user into the computer during an operational mode; comparing the test data with the profiled historical data in accordance with a predetermined similarity metric during the operational mode to produce similarity results; and, evaluating the similarity results during the operational mode to identify abnormal data.
[0013] In accordance with another aspect of the present invention, a computer implemented method for detecting intruders into a computer system comprises the following: establishing clusters of training data input into the computer system by a user during a training mode, wherein each cluster includes a representative instance, a frequency associated with the representative instance, and pointers that point to a list of non-representative instances whose similarity scores with the representative instance is above a predetermined threshold, and wherein the similarity scores are based on a predetermined similarity metric; comparing test data with the representative instances of the clusters in accordance with the predetermined similarity metric during an operational mode to produce similarity results, wherein the test data is input by the user into the computer system; and, evaluating the similarity results during the operational mode to identify intrusions.
[0014] In accordance with still another aspect of the present invention, a computer implemented method for detecting intruders into a computer system comprises the following: capturing first data input into the computer system; establishing clusters of the first data, wherein each cluster includes a representative instance, a frequency associated with the representative instance, and pointers that point to a list of non-representative instances whose similarity scores with the representative instance are within a predetermined range, and wherein the similarity scores are based on a predetermined similarity metric; capturing second data input into the computer system; comparing the second data with the representative instances in accordance with the predetermined similarity metric to produce similarity results; and, evaluating the similarity results to identify abnormal data.
BRIEF DESCRIPTION OF THE DRAWING
[0015] These and other features and advantages will become more apparent from a detailed consideration of the invention when taken in conjunction with the drawings in which:
[0016] FIG. 1 illustrates an example device 10 suitable for implementing the present invention;
[0017] FIG. 2 illustrates an example table useful in describing a data structure maintained by the example device of FIG. 1 ;
[0018] FIGS. 3A and 3B illustrate a flow chart for a clustering program that can be executed by the example device of FIG. 1 ;
[0019] FIGS. 4A and 4B are useful in explaining data clustering and the creation of the data structure shown in FIG. 2 ;
[0020] FIGS. 5A and 5B illustrate a flow chart for a program that can be executed by the example device of FIG. 1 to determine if a test instance is an outlier.
DETAILED DESCRIPTION
[0021] The present invention can be implemented in the context of a processor, work station, or other device 10 having an example construction such as that shown in FIG. 1 . The example device 10 includes a processor 12 , such as a CPU, coupled to output devices 14 , input devices 16 , and a memory 18 . The output devices 14 , for example, may include a printer, an alarm or other system administrator alert, and/or display so that the user can view the outputs of the example device 10 and so that the system administrator can be notified of possible intrusions. The input devices 16 , for example, may include a keyboard and/or mouse so that the user can input data and instructions to the example device 10 . The memory 18 stores programs and data at least some of which may be the data structure and clustering algorithm described below. The example device 10 may further include a transceiver 20 such as a modem, network interface, or other device that permits the example device 10 to communicate with other devices through an intranet, internet, or otherwise. The intrusion alerts can be provided to the system administrator by use of the transceiver 20 .
[0022] As suggested above, the example device 10 may have other constructions and may have additional and/or other input and/or output devices than those described above.
[0023] As also suggested above, the example device 10 can be a user terminal in a network such as a local area network or a wide area network. The example device 10 and some or all of the other user terminals in the network may include a data structure and a clustering algorithm as described below so that each terminal monitors the activities of its user in order to detect anomalies.
[0024] Alternatively, in some networks, it may be desirable to provide a single user terminal or non-user terminal that includes a data structure and a clustering algorithm as described below so that all user activities in the network are monitored by the single terminal in order to detect network wide anomalies. Other variations are also possible.
[0025] In one embodiment of the present invention, an instance based learning framework provided by the data structure and clustering algorithm develops a user behavior profile and compares observed user behavior with the profile in order to classify the user behavior as an anomaly and, therefore, a possible intrusion. In order to assist in user behavior profiling, the instance based learning framework uses the data structure, which may be a single data structure, and the clustering algorithm that populates the data structure with data. This instance based learning framework also addresses the problem of data reduction and the periodic updating of the behavioral profile to thereby eliminate the need of a multi-agent based architecture for anomaly intrusion detection. Another advantage of the instance based learning framework is that it addresses the problem relating of memory utilization through instance compression.
[0026] In order to enable intrusion detection based on anomalous behavior, a profile of a user's normal behavior is first created during a training mode. UNIX shell command traces can be used to profile a behavior by converting streams of shell command traces into a set of fixed length instances of temporally adjacent user actions. The raw stream of shell command traces is partitioned so that every position i of the event stream is considered as a starting point for an instance of length n. The instance of length n starting at position i in the raw stream is referred to as the instance with time stamp value equal to i. All such instances are collected over a period of time to form the training data required to profile the user's normal behavior. This profiling is performed through use of the data structure and the clustering algorithm described below.
[0027] As an example of partitioning, let x 1 , x 2 , x 3 , x 4 , x 5 , x 6 , . . . be a command trace generated by a user during a session, and let n=5 so that the length of each instance is 5. Then, the command trace is partitioned so that (x 1 , x 2 , x 3 , x 4 , x 5 ) is the instance with time stamp value=1, (x 2 , x 3 , x 4 , x 5 , x 6 ) is the instance with time stamp value=2, and so on.
[0000] Accordingly, the raw stream of shell command traces is typically partitioned to generate several instances.
[0028] The data structure is a list of tables, where each table in the list has a size M defined by the following equation:
M = ⌈ n 2 ⌉ + 1
where n is the length of each of the instances that are used to populate the tables in the list, and where M defines the number of entries or rows in each of the tables.
[0029] An example table is shown in FIG. 2 . The first entry in the table has fields to accommodate a representative instance and the frequency of that representative instance in the training data. The first entry also contains two other fields—one to store a time stamp value, and the other to store a pointer to the next table in the list. All other remaining entries in a table contain a pointer pointing to the head of a list of exemplar instances. These exemplar instances are mapped to the table by a hash function. For example, at entry M−1, a pointer points to the head of a list of exemplar instances. The instance,frequency block shown in FIG. 2 is the head node of the list of exemplar instances, and the address of this node is stored as the pointer in the (M−1) th entry in the table. This block in turn points to another block of the same type.
[0030] Each instance is a vector of fixed length n. The first entry in the table contains the representative instance X=(x 0 , x 1 , x 2 , . . . ,x (n−1)) . Assume that another instance Y is to be added to the same table. The similarity k 1 between X and Y is calculated as k 1 =Sim(X,Y). The hash value for Y is computed as follows. The minimum non-negative root of the equation r(n−r+1)=n(n+1)/2−k 1 is found and is denoted by t. The hash value h(k 1 ) is assigned the value round(t)+1, where round(t) rounds t to the closest integer. Instance Y is then be added to the list of exemplar instances and is accessible by a pointer that is stored in the h(k 1 ) th entry of the table. This process is also discussed below.
[0031] The instance in the first entry of a table is referred to as the representative instance (R) of that table and is representative of all other instances to which the pointers in that table point.
[0032] As discussed above, the hash function h which maps an instance into a particular entry of a table is given by h(k)=round(t)+1, where t is the minimum non-negative root in r of the following equation:
r ( n - r + 1 ) = n ( n + 1 ) 2 - k ( 1 )
where k is the similarity score between that instance and the representative instance R of a table. If k=Sim max , for example, then equation (1) becomes simply r(n−r+1)=0, since Sim max =n(n+1)/2. Therefore, the root r has two values, 0 and n+1. The value t is assigned the value 0 because, out of the two roots, the root 0 is the minimum non-negative root. Hence, h(Sim max )=round( 0 )+1=1.
[0033] The tables in the data structure can be populated with data by a process referred to herein as clustering. A cluster is usually represented by a single exemplar instance, which is the instance having the smallest distance from all other instances in the cluster. However, in the clustering process described herein, such a representative instance of a cluster is not determined. Rather, distinct instances are grouped to form clusters depending on their similarity values.
[0034] The criterion that is used to cluster instances X and Y together in the same cluster is to determine a representative instance R that satisfies two conditions. The first condition is that both the Sim(X,R) and Sim(Y,R) fall in the interval I defined as follows:
I = [ Lb n 1 , n ( n + 1 ) 2 ] .
The second condition is that Sim(X,R)≧Sim(X,R′) and Sim(Y,R)≧Sim(Y,R′) for all R′ for which the first condition (i) is satisfied. For each distinct instance captured during the training mode, a single copy will be retained along with its frequency in the training data. Again, for similarities k∈I, the roots of equation (1) are always real and non-negative, and h(k)∈
[0035] ={1, . . . , M}. The clustering algorithm described below centers around the observation that the instances whose similarity scores with R are in the interval I will form a cluster. Hence, a set of instances, which can be accessed via a particular table, have their similarity scores with the representative instance R of that table in the interval I and thus forms a cluster.
[0036] The pseudo code for the clustering algorithm is as given below.
[0000] Proc Clustering
[0000] Begin
[0037] Let Y be an instance under consideration.
Step 1. Move through the Tables in the list by checking only the data in the first entry of each table to find a set S of instances R′ such that Sim(R′,Y)≧Lb n 1 . Step 2. If there is no such R′, then
Initialize a table of size M with Y in the 1st entry. Add this table at the end of the list of tables. Initialize the time stamp field by the time stamp value of the instance Y also set the frequency of this instance to 1.
Else
Find an instance R∈S such that SIM(Y,R)≧SIM(R′,Y)∀R′∈S. Update the time stamp value of the table associated with R by the time stamp value of the instance Y. Compute z=h(Sim(R,Y)) where the hash function h is defined above. Go to Step 3 .
End Step 3. If z==1,
Increment the frequency of the instance in the first entry of the table for R by 1.
Else
Add Y in the list issued from the z th entry of the table for R if it is not there previously. Set the frequency for that instance to be equal to 1. If Y is already there in the list corresponding to the z th entry of the table for R, then increment it's frequency by 1.
End Step 4. Repeat Steps 1 to 3 until all the training instances are examined.
End
End Proc
[0057] The above algorithm will output a list of tables with each distinct instance being present in only one of the tables. For each distinct instance, the algorithm also outputs the frequency of the instance in the training data (also referred to as the instance dictionary).
[0058] This clustering algorithm may be implemented as a program 50 which is shown by way of the flow chart of FIGS. 3A and 3B , which may be stored in the memory 18 , and which may be executed by the example device 10 . Accordingly, at 52 , the next instance Y derived from the actions of a user is considered. At 54 , a variable i is set equal to one and, at 56 , the similarity between the instance Y and a representative instance R i from the Tables in the list is computed. If Sim(R i ,Y)≧Lb n 1 for instance Y as determined at 58 , the representative instance R i is added to the set S at 60 . After the representative instance R i is added to the set S at 60 , or if Sim(R i ,Y)<Lb n 1 , a test is made at 62 to determine whether all representative instances R i in the list of tables have been tested. If not, i is incremented by one at 64 and flow returns to 56 .
[0059] If all representative instances R i in the list of tables have been tested, a test is made at 66 to determine whether the set S is empty. If the set S is empty, the instance Y did not compare closely enough to the representative instances R i in the current tables in the list. Therefore, a new table of size M is made at 68 with Y as its representative instance in the 1st entry of the new table, this table is added at the end of the list of tables at 70 , the time stamp field is initialized by the time stamp value of the instance Y and the frequency of this instance is set to one at 72 , and program flow returns to 52 .
[0060] On the other hand, if the set S is not empty as determined at 66 , a representative instance R is found in the set S (R∈S) at 74 such that SIM(Y,R)≧SIM(R′,Y)∀R′∈S. In other words, the representative instance R producing the largest similarity score of all representative instances in the set S is found. The time stamp value of the table associated with this R is set to the time stamp value of the instance Y at 76 . Also at 76 , the frequency of this instance R should be set to 1. At 78 , the hash value based on the similarity score between this instance Y and the representative instance R determined at 74 is computed as described above and is assigned to the variable z.
[0061] At 80 , a test is made to determine if the variable z is equal to 1. If so, the instance Y is identical to the representative instance R found at 74 and the frequency for this representative instance R is incremented by one at 82 . If the variable z is not equal to 1, a test is made at 84 to determine whether this instance Y is already in the list of exemplar instances corresponding to the z th entry of the table for R. If not, the instance Y at 86 is added to the list of exemplar instances and a pointer is entered in the z th entry of the table for the representative instance R found at 74 that points to head of the list. Also, at 88 , the frequency for this instance Y is set equal to 1. On the other hand, if this instance Y is already in the list of exemplar instances corresponding to the z th entry of the table for R, then it's frequency is incremented by 1 at 90 .
[0062] After processing at 82 , or at 88 or at 90 is completed, program flow returns to 52 to process the next instance Y.
[0063] Each of the resulting clusters represents a specific corresponding behavioral pattern of the user. These clusters can be periodically updated by re-initiating the training mode and processing an updating set of training data by the clustering algorithm.
[0064] The resulting data structure is also of help in determining changes in behavioral profiles. It may be assumed that behavioral profiles change relatively slowly. The clustering algorithm applied on an initial set of training instances may not yield tables with all its entries filled up. However, it can be expected that, as user behavior changes over time, these unfilled entries of each table in the list will start getting filled as the clustering algorithm is applied periodically.
[0065] As indicated by the clustering algorithm, a completely new instance, which cannot be put in any of the existing tables in the list, is used to initiate a new table at the end of the list, with this instance as the representative instance R of that table.
[0066] An upper bound (Ub) may be placed on the size of the list of tables in order to place an upper limit on the size of the data structure so that memory utilization can be maintained at a reasonable level. If so, a possible strategy to determine changes in the behavioral profile is LRU (least recently used) as has been suggested by Lane and Brodley in “Temporal Sequence Learning and Data Reduction for Anomaly Detection,” Proceedings of the 5 th Conference on Computer and Communication Security, ACM Press, New York, N.Y. In this context, the table with the oldest time stamp value is identified, and all instances, including the representative instance R, that can be accessed via this table are deleted. New profile data can then be made representative (R) of this table. Thus, a single data structure accounts for both storage reduction and also updating of the behavioral profile.
[0067] The following is an example of the population of tables by clustering. The list corresponding to a particular entry of a table as described above is made up of linked nodes, where each node contains a reference to the next node in the list. A linked list is considered a recursive data structure because it has a recursive definition. In addition, each node contains data. A linked list may be either empty, represented by NULL, or a node that contains data and a reference to a linked list.
[0068] As described above, the data in each node includes an instance and its corresponding frequency. Also, each node contains one pointer that points to the next node of similar kind in the list. Each node by default is initialized with its pointer field set to NULL.
[0069] Assume the following instances are in the instance dictionary: A=(x 1 , x 2 , x 3 , x 4 , x 5 , x 6 ); B=(x 1 , x 2 , x 3 , x 4 , x 5 , y 6 ); C=(y 1 , x 2 , x 3 , x 4 , x 5 , x 6 ); D=(x 1 , y 2 , x 3 , x 4 , x 5 , x 6 ); and E=(y 1 , y 2 , x 3 , x 4 , x 5 , x 6 ). Each instance has six elements and, therefore, n=6. With n=6, M=4, Lb n 1 =9, and Sim max =21.
[0070] In applying the clustering algorithm, instance A (as the first instance) is made the representative instance of the first table. Next, the similarity score between instance A and instance B is computed as Sim(A,B)=15 using the above equations. This similarity score is in the predetermined interval I of [9, 21]. So, using equation (1) to determine t, h( 15 )=round( 1 )+1=2, since the minimum non-negative root t in this case is equal to 1. As a result, a node in the list is created with B as the instance and with its frequency set to 1, and the address of this node is stored in the 2 nd entry of the table as a pointer.
[0071] Next, as there is no other table yet in the list, only the similarity score between instance A and instance C is computed as Sim(A,C)=15. This similarity score is also in the predetermined interval I of [9, 21]. Again, round( 1 )+1=2, since the minimum non-negative root t in this case is equal to 1. As a result, another node is created with C as the instance and with the frequency set to 1. As shown in FIG. 4A , The address of this node is stored in the reference field of the node for instance B.
[0072] In FIG. 4A , Pointer=NULL means the pointer points nothing because, at the present time, there is not yet an instance for which h(k) has a value of 3 or 4. Similarly, the node for the instance C does not contain any arrow because the instance C does not point to anything, i.e., its pointer value is NULL. Its now evident from this description that the first instance which gets mapped (by the hash function) to a particular entry of a table becomes the head node of the list and it is the address of this node which is stored as a pointer to the corresponding entry of the table. All other instances which get mapped to this entry of the table, are then added to the end of the list. In the example above, the node for instance B is the first node and becomes the head node of the corresponding list while the node for instance C is added at the end of the list.
[0073] For instance D, Sim(A,D)=11 and h( 11 )=round( 2 )+1=3. Similarly, for instance E, Sim(A,E)=10 and h( 10 )=round( 2 . 38 )+1=3. Only the instance A is used to compute the similarity scores because, as yet, there is no other table. Since the similarity values for both these instances lie in the predetermined interval I, instances D and E are added as shown in FIG. 4B .
[0074] As indicated above and in connection with FIG. 2 , the pointers of all instances for a particular entry can be stored in the entry itself. That is, the addresses of both the nodes for the instances B and C can be stored in the 2 nd entry of the table. However, a problem with this approach is that, at the time of training, the number of instances that will be mapped to a particular entry of a table is unknown. For each different entry, this number can very well be different. Therefore, the number of pointers that will be needed could vary from one entry to another and, as the number is not known beforehand, it is very difficult to allocate storage to save these pointer values in a particular entry of the table. Therefore, it is preferable to store the instances as nodes in a list and to point from these nodes to the next node in the list.
[0075] Also, as should be understood from the above description in connection with FIG. 3 , if the next instance F does not produce a similarity score with instance A that is within the interval I, instance F is used to create a new table with the instance F as the representative instance of this new table. Then, for the next instance G, a first similarity score is computed between the instance G and the instance A, and a second similarity score is computed between the instance G and the instance F. If the first similarity score is within the interval I, then instance G is added to the table of instance A in the manner described above. However, if instead the second similarity score is within the interval I, then instance G is added to the table of instance B in the manner described above. But, if neither the first nor the second similarity score is within the interval I, then instance G is used to start a new table. Again, if both the first and second similarity scores are within the interval I, then the instance A or F with which similarity score is higher is found, and then the instance G is added into it's table in the manner described above.
[0076] The similarity function as described above enjoys some useful properties, and these properties can be used to address some of the relevant problems of Instance Based Learning. The goal is to establish a platform which will facilitate introduction of a new outlier detection algorithm applicable to anomaly intrusion detection during the operational mode of the present invention.
[0077] A first of the useful properties of the similarity function is that equation (1) always yields a real, non-negative root for each possible similarity score k in the interval I. In fact, the hash function h(k)=round(t)+1 is an onto mapping from S to {1, . . . , M} where S(⊂I) is the collection of scores that the similarity measure can assume for two instances of length n.
[0078] This property can be proven as follows. Equation (1) can be re-written as follows:
r 2 - ( n + 1 ) r + d = 0 , where d = n ( n + 1 ) 2 - k ( d ≥ 0 ∀ k ∈ I )
The discriminant D of this equation is given by the following equation:
D =( n +1) 2 −4d.
A careful look at the discriminant for k∈I shows that the minimum value of D is either 1 or 0 depending on whether n is even or odd, which guarantees that equation (1) always yields a real root for k∈I. Again, since the maximum value of D is (n+1) 2 , the fact that roots of equation (1) that are non-negative is also proven.
[0079] Let y∈{1, 2, . . . , M} be any integral value, and let k be given by the following equation:
k = ( y - 2 ) ( y - 1 ) 2 + ( n - y + 1 ) ( n - y + 2 ) 2
If an instance X has only one mismatch with a representative instance R in the (y−1) th position starting from the left, then Sim(X,R)=k≧Lb n 1 . Hence, k∈S. For this value of k, the roots of equation (1) in r are (y−1) and (n−y+2). Because
y ≤ M = ⌈ n 2 ⌉ + 1 = { n 2 + 1 if n is even ( n + 1 ) 2 + 1 if n is odd
then the following relationship is implied:
y - 1 { < n - y + 2 if n is even ≤ n - y + 2 if n is odd
So, (y−1) is the minimum of the two roots of equation (1) in r and, hence, h(k)=y. Thus, it is proven that the hash function as described is an onto mapping from S to {1, 2, . . . , M}.
[0080] A second of the useful properties of the similarity function is that the similarity score between two instances that have consecutive mismatches at the end or at the start of the instances is greater than the similarity score between any other pair of instances of the same length having the same number of mismatches at any position.
[0081] This property can be proven as follows. Let X be a given instance of length n. Now, for some p∈{1, 2, . . . , n}, let Y and Z be two other instances of same length each having p mismatches with X. Let all the p mismatches of Y with X be in consecutive positions at either the start or end of the instance X, and let all of the p mismatches between Z and X be in any p positions. Then, the similarity score between X and Y is given by the following equation:
Sim ( X , Y ) = ∑ m = 1 n - p m = ( n - p ) ( n - p + 1 ) 2
Now, p mismatches with X will divide the instance Z into (p+1) disjoint runs of consecutive matches, where the length of some of the runs can be zero. Let 1 1 , 1 2 , . . . , 1 p+1 be the lengths of these runs of consecutive matches with X such that the contribution of the k th run to the final similarity score is given by
∑ m = 0 l k m .
Hence, the similarity score between instance X and instance Z is given by the following equation:
Sim ( X , Z ) = ∑ k = 1 p + 1 ( ∑ m = 0 l k m )
such that
∑ k = 1 p + 1 l k = n - p with 0 ≤ l k ≤ n - p
Thus, n−p gives the number of positions where the elements of the instance X is same as that of the elements of the instance Z. For example, if X=(x 0 , x 1 , x 2 , x 3 , x 4 , x 5 , x 6 , x 7 ) and Z=(x 0 , z 1 , x 2 , x 3 , z 4 , z 5 , x 6 , x 7 ) (x 0 , z 1 , x 2 , x 3 , z 4 , z 5 , x 6 , x 7 ) where X and Z have three mismatches at the 2 nd , 5 th , and 6 th positions, p=3. Therefore, these 3 mismatches will divide the instance Z in to (3+1)=4 disjoint runs of consecutive matches. The value l k 's represents the lengths of those consecutive matches. The sum of these lengths will be equal to n−p=8−3=5. If only one l k is non-zero and all others are zero, then Sim(X,Z)=Sim(X,Y).
[0082] Let it now be assumed that two l k s are non-zero and let them be l i and l j such that l i ≦l j . Because
∑ m = 1 l i m < ∑ m = l j + 1 n - p = l i + l j m
it follows that Sim(X,Z)<Sim(X,Y). Following a similar recursive argument, it can be inferred that Sim(X,Z)≦Sim(X,Y) for all Z with p mismatches with X.
[0083] A third of the useful properties of the similarity function is that the maximum number of mismatches that an instance can have with the representative instance R and still be in the same table with the representative instance R is given by the following expression:
min k { k : ( n - k - 1 ) ( n - k ) 2 < Lb n 1 }
[0084] This property can be proven as follows. Let C be the maximum number of mismatches that an instance X can have with the representative instance R and still be in the same table with the representative instance R. This assumption implies that, if the instance X has (C+1) consecutive mismatches with the representative instance R either at the end or at the start of the instance X, then the instance X has a similarity score with R that is out of the region I, that is, less than the value of Lb n 1 . So, it now follows from the second property that C is the minimum of k such that k+1 consecutive mismatches between X and R at the end or at the start of the instance X yields a similarity score between X and R of less than Lb n 1 . In other words, C is given by the following expression:
C = min k { k : ∑ m = 1 n - ( k + 1 ) m < Lb n 1 }
which computes to
C = min k { k : ( n - k - 1 ) ( n - k ) 2 < Lb n 1 } .
[0085] The similarity score of an instance X that has i(≦C) mismatches with a representative instance R either at the end or at the start of the instance X is given by the following equation:
Sim ( X , R ) = ∑ m = 1 n - i m = ( n - i ) ( n - i + 1 ) 2 = K i ( 2 )
The interval
I = [ Lb n 1 , n ( n + 1 ) 2 ]
can be partitioned into some subintervals as follows. Note that K i is an interior point in the interval I for all i=1, 2, . . . , C. Letting K 0 =(n(n+1))/2 and K C+1 =Lb n 1 , its easily observable from equation (2) that
K i >K i+1 ∀i=0, 1, . . . , C.
Therefore, the interval I can be written as I=∪ i=0 C [K i+1 ,K i ].
[0086] A definition is appropriate before the description of the fourth of the useful properties. For any two instances X and Y each of length n, a max-length-of-consecutive-matches is denoted m XY and is defined as the maximum length of all runs of consecutive matches between X and Y. From this definition, it follows that m XY =m YX . As for example, Sim(X,Y)=0 implies that m XY =0, and Sim(X,Y)=(n(n+1))/2 implies that m XY =n. Also, if Sim(X,Y)=Lb n 1 , then
m XY = ⌊ n 2 ⌋ .
[0087] The fourth of the useful properties of the similarity function is that m XR =n−i−1 for 9≦n≦18 is a necessary and sufficient condition for an instance X to have a similarity score with R in the interval [K i+1 ,K i ) for all 1≦i<C−1.
[0088] This property can be proven as follows. Let it be assumed that an instance X produces a similarity score with R in the interval [K i+1 ,K i ) for any 1≦i<C−1. For any 1≦i<C−1, if the instance X is such that m XR ≧n−i, then Sim(X,R)≧K i . Let it now be assumed that M XR =n−i−2. Without loss of generality, it may be assumed that the first (n−i−2) positions in X have a match with R. This latter assumption implies that the (n−i−1) th position from the start (left end) must be a mismatch. Now, if all the remaining (i+1) positions at the right end are a match (this run of consecutive matches does not change the value of m XR because, for 9≦n≦18 and 1≦i<C−1, the inequality n−i−2>i+1 always holds), then
Sim ( X , R ) = ( n - i - 2 ) ( n - i - 1 ) 2 + ( i + 1 ) ( i + 2 ) 2 ( 3 )
Therefore,
K i + 1 - Sim ( X , R ) = ( n - i - 1 ) ( n - i ) 2 - ( n - i - 2 ) ( n - i - 1 ) 2 - ( i + 1 ) ( i + 2 ) 2 = n - ( i + 1 ) ( i + 4 ) 2 > 0
for it is verifiable that, for n≦18 and for any 1≦i<C−1, n>((i+1)(i+4))/2.
[0089] The similarity score given in equation (3) is an upper bound of all similarity scores for instances X in which m XR ≦n−i−2. Hence, it follows from the description above that m XR ≦n−i−2 implies that Sim(X,R)<K i+1 . So, for both m XR ≧n−i and m XR ≦n−i−2, Sim(X,R) cannot be in the interval [K i+1 ,K i ) and, therefore, m XR =n−i−1.
[0090] Conversely, an instance X such that m XR =n−i−1 for any 1≦i<C−1 can be considered. Since a run of consecutive matches of length n−i−1 between two instances contributes a score equal to K i+1 to the similarity score, it therefore follows that Sim(X,R)≧K i+1 . Following a similar reasoning as above, it can now be shown that, for any 1≦i<C− 1 , K i −Sim(X,R)>0 for all X with m XR =n−i−1. Accordingly, Sim(X,R)∈[K i+1 ,K i ).
[0091] For 9≦n≦18, we have from property 3 that 3≦C≦5. Therefore, from the fourth property as described above, the similarity that an instance X should have with a representative instance R is such that Sim(X,R)∈[K i+1 ,K i ) for all 1≦i<C−1.
[0092] A fifth of the useful properties of the similarity function is that n−C−1≦m XR ≦n−C for 4≦n≦11 and n−C−2<m XR ≦n−C for 12<n<18 are necessary conditions for an instance X to have a similarity score with R in the interval [K C ,K C−1 ).
[0093] This property can be proven as follows. Let X be an instance for which Sim(X,R)∈[K C ,K C−1 ). For any instance Y, Sim(Y,R)=Lb n 1 implies that
m YR = ⌊ n 2 ⌋ ,
and also that Lb n 1 upper bounds all similarity scores for all instances Y for which
m YR = ⌊ n 2 ⌋
is true. Hence, it follows that
m YR < ⌊ n 2 ⌋
implies that Sim(Y,R)<Lb n 1 ≦K C . Therefore,
m XR ≥ ⌊ n 2 ⌋
and, from the fourth property described above, it follows that m XR ≦n−C.
[0094] It may be now assumed that
m XR = n - C - k ≥ ⌊ n 2 ⌋
for some k∈N. The upper bound of all similarity scores for all such X's for which m XR =n−C−k is true is given by the following expression:
u = ( n - C - k ) ( n - C - k + 1 ) 2 + ( C + k - 1 ) ( C + k ) 2
Therefore
K C - u = ( n - C ) ( n - C + 1 ) 2 - ( n - C - k ) ( n - C - k + 1 ) 2 - ( C + k - 1 ) ( C + k ) 2 = kn - C 2 + 4 Ck + 2 k 2 - 2 k - C 2
[0095] The following table can be assembled based on the above equations:
n C K C − u for k = 1 K C − u for k = 2 K C − u for k = 3 4 1 2 — — 5 2 0 — — 6 2 1 — — 7 2 2 3 — 8 2 3 5 — 9 3 0 1 — 10 3 1 3 — 11 3 2 5 6 12 4 −2 0 — 13 4 −1 2 3 14 4 0 4 6 15 4 1 6 9 16 5 −4 0 2 17 5 −3 2 5 18 5 −2 4 8
Every row in the above table can be identified by using the value of n. A “−” in a row indicates that for a value of n, the corresponding value n−C−k falls below
⌊ n 2 ⌋
and so is ignored because only values of K C −u for
m XR = n - C - k ≥ ⌊ n 2 ⌋
are of interest.
[0096] From the above table, it can be seen that all the entries in the fifth column (k=3) either are ignored or are greater than zero, while the fourth column (k=2) has zero for some values of n. An inference that can be made from this observation is that, for 4≦n≦11, m XR should be greater than or equal to n−C−1 so that Sim(X,R) is in the interval [K C ,K C−1 ). Similarly, it can be inferred that for 12≦n≦18, m XR should be greater than or equal to n−C−2. Hence, it can be concluded that n−C−1≦m XR ≦n−C for 4≦n≦11 and n−C−2≦m XR ≦n−C for 12≦n≦18 are necessary conditions for an instance X to have a similarity score with R in the interval [K C ,K C−1 )
[0097] The fourth and fifth properties described above demonstrate values for m XR if Sim(X,R)∈[K i+1 ,K i ) ⊂ I for all 1≦i≦C−1. However, the properties described above fail to demonstrate values for m XR if Sim(X,R)∈[K C+1 ,K C ), but
m XR ≥ ⌊ n 2 ⌋ .
This expression for m XR provides a scope for the compression of the instance X with respect to R through run length coding. Also, because of the properties described above, it is evident that compression permits at least a 50% savings of memory.
[0098] Given a query instance Q and a search distance r, a range query is defined by selecting all instances Z from the instance dictionary such that Dist(Q,Z)≦r. A ball centered at Q with radius r is denoted B(Q;r) and is defined such that B(Q,r)={Z: Z is present in the instance dictionary and Dist(Q,Z)≦r}.
[0099] In the application of anomaly intrusion detection, the range query has significance because, for a query instance Q (traces of shell commands), the system administrator may want to determine all instances that are within a distance r of the query instance Q. This determination helps to better analyze the query instances with respect to the user profile that has been created from the instance dictionary. The instance dictionary refers to the training data that is used to learn a profile model. In the present case, the instance dictionary (which is also referred herein as the exemplar instances) has been used to learn the normal behavioral profile of an user.
[0100] It may be thought that the number of distance computations that are required to answer any range query is equal to the size of the instance dictionary. However, the data structure proposed herein can help to answer any range query with a lesser number of distance computations because all the instances in the instance dictionary are partitioned into clusters, each cluster being represented by a representative instance R. Thus, this data structure is useful to restrict the number of distance computations. That is, those clusters for which B(Q,r) has an empty intersection is first determined. This determination requires a number of distance computations equal to the number of representative instances in the clusters. Because the clusters with which B(Q,r) has an empty intersection do not contribute any instance that answers the range query, no further distance computations are required with respect to these clusters. However, each of the clusters with which B(Q,r) has a non-empty intersection may contribute one or more instances that answer the range query. Therefore, for each of these clusters, some instances may answer the range query B(Q,r) and some may not. In order to find these instances that answer the range query, a distance calculation must be made for each instance in these clusters. Accordingly, the total number of distance computations that is required to answer a range query is the number of distinct instances present in all the clusters with which B(Q,r) has non-empty intersection. This number is greater than or equal to the number of representative instances and less than or equal to the total number of distinct instances present in the instance dictionary.
[0101] Because of the definition of cluster, if Dist(Q,R)>r+(n(n+1))/2−Lb n 1 , or in other words if Sim(Q,R)<Lb n 1 −r, then the cluster with representative instance R will have an empty intersection with B(Q,r). So, to answer a range query, all clusters whose representative instances R have a similarity score with the query instance Q that satisfies the inequality Sim(Q,R)<Lb n 1 −r will be discarded, thereby justifying the assertion that all query inquiries can be answered with fewer distance computations.
[0102] To classify instances through outlier detection, let T be a new command trace under test, i.e., a test instance that is evaluated during the operational mode of the present invention. This test instance T can be an instance which the system has seen previously and, if so, then the test instance T is normal data. However, if the test instance T does not produce a similarity score with the representative instance of a table in the interval I
( I = [ L b n 1 , n ( n + 1 ) 2 ] )
for any table in the list, then the test instance T is an outlier to all the clusters and hence will be considered as a possible case of intrusion.
[0103] Moreover, let the test instance T produce similarity scores in the interval I for some of the tables in the list and let these tables be denoted as HT 1 , HT 2 , . . ., HT k . Also, let D i be the similarity score of the test instance T with R i , i.e., the representative instance of table HT i . Further, let d i and σ i denote, respectively, the weighted mean and the standard deviation of the similarity scores between the instances in the table HT i with the representative instance R i of the table HT i . By instances in the table HT i , we mean those instances which can be accessed via the pointers stored in the entries of the table HT i . If D i <d i σ i , for all i=1, 2, . . . , k, then the example device 10 will alert the system administrator because the test instance T may be indicative of a possible intrusion. Otherwise, the test instance T will be considered normal.
[0104] Accordingly, a program 100 shown as a flow chart in FIGS. 5A and 5B may be stored in the memory 18 and executed by the example device 10 to determine if a test instance T is an outlier. At 102 , the next test instance T is acquired and, at 104 , a variable i is set equal to one. At 106 , the similarity score D i between the test instance T and the representative instance R of Table i is computed and, at 108 , this similarity score D i is saved.
[0105] At 110 , the similarity score D i is compared to the interval I defined above. If the similarity score D i is in the interval I, the Table i is added to a list HT at 112 . If the similarity score D i is not in the interval I, or after the Table i is added to the list HT, i is compared to i max , at 114 . The quantity i max is the number of tables in the list of all tables. If i is not equal to i max , i is incremented by one at 116 and flow returns to 106 .
[0106] If i is equal to i max , a test is made at 118 to determine if the list HT is empty. If the list HT is not empty, i is reset to one at 120 . The similarity score D i is compared at 122 to the difference between the weighted mean d i and the standard deviation σ 1 relative to the HT i as defined above. If the similarity score D i is not less than the difference between the weighted mean d i and the standard deviation σ i , then the test instance T is not an anomaly and flow returns to 102 to acquire the next test instance T. However, if the similarity score D i is less than the difference between the weighted mean d i and the standard deviation σ i , a test is made at 124 to determine if i=i max where i max is the number tables in the list HT. If i is not equal to i max , then i is incremented by one at 126 and the next similarity score D i is tested. If i reaches i max , the similarity scores D i for all tables in HT are less than the difference between the weighted mean d i and the standard deviation σ i , then the test instance T is an anomaly and the system administrator is alerted at 128 . Moreover, if the list HT is empty as determined at 118 , then the test instance T did not compare within the interval I to any of the representative instances of the tables on the list of tables, and the test instance T, therefore, is an outlier such that an alert is given at 128 .
[0107] Certain modifications of the present invention have been discussed above. Other modifications of the present invention will occur to those practicing in the art of the present invention. For example, as described above, UNIX shell command traces are used as instances for profiling the behavior of a user or network and for determining outliers. However, shell command traces of other operating systems can be used to form instances that are useful for profiling the behavior of a user or network and for determining outliers. Moreover, data traces other than shell command traces can be used to form instances that are useful for profiling the behavior of a user or network.
[0108] Also, as described above, a training instance is an instance that is processed during the training mode, and a test instance is an instance processed during the operational mode in which outliers are detected. A query instance can be either a training sequence or a test sequence.
[0109] Accordingly, the description of the present invention is to be construed as illustrative only and is for the purpose of teaching those skilled in the art the best mode of carrying out the invention. The details may be varied substantially without departing from the spirit of the invention, and the exclusive use of all modifications which are within the scope of the appended claims is reserved.
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Intruders into a computer are detected by capturing historical data input into the computer by a user during a training mode, by profiling the historical data during the training mode to identify normal behavior, by capturing test data input by the user into the computer during an operational mode, by comparing the test data with the profiled historical data in accordance with a predetermined similarity metric during the operational mode to produce similarity results, and by evaluating the similarity results during the operational mode to identify abnormal data.
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This application is a 35 U.S.C. §371 National Stage Application of PCT/EP2011/000458, filed on Feb. 1, 2011, the disclosure of which is incorporated herein by reference in its entirety.
BACKGROUND
The present disclosure relates to a housing, preferably of a valve having rounded channel portions according to the description below.
In housings of components which are under hydraulic/pneumatic pressure, such as, for example, valves, there are generally formed pressure channels which can be opened and closed by means of valve coils or similar closure members. To this end, the closure members are displaceably accommodated in closure member chambers (valve bores) in which the pressure channels open. The opening locations form, during operation of the component, regions of high material stress in the housing and therefore constitute danger locations in principle for material fracture.
From the prior art, it is therefore known to construct the opening location of a pressure channel, for example, in the valve piston chamber (valve bore) of a sliding valve in such a manner that a peripheral groove in the housing is formed within the valve piston chamber in the operating range of a control edge of the valve piston and is connected to a fluid channel. However, the peripheral groove is not formed in an angular manner, but instead “rounded”. That is to say that the peripheral groove assumes a semi-circular form in its cross-section (transversely relative to the peripheral direction), preferably having a radius=½ channel width, and has a constant radius over the entire periphery in cross-section. A notch effect in the region of the peripheral groove can thereby be reduced and consequently the durability of the component housing as a whole can be increased.
It should be noted at this point, however, that housings of mass-produced hydraulic components are generally in the form of a cast member, produced from a grey iron or an aluminum alloy, the materials used for this purpose having different properties of durability. Often, the compression strength and consequently the compression threshold strength are, for material reasons, considerably higher than the tensile strength and consequently the tensile threshold strength. Detailed tests by the Applicant of this disclosure have shown that in housings of the above-described type, in the region of the peripheral grooves during operation both tensile and compression loads occur simultaneously at different locations in the housing material, the maximum load of the housing reaching its limit in accordance with the material used in the tension-loaded region far more quickly than in the pressure-loaded region.
In view of these technical recognitions, the object of the disclosure is to develop the housing of a hydraulically/pneumatically pressure-loaded component in such a manner that the general hydraulic/pneumatic compression strength thereof can be increased without increasing the outer dimensions or housing wall thicknesses thereof. Furthermore, a method for producing such a housing is intended to be provided.
SUMMARY
This object is achieved with a housing of the generic type having the features described below and by a method having the method steps described below. The description below relates to other advantageous embodiments of the disclosure.
The notion of the disclosure consequently involves the rounded channel portion in the housing of a pressure-loaded component, for example, a valve, being adapted in accordance with the tensile/compression strength properties of the housing material and the stresses which occur in the housing material during operation, optionally with an asymmetrical portion being formed in the rounding path. More specifically, the rounded portion of the relevant groove-like channel guide does not receive in the peripheral groove cross-section and/or along the periphery of the groove and/or in the peripheral longitudinal groove section a radius or groove path which is in principle continuously the same and consequently symmetrical, but instead the rounded portion is adapted to the material stresses during operation established by analysis/calculation in such a manner as to reduce and/or also to increase load peaks in the more highly loaded regions. There is thereby optionally produced an individual asymmetry in the peripheral groove cross-section along the relevant peripheral groove (that is to say, with respect to the groove cross-section center axis) and/or along the periphery of the groove and/or in the longitudinal groove section, whereby the maximum material load limit under operating conditions can be increased, but for which no increase in the outer dimensions of the housing is required.
It is advantageous to construct only the pressure-loaded channel guides in a selective manner with asymmetrically shaped rounded portions since the greatest adaptation effect to the tensile/pressure load in the material can be achieved at these locations and the detection and production complexity remains the lowest in this instance.
It is further advantageous to construct the rounded channel portions for each channel guide in an individual, preferably different manner. Alternatively, however, it is also possible (optionally with an acceptable reduction of the adaptation effect) to standardize the rounded channel portions of the individual, comparably loaded channel guides in order to thereby reduce the production costs.
BRIEF DESCRIPTION OF THE DRAWINGS
The disclosure is explained in greater detail below with reference to a preferred embodiment and the appended drawings.
In the drawings:
FIG. 1 is a partial longitudinal section through the housing of a hydraulically/pneumatically loaded component which is in the form of, for example, a directional sliding valve according to a preferred embodiment of the disclosure, and
FIG. 2 is a partial longitudinal section through the housing of a directional sliding valve having the same structure as FIG. 1 , but in accordance with a conventional construction type.
FIG. 3 is a partial longitudinal section through the housing of a directional sliding valve having the same structure as FIG. 1 , but with asymmetric peripheral grooves.
DETAILED DESCRIPTION
FIG. 2 shows a portion of the housing 1 of a conventional directional sliding valve as a possible example of a component which can be pressure-loaded and in which the subject-matter of the disclosure can be implemented. It is naturally also possible to use the disclosure, for example, in integrated hydraulic/pneumatic control systems in the form of control blocks, modules, etc., as components which can be pressure-loaded.
According to FIG. 2 , the conventional directional sliding valve which is shown purely by way of example has the housing 1 in which a longitudinally extending valve bore (valve piston chamber) 2 is formed. The valve bore 2 serves in this instance to displaceably receive a valve piston or valve sliding member which is not shown in greater detail and on which a number of control edges are formed.
In the valve bore 2 , there are formed with axial spacing from each other peripheral grooves 3 to 7 , which are opened or closed (or optionally also partially opened) via the control edges of the valve piston which is not shown, depending on the axial position thereof. Housing bores (connection holes) TA, A, P, B, TB, via which the peripheral grooves 3 to 7 can be acted on with a hydraulic/pneumatic pressure or depressurized, open in the peripheral grooves 3 to 7 .
In detail, in the present embodiment there are formed five peripheral grooves 3 to 7 along and in the valve bore 2 , of which the three inner peripheral grooves 4 , 5 , 6 are each connected to connections which can be pressure-loaded (connection bores) A, P, B, and the two axially outer peripheral grooves 3 , 7 are connected to a pressure relief connection (tank connection bores) TA, TB which leads to a tank which is not shown in greater detail. The two axially outer peripheral grooves 3 , 7 are further in fluid connection with each other via an upper (or lower) channel bridge 8 . In the comparison component known from the prior art according to FIG. 2 , the peripheral grooves 3 to 7 are trough-like, that is to say, constructed in groove cross-section (transversely relative to the peripheral direction) over the entire periphery in a constant, semi-circular manner with a predetermined radius=½ channel width.
In conventionally established stress charts (for example, using expansion measurement strips or via finite element programs), it is possible to set out the stress distribution in the housing material during a simulated operation of the directional sliding valve according to the conventional structure. Consequently, owing to the known completely rounded portions of the peripheral grooves according to the illustration in FIG. 2 , the smallest possible notch effects are achieved in principle, whereby the stresses in the housing material in the present test example could be limited in a predetermined (simulated) operating situation to a maximum of approx. 152 N/mm 2 . The arrows which are indicated with the reference numeral Pf 1 in FIG. 2 and which are drawn in the rounded region of the peripheral grooves 4 and 6 and are orientated substantially in the direction towards the cross-section halves of the peripheral grooves 4 and 6 facing the respective pressure-relief grooves 3 , 7 indicate the locations with high tensile stress in the housing material. The arrows which are indicated with the reference numeral Pf 2 in FIG. 2 and which are also drawn in the rounded region of the peripheral grooves 4 and 6 but which are counter to the arrows Pf 1 with respect to the groove cross-section center axis indicate the locations with particularly high compression stress in the housing material.
From the operation which is simulated by way of example, a maximum hydraulic/pneumatic compression strength of the tested comparison housing according to FIG. 2 of approximately 400 bar has ultimately been achieved, which strength according to experience is sufficient statistically (including material fluctuations) to ensure a hydraulic/pneumatic compression strength of approximately 300 bar.
FIG. 1 also shows the directional sliding valve according to FIG. 2 , but with a modification of the peripheral groove rounded portions according to the disclosure. All other technical configurations of the directional sliding valve according to the disclosure correspond to the above-described comparison valve of conventional structural type. Only the modification according to the disclosure will therefore be discussed below.
In specific terms, in the conventional valve according to FIG. 2 in the case of a simultaneous fluid pressure load (pulsing), in the three inner peripheral grooves 4 , 5 , 6 a housing breakage has occurred in the region of the two peripheral grooves 4 , 6 directly adjacent to the two tank connections TA and TB. Consequently, in the present example according to the disclosure, these two peripheral grooves 4 , 6 , with respect to their rounded shape, received a cross-section geometry which is different from the conventional valve.
In other words, in the conventional test model and in the test model according to the disclosure in accordance with the present embodiment, GG 30 (but GGG 40 is also possible) having a tensile strength of 300 N/mm 2 and a compression strength of 960 N/mm 2 is used as a housing material. Therefore, in this generally conventional material, the compression threshold strength is significantly greater than the tensile threshold strength. Owing to a displacement of the channel rounded portions in the peripheral groove cross-section along the valve bore axis, that is to say, owing to the formation of the rounded channel portion by placing two circular segments with different radii in the peripheral groove cross-section (smaller radius r 1 in the region of the compression stresses to be anticipated in the housing material, larger radius r 2 in the region of the tensile stresses to be anticipated in the housing material), the hydraulic/pneumatic compression strength of the housing was able on the whole to be increased. In specific terms, the channel rounded portion in the peripheral groove cross-section (that is to say, transversely relative to the peripheral direction) according to FIG. 1 was deformed for the channels 3 and 6 (these peripheral grooves are in fluid connection with the connections A and B which can be pressure-loaded) by a cross-section portion of the channel having the radius r 1 and the other cross-section portion of the channel having the radius r 2 being rounded. The channel cross-section was thereby generally adapted in such a manner that it was possible to reduce the tensile stresses in the housing material (by increasing the groove radius r 2 at an appropriate location, that is to say, at the groove cross-section half facing the pressure relief groove 3 , 7 in each case) and at the same time to increase the compression stress in the housing material (by reducing the groove radius r 1 at the appropriate location, that is to say, at the groove cross-section half facing away from the pressure relief groove 3 , 7 in each case). The “asymmetrical” properties of the cast material used (permissible compression stress significantly higher than the permissible tensile stress) were used in an advantageous manner for this purpose.
In the simulated operation test with the component according to FIG. 1 (corresponding to the above-described operational test with the conventional component according to FIG. 2 ), it was possible to reduce the material stresses in the housing modified according to the disclosure to 118 N/mm 2 (in the conventional valve still 152 N/mm 2 ). The theoretical hydraulic/pneumatic compression strength of the housing modified according to the disclosure, owing to the use of the disclosure with the same outer dimensions and housing materials as the conventional valve were now 470 bar. This compression strength is sufficient to statistically (including material fluctuations) ensure a hydraulic/pneumatic compression strength of the housing of approximately 350 bar (that is to say, approximately 15% increased durability when the subject-matter of the disclosure is used compared with the conventional structure).
As can be seen clearly in FIG. 1 , there is produced during the individual cross-section adaptation of the respective channel rounded portions in the peripheral grooves 4 and 6 which are connected to the connections A and B which can be pressure-loaded, a groove cross-section which is asymmetrical with respect to the groove cross-section center axis, whereas the rounded channel portion of at least the two tank channels (peripheral grooves) 3 and 7 and in this instance also the central channel (peripheral groove) 5 which is in fluid connection with the pressure connection P, remain symmetrical.
Finally, it should be noted that the individual rounding of the groove cross-sections can be calculated based on models or established analytically in tests. During the individual adaptation of the channel rounding to the material stresses which actually occur, taking into account the different pressure/tensile durability of the housing material used, an asymmetry in the groove cross-section does not necessarily have to occur, as shown in the present example of channel 5 . Instead or in addition, this is because it is also conceivable for the channel cross-section to change symmetrically and/or asymmetrically not (not only) in the transverse channel direction but also (instead) in the peripheral direction of the peripheral groove. Furthermore, it is practically possible for the two outer peripheral grooves 3 and 7 which are connected in fluid terms to the tank connections TA, TB and/or the centrally arranged peripheral groove 5 also to each have a rounded channel portion which is asymmetrical in the groove cross-section and which has two different radii with respect to the groove cross-section center axis, as depicted in FIG. 3 .
The adaptation of the curvature paths or the occurrences of asymmetry to the prevailing stress progressions in the housing material may also lead to the rounded channel portions being constructed in an asymmetrical manner not only in the peripheral groove cross-section, but also or alternatively with respect to the longitudinal axis of the valve bore or in the peripheral direction of the respective peripheral groove (in the longitudinal groove section). Finally, the different radii r 1 , r 2 for the channels 4 and 6 according to the present embodiment do not necessarily have to be the same but can instead assume different values for each channel.
LIST OF REFERENCE NUMERALS
1 Housing
2 Valve piston chamber
3 to 7 Peripheral grooves
8 Channel bridge
A, P, B Pressure connections
TA, TB Tank connections
r 1 , r 2 Radii of the rounded channel portion
Pf 1 , Pf 2 Material stress arrows
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A housing of a pressure-loaded component includes a pressure-loaded channel system which corresponds to the tensile and/or compressive strength properties of the housing material and to the tensile and/or compressive stresses in the housing material during operation of the pressure-loaded component. The housing also includes a channel rounded profile configured to be adapted to include a formed asymmetry. The formed asymmetry is configured to reduce tensile stresses occurring in operation and thus increase the load carrying capacity of the housing as a whole.
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BACKGROUND OF THE INVENTION
This invention relates to precision mechanical positioning apparatus with particular application in translating physical position into an electronic format.
Encoders of various configurations have been utilized to translate information from the physical world to the electronic format required for calculation and further processing. These "sensors" have wide applicability in moving machinery and in rotating machinery in particular. Servo mechanisms, such as used in robotics and other industrical applications, have particular need for precise locating sensors which can reliably and quickly provide an input to a digital or analog control system to provide feedback knowledge with respect to current position. Thereafter, rate of change of that position as velocity is readily determined when required. Typically, an aperture is provided in a moving shutter plate which will allow light to pass between a light source and an optically sensitive sensor which will indicate the position when the aperture is properly positioned therebetween. This basic configuration has limitations in the numbers of sensors as well as the size and placement of apertures in the rotating shutterplate. Furthermore, to obtain improved resolution, a direct function is related between the numbers of apertures and sensor tracks and the resolution capability.
SUMMARY
Accordingly, it is an object of the present invention to provide a motion encoder capable of amplifying actual motion and thereby reducing the numbers of sensor tracks required. In so meeting this objective, the size of the encoder may be reduced, design simplified, and a high resolution obtained simultaneously.
Briefly, and in accordance with the present invention, a motion encoder comprises a first aperture plate having a first predetermined plurality of evenly spaced apertures therein, a second aperture plate in a spaced parallel relationship with the first aperture plate and having a second predetermined plurality of apertures evenly spaced therein, the number of the second predetermined plurality different from the first, and cooperative coupling means for movement of said first aperture plate with respect to the second aperture plate whereby select members of the plurality of apertures in the first aperture plate variably align with select members of the plurality of apertures in the second aperture plate as a direct function of the movement, wherein the variable alignment occurs at an apparent speed greater than the actual movement.
In one embodiment in accordance with the present invention, an apparent motion amplifier comprises first and second shutter means disposed in a rotatably attached and spaced parallel relationship, each having a respective plurality of apertures evenly spaced in an annular pattern, coordinated with respect to each other, one shutter having fewer apertures than the other, the first and second shutter means coincident upon a single axis of rotation and for amplifying apparent motion.
In a preferred embodiment, an amplifier as above further comprises a coarse position index aperture disposed on one of said shutter means and having a minimum size defined by the maximum number of adjacent sensors which may be simultaneously activated, plus at least one. Therefore the index aperture located on one or the other of the cooperating shutter means is constructed to incorporate at least three apertures when two adjacent sensors may be simultaneously activated. The index aperture may be larger.
Additionally a detented system may be used having a mechanical index such as a ball bearing and spring detent or an optical fine index to simplify operation.
BRIEF DESCRIPTION OF THE DRAWINGS
The operation of the present invention will become apparent to those skilled in the art upon reference to the following drawings in which:
FIGS. 1a-c are a simplified representation of one embodiment of a non-detented amplified motion encoder in accordance with the present invention.
FIGS. 2a-e are respective timing diagrams of the outputs of the sensors in FIG. 1c in proper relative positions.
FIGS. 3a-b are the two respective shutter plates in an embodiment of the present invention having a coarse index aperture.
FIGS. 4a-c are an embodiment combining two amplified motion encoders in accordance with the present invention in a back-to-back configuration.
FIGS. 5a-e are timing diagrams of a detented version of the present invention showing the outputs of the respective sensors in their proper relative positions.
DETAILED DESCRIPTION OF THE INVENTION
Referring now to FIG. 1a, the turning member of the amplified motion encoder in accordance with one implementation of the present invention, is shown in a relatively simple construction having four apertures 110 numbered 1-4 and positioned annularly in an evenly spaced pattern on aperture plate 112. The mounting provision for the rotatable input shaft is shown at 111.
Referring now to FIG. 1b, the stationary member of the aperture plate pair is shown, 114, having apertures 113 lettered A-E and shown superimposed over light sensors 115.
FIG. 1c is a combination of the turning aperture wheel 112 of FIG. 1a in combination with the stationary aperture wheel 114 shown on end. The light sensor board 116 has mounted thereon a plurality of light sensitive devices such as photocells or other optical switches, in the preferred embodiment, capable of receiving light from floodlight source 120. The rotational input shaft 119 provides movement relatively between plate 112 and plate 114, causing variable alignment of the apertures on each of the respective plates with the other apertures in accordance with the timing diagrams of FIG. 2.
Referring now to FIGS. 2a-2e, FIG. 2a shows the ON signal output by sensor and aperture combination a of FIG. 1b as a function of clockwise rotation of input shaft 119 of FIG. 1c. Likewise, FIGS. 2b-2e show the on versus off time as a function of such clockwise rotation of rotation input shaft 119, and therefore it can be seen that when shaft 119 is positioned between 0° and 9° from the starting position shown in FIG. 1a in combination with FIG. 1b, the region described as segment 210 is the combined output of the sensors on board 116 of FIG. 1c providing sensor A output high and sensors B, C, D and E, output low. When moving from 9° to 18°, in the region described by section 211, the outputs of the sensors on board 116 are as follows: sensor A and B high, sensors C, D and E low. In the region described by section 212, the outputs of the sensors are as follows: sensor A low, sensor B high, sensors C, D and E low. This pattern continues through the clockwise rotation of input shaft 119 until 90° is reached, at which point the pattern begins to repeat itself. Thus, in the embodiment shown in FIG. 1, the resolution for 90° rotation is a ten-part encodable output, resulting in a position determination having forty distinct locations for a 360° rotation of the input shaft.
One aspect of the present invention is the necessity to determine which of the repeated patterns and therefore rotational quadrants the shaft is positioned in. This is accomplished by utilizing a coarse index aperture, item 320 of FIG. 3b which will provide information as to which of the four quadrants of the 360° rotation pattern is being occupied. This coarse index aperture is required for either the detented or non-detented embodiments.
An important aspect of the present invention is the requirement to appreciate the apparent amplification of motion in that for every complete rotation of the turning aperture wheel 112, the apparent alignment of various select apertures on turning aperture wheel 112 with the stationary aperture wheel 114 and its associated apertures, will make four complete revolutions. For example, at the starting position shown in FIG. 2 by the section 210, aperture 1 on aperture wheel 112 is in direct alignment with aperture A on aperture wheel 114. This provides the high output shown in FIG. 2a between 0° and 9°. As the turning aperture wheel 112 rotates clockwise, the next aperture on wheel 112 to come into alignment with an aperture on wheel 114 will be aperture 4 which will align with aperture B. This occurs since the number of apertures on wheel 112 is less than the number of apertures on wheel 114 and, since both sets of apertures are evenly spaced, the distance between apertures on aperture wheel 112 (with fewer apertures) is greater than the distance between apertures on wheel 114 (with more). Thus, as aperture 4 aligns with aperture b, the clockwise rotation segment from 9°-18° provides for a high output from sensors A, B, and still low outputs from sensors C-E. Subsequently, aperture 1 is no longer in alignment with aperture A, but is moving into the region 18°-27°, providing the corresponding output shown by section 212. Therefore it can readily be seen that the actual motion, limited to rotation of the few degrees in actuality, results in an apparent aperture alignment and therefore amplified motion in the opposite direction on the order of four times faster than the actual movement for this embodiment.
It should be noted that a key aspect of the operation of the present invention in this regard is the difference between the numbers of apertures resulting in different distances between apertures. Additionally, the alignment of the apertures is a necessary function of the invention requiring the distance from the center of rotation for the position of each aperture set to be substantially identical.
Although described with respect to a relatively simple exemplary embodiment, it can be seen that the numbers of apertures can be increased to improve resolution, improve amplification, or reduced to accommodate sizing requirements. In this embodiment, the same pattern could have been generated by four rotations of a plate with only a single aperture on turning plate 112. This apparent amplification is therefore a function of the number of apertures as well as a function of the difference in number between the two relatively moving aperture plates.
Additionally, although an aperture described herein generally is a void in a shutter plate allowing light to pass therethrough, and as a result intercommunication is possible between an optically coupled source and sensor pair or floodlight source and photoelectric sensor combination, the present invention is equally applicable in many other sensor technologies such as Hall effect, etc., in addition to light sensors. Accordingly, the term aperture as used in this document is defined as a structure capable of stimulating a physical response in a sensor utilizing heat, light, sound, pressure, or magnetism, to produce a resulting impulse.
DESIGN CONSIDERATION
The following relationships must be maintained to build an operational encoder, providing that n 1 equals the number of stationary apertures/sensors, and n 2 equals the number of rotating aperture positions, and further defining N 12 equals the resolution of the resulting encoder, and further that n 1 equals Km 1 and n 2 equals Km 2 where n 1 , n 2 , m 1 , m 2 , K, and N 12 are integers, m 1 and m 2 are mutually prime, and K is larger than 1. The following formula defines the relationship:
N.sub.12 =2Km.sub.1 m.sub.2 =(2n.sub.1 n.sub.2 /K)
From the foregoing, it can be seen that n 1 and n 2 may be any two integers which are not factors of each other, and which have a common integer factor larger than one. If K is the largest common factor of n 1 and n 2 , then an encoder requiring detents may be made with (n 1 ×n 2 )/K unique positions in a single turn. A nondetented encoder may be made with [2(n 1 ×n 2 )]/K unique positions. Since the nondetented encoder will still work with the detent, and since it provides twice the resolution with no additional sensors, it is a preferred embodiment.
For example, utilizing an encoder having n 1 =10, and n 2 =12, the resolution will be defined by
2(2×5×6)=(2×10×12)/2=10×12=120
This discussion has been directed toward defining the resolution which is necessarily a function of the number of apertures of one of the plates with respect to the other. It can be seen that there must exist a difference between n 1 and n 2 and that such difference is an important consideration in defining resolution and designing such an encoder.
Furthermore, the need for determining which quadrant the moving aperture plate is physically located in, as in the previous example (FIG. 1, 2) leads to an additional inventive aspect of the present invention in the index aperture. Referring now to FIGS. 3a, b, the aperture plate 310 is shown having ten apertures 312 for use in combination with aperture plate 314 of FIG. 3b having a design aperture capability for twelve apertures 316, as was discussed previously. However, the combination of the coarse index requirement results in a much larger aperture incorporating five of the spaces for apertures 316 to provide for index aperture opening 320. The relative spacing of apertures 316 remains as if there were actually twelve apertures. This results in the same closer spacing of apertures 316 relative to apertures 312 to develop the amplified motion. Without the index aperture, no more than two adjacent stationary apertures 312 will be illuminated, and therefore in a high signal state, at any time. With the index aperture, and in the embodiment shown in FIG. 3b at least three adjacent apertures 312 will be open to illumination at any position of rotation of aperture plate 314 resulting in ready identification of the coarse position or quadrant location as previously discussed, as well as fine location through the amplified motion of the combination of apertures 316 with apertures 312. The required common factor of n 1 and n 2 ensures that the amplified motion pattern is duplicated K times at evenly spaced intervals around the aperture plates. This guarantees that at least one of the apertures 312 will be activated separately from those under aperture 320. Therefore this combination is a preferred embodiment which maintains a precision resolution and apparent amplified motion while eliminating the need for mechanical detent. The size of the coarse index aperture 320 must be large enough to ensure that it is readily distinguished from the normal amplified motion pattern. In a preferred embodiment with output patterns as shown in FIG. 2, this requires that the coarse index aperture be at least three positions.
It is also an object of the invention that the coarse position index aperture be aligned along the same radius of the rotating aperture plate on the individual fine position apertures, thus utilizing the same sensor for both fine and coarse position determination. Additionally, all sensors and objects should be aligned on that same radius of the aperture plates, effectively requiring only one encoding track, thus simplifying the design and manufacture of the encoders while allowing a smaller package size.
Referring now to FIG. 4a a combination of two amplified motion encoders is shown having sensor plate 414, stationary aperture plates 413, rotating aperture plate 415 geared through idler 410 to rotating aperture plate 412, and light sources 411 for lighting through the combination of rotating plate 412 and light sources 416 for lighting through the combination with rotating aperture plate 415. It is suggested that the combination of gearing through the idler 410 and rotating aperture plates 412 and 415 may be selected in accordance with principles well-known in the art to provide for any desired degree of resolution for shaft 417. A sensor construction such as shown in FIG. 4b having a reflector 430, sensors 432 and a central mounting structure 434, could be readily applied in the structure of FIG. 4a with the detail as is shown in FIG. 4c having sensor 458 mounted on a central mounting structure 456, in close proximity with rotating aperture plate 452 and the aperture 451 in alignment with reflector 450 for stimulating sensor 458. This combination facilitates ready implementation of the novel and unobvious aspects of the present invention in a wide variety of applications.
Another advantage of the present invention is that the use of the combination of two aperture plates tends to provide a parallel path to the sensors, for many of the disclosed embodiments herein. This results in a more narrowly defined light signal, and correspondingly sharper output signals.
Referring now to FIG. 5, the similarity between the timing diagrams of FIGS. 5a-e with those of FIGS. 2a-e, is intentional, so that the practitioner may readily discern the differences between the non-detented version of FIG. 2 and the detented version of FIG. 5. The ambiguity in the region 511 is eliminated by precluding a valid output while occupying this region. A mechanical detent holds the structure in regions 510, 512, etc. to eliminate the potential for the ambiguity caused by the similarity of the combined outputs in regions 9°-18°, 27°-36°, and so forth. Again, the coarse position index aperture will define the appropriate quadrant position, in this embodiment. The region 510 for the clockwise rotation of the input shaft of FIG. 1 is essentially the same output for 0°-9° rotation. However, the segment from 9°-18° shown as section 511 provides low output signals for all five sensors. Similarly, this pattern is repeated and low outputs will be received for segments from 27°-36°, 45°-54°, 63°-72°, and 81°-90°. These locations are undefined. Therefore, either a hardware detent or a fine position index may be used, as known in the art, to prevent any attempt to decode this position.
Other modifications of the disclosed embodiments may become apparent to persons skilled in the art without departing from the spirit and scope of the invention as defined by the appended claims.
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A single turn absolute position encoder is disclosed capable of being manufactured in extremely small size while maintaining high resolution. An indented version having a discrete position output signal is disclosed as well as a non-indented continuous position output device having an index for coarse position location as well as apertures for fine position location. This device may be designed for extremely high resolution in a single turn device, or may be geared to further improve resolution.
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BACKGROUND INFORMATION
[0001] A cable tie is used for fastening, binding, bundling, and/or organizing cables/wires. Different types of cable ties are made for use in different environments and applications. For example, some cable ties are made for outdoor use. Some cable ties are made for a specific industry, such as the food industry. Some are made for heavy-duty use (e.g., cable ties made of metal), for bundling large cables.
BRIEF DESCRIPTION OF THE DRAWINGS
[0002] The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate one or more embodiments described herein and, together with the description, explain the embodiments. In the drawings:
[0003] FIG. 1A is an isometric perspective top/side view of an exemplary cable tie in an open configuration according to one implementation;
[0004] FIG. 1B is an isometric perspective bottom/side view of the cable tie of FIG. 1A in the open configuration;
[0005] FIG. 2 is an expanded isometric perspective top/side view of the cable tie of FIG. 1A in the closed configuration;
[0006] FIG. 3 is an isometric cut-away perspective top/side view of the cable tie of FIG. 1A in the closed configuration;
[0007] FIG. 4A is a cross-sectional side view of the cable tie before an end of the cable tie of FIG. 1A is inserted into a locking body of the cable tie;
[0008] FIG. 4B is a cross-sectional side view of the cable tie when the end of the cable tie of FIG. 1A is partially inserted into the locking body of the cable tie;
[0009] FIG. 4C is a cross-sectional side view of the cable tie after the end of the cable tie of FIG. 1A is partially inserted into the locking body and the cable tie is in the closed configuration;
[0010] FIG. 5A is an isometric cut-away perspective top/side view of the cable tie according to another implementation;
[0011] FIG. 5B is an isometric cut-away perspective top/side view of the cable tie according to yet another implementation; and
[0012] FIGS. 6A-6C are cross-sectional side views of the cable tie according to different implementations.
DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS
[0013] The following detailed description refers to the accompanying drawings. The same reference numbers in different drawings may identify the same or similar elements.
[0014] As described herein, an anti-slip cable tie provides for a small/minimum slack in binding, fastening or bundling cables. To tie/bundle cables using the anti-slip cable tie, one end of a band, of the cable tie, that encircles the cables is inserted into the housing of a locking body of the cable tie. When the end of the band is inserted within the housing of the locking body, the band pushes a ball bearing within the housing toward an inner wall of the housing. Another ball within the housing, however, prevents the ball bearing from moving backwards beyond a point and bumping into the inner wall. When the band is pulled/tugged in the forward direction away from the inner wall, the ball bearing, being close to a front of the wall, prevents the end of the band from slipping and locks the band in place. Because the other ball prevents the ball bearing from moving about in the housing, the ball bearing continues to lock the band in place.
[0015] FIG. 1A shows an isometric perspective top/side view of an exemplary cable tie 100 in an open configuration according to one implementation, together with an xyz-axes 101 . As shown, cable tie 100 includes locking body 102 and a band 104 . In FIG. 1A , cable tie 100 is oriented such that band 104 extends along the x-axis of xyz-axes 101 and the unit normal vector of the flat surface of band 104 is parallel to the z-axis. Band 104 has an interior portion inside of housing 108 .
[0016] When band 104 is wrapped about cables and an end of band 104 (e.g., section 116 - 3 ) is inserted within locking body 102 , locking body 102 prevents the end from slipping back out of locking body 102 and the band from unwrapping about the cables.
[0017] Locking body 102 includes a side wall 106 - 1 , a top wall 106 - 2 , a side wall 106 - 3 , bottom walls 106 - 4 and 106 - 5 (shown in FIG. 1B ), and housing 108 . Walls 106 - 1 through 106 - 5 (collectively referred to as “walls 106 ”) extend along the x-axis from a side face 112 - 1 to a side face 112 - 2 (shown in FIG. 1B ). In one implementation, walls 106 may be made of one continuous strip of rigid material wrapped (e.g., loosely) about band 104 , such that there is a gap/opening 114 - 1 and gap/opening 114 - 2 ( FIG. 1B ) between walls 106 and band 104 .
[0018] Housing 108 includes a side portion 110 - 1 (also referred to as a “stop 1101 -”), a top portion 110 - 2 , and a side portion 110 - 3 (collectively referred to as “portions 110 ”). As further described below, portions 110 are configured/shaped to enclose and interact with elements within housing 108 , to prevent a portion of band 104 (which was inserted through opening 114 - 1 and 114 - 2 ) from sliding out from housing 108 when anti-slip cable tie 100 is in the closed configuration. In FIG. 1A , housing 108 is in the shape of a dome, and may be made of steel, plastic, or another suitable material.
[0019] Band 104 includes an entrance section 116 - 1 , a middle section 116 - 2 , and an end section 116 - 3 . Band 104 also includes a side edge 120 - 1 , a front edge 120 - 2 , and a side edge 120 - 3 (not shown). In one embodiment, side edge 120 - 1 and front edge 120 - 2 form an acute angle, such that, along the side edge 120 - 1 and parallel to the x-axis, the end of band 104 tapers to a tip 122 that can be more easily inserted into a gap/opening 114 - 2 (see FIG. 1B ) after band 104 is bound around cables/wires, to result in a closed (loop) configuration. The end of tip 122 may be rounded, so that a user may not easily and accidentally puncture oneself with tip 122 . In one embodiment, when band 104 binds/bundles cables/wires, bottom surface 118 - 2 ( FIG. 1B ) of band 104 may face the cables/wires and be in contact with the cables/wires. Band 104 may be made of flexible material, such as steel, or another material.
[0020] FIG. 1B shows an isometric perspective bottom/side view of cable tie 100 in an open configuration, together with an xyz-axes 101 . FIG. 1B illustrates a number of features, of cable tie 100 , that are not shown in FIG. 1A . For example, FIG. 1B shows side edge 112 - 2 with gap/opening 114 - 2 . FIG. 1B also shows band 104 extending from entrance portion 116 - 1 into locking body 102 (along the negative axis) and exiting from locking body 102 via opening 114 - 2 to form a clip 124 with a flap 126 that covers bottom walls 106 - 4 and 106 - 5 in the direction of the x-axis. As shown, clip 124 and flap 126 are integrally formed with band 104 . In a different implementation, clip 124 and flap 126 may be constructed separately from band 104 and then affixed together via screws or another mechanism.
[0021] As shown in FIG. 1B , flap 126 includes, in one embodiment, at about the middle of its surface, a tab 128 with a crease 130 . Bottom walls 106 - 4 and 106 - 5 above tab 128 has a hole (e.g., a square hole whose front edge is aligned with a front edge of tab 128 ) (not shown in FIG 1B ). Tab 128 is thrust upward in the direction of arrow 129 into the hole, bent about crease 130 (e.g., in the direction of the z-axis).
[0022] In this configuration, side walls 106 - 1 and 106 - 3 of locking body 102 , clip 124 , and tab 128 hold/affix a portion of locking body 102 to an interior portion of band 104 , with the bottom surface 118 - 2 of band 104 being flush with an interior surface (the surface within locking body 102 ) of bottom walls 106 - 4 and 106 - 5 and the top surface of flap 126 being flush with the exterior surface (the surface in the z-direction) of bottom walls 106 - 4 and 106 - 5 . Side walls 106 - 1 and 106 - 3 prevent the interior portion of band 104 from moving laterally in the negative/positive y-direction with respect to locking body 102 . Clip 124 , which is integral to band 124 , prevents locking body 102 from sliding in the negative/positive x-direction relative to the interior portion of band 104 . Tab 128 , having been pushed into the hole in bottom walls 106 - 4 and 106 - 5 , catches an edge of the hole when an external force is applied to locking body 102 relative to the interior portion of band 104 in the positive x-direction. Tab 128 and the hole prevents locking body 102 from sliding in the x-direction relative to the interior portion of band 104 .
[0023] FIG. 2 is an expanded isometric perspective top/side view of cable tie 100 in the closed configuration. In FIG. 2 , end portion 116 - 3 of band 104 has been inserted into gap/hole 114 - 2 formed at side wall 112 - 2 of locking body 102 , and passed through and out of locking body 102 via gap/hole 114 - 1 , resulting in the closed configuration. In the configuration, a section/portion of band 104 (e.g., end section 116 - 3 ) overlaps with entrance portion 116 - 1 of band 104 . In FIG. 2 , bottom surface 118 - 2 of end section 116 - 3 would be in contact with the top surface 118 - 1 of entrance section 116 - 1 .
[0024] FIG. 3 is an isometric cut-away perspective top/side view of cable tie 100 in the closed configuration. FIG. 3 shows a number of features that are not visible in FIG. 1A through FIG. 2 . As shown, housing 108 encloses space 302 in which a ball bearing 304 and sphere 306 are placed. In one implementation, ball bearing 304 may be made of metal (e.g., steel) and sphere 306 may be made of elastomeric or another material (e.g., plastic, rubber, sponge-like or spring-like material, stainless steel sponge, etc.). In the implementation illustrated in FIG. 3 , ball bearing 304 and sphere 306 may have approximately the same diameter. In other implementations, the diameters may be different.
[0025] FIG. 3 also shows entrance portion 116 - 1 extending into housing 108 as an interior section/portion 308 , which joins clip 124 . In the closed configuration, interior section 308 is underneath end section 116 - 3 and above bottom walls 106 - 4 and 106 - 5 . In FIG. 3 , bottom wall 106 - 4 is illustrated as having front area 310 - 1 and a rear area 310 - 2 . Between front area 310 - 1 and rear area 310 - 2 is a rectangular/square hole 312 , into which tab 128 protrudes in the direction of arrow 129 . As explained above, an edge of tab 128 engages an edge of square hole 312 if housing 108 is pushed/pulled in the x-direction relative to interior section 308 . and prevents housing 108 from sliding in the x-direction relative to interior section 308 (e.g., prevents housing 108 from detaching from interior portion 308 of band 104 ).
[0026] FIGS. 4A through 4C are cross sectional side views of cable tie 100 at different stages of closing cable tie 100 into a loop. FIG. 4A is a cross sectional side view of cable tie 100 before end section 116 - 3 of band 104 is inserted into locking body 102 via gap/opening 114 - 2 to be in the closed configuration. Like FIG. 3 , FIG. 4A shows ball bearing 304 and sphere 306 occupying space 302 of housing 108 .
[0027] FIG. 4B is a cross sectional side view of cable tie 100 when end section 116 - 1 of band 104 is partially inserted into locking body 102 of cable tie 100 . Un FIG. 4B , after band 104 is wrapped about a bundle of cables/wires, end section 116 - 3 is pushed in the direction of arrow 406 via gap/opening 114 - 2 into housing 108 . Consequently, end section 116 - 3 overlaps with interior section 308 . As end section, 116 - 3 moves further in the direction of arrow 406 , section 116 - 3 also pushes ball bearing 304 , causing ball bearing 308 to move in the direction of arrow 408 , such that section 11603 may slide underneath ball bearing 108 . In addition, section 116 - 3 also pushes ball bearing 304 in the direction of arrow 410 , causing an area 412 on ball bearing 304 to contact an area 414 of sphere 306 . Although the force on area 414 pushes sphere 416 in the direction of arrow 416 , because area 418 of sphere 416 is in contact with stop 110 - 1 (or the interior surface of side portion 110 - 1 ) of housing 108 , sphere 306 moves, in the direction of x-axis, little or no distance. Accordingly, sphere 306 prevents ball bearing 304 from moving further in the direction of arrow 410 and touching stop 110 - 1 .
[0028] FIG. 4C is a cross sectional side view of cable tie 100 after end section 116 - 3 of band 104 is inserted into locking body 102 and cable tie 100 is in the closed configuration. In FIG. 4C , having been inserted fully into housing 108 , end section 116 - 3 overlaps with entrance section 116 - 1 . From this position, if band 104 is pulled in the direction of arrow 419 , the frictional force between band 104 and ball bearing 304 causes ball bearing 304 to move in the direction of arrow 420 to the extent that there is space/clearance in space 302 . Because space 302 within housing 108 is tapered in the negative x-direction, as ball bearing 304 is driven in the direction of arrow 420 until ball contacts the surface of portion 110 - 3 (also referred to as “stop 110 - 3 ”), area 424 and 422 of ball bearing 304 exert increasing force on the interior surface of portion 110 - 3 of housing 108 and on the top surface of end section 116 - 3 of band 104 , respectively. The downward force exerted by area 422 of ball bearing 304 on end section 116 - 3 may pinch end section 116 - 3 between ball bearing 304 and interior section 308 , and thus prevent end section 116 - 3 from retreating back in the direction of arrow 410 through gap/opening 114 - 2 . That is, ball bearing 304 provides for the locking mechanism of cable tie 100 .
[0029] As briefly discussed above, in a different embodiment without sphere 306 in space 302 , when end section 116 - 3 is inserted into housing 108 , end section 116 - 3 may cause ball bearing 304 to move all the way (or significant portion of the way) to stop 110 - 1 of housing 108 . With ball bearing 304 in such a position, if band 104 were pulled back in the direction of arrow 419 (e.g., due to the weight of cables that are bound by cable tie 100 ), as end section 116 - 3 moves in the same direction relative to housing 108 , ball bearing 304 would also move from the stop 110 - 1 of housing 108 toward the interior surface of portion 110 - 3 of housing 108 , until ball bearing 304 locks end section 116 - 3 , and, therefore, band 104 . The distance covered by ball bearing 304 until ball bearing 304 locks band 104 is approximately the amount of slippage of band 104 allowed by cable tie 100 . The slippage may result in an undesirable amount of slack in band 104 when cable tie 100 is in the closed configuration, with band 104 wrapped about cables/wires.
[0030] In contrast, with sphere 306 in place as illustrated in FIGS. 3, 4A, 4B, and 4C , ball bearing 304 cannot move in the direction of arrow 410 when end section 116 - 3 is inserted into housing 108 (or can only move a small amount). Hence, when band 104 is pulled in the direction of arrow 419 (e.g., by the weight of the cables that are wrapped by band 104 ), ball bearing 304 cannot travel a significant distance until ball bearing 304 locks band 104 . In other words, sphere 306 prevents band 104 from slipping, and thus creating slack between band 104 and the cables bundled by cable tie 100 (e.g., slipping distance<the distance occupied by sphere 306 (e.g., the diameter)).
[0031] FIG. 5A is an isometric cut-away perspective top/side view of cable tie 100 according to another implementation. In this implementation, cable tie 100 includes, in the place of sphere 306 , a cylinder 502 . Cylinder 502 may play a role similar to that of sphere 306 in the implementations described above.
[0032] FIG. 5B is an isometric cut-away perspective top/side view of cable tie 100 according to another implementation. In this implementation, cable tie 100 includes, in the place of sphere 306 , a block 504 . Block 504 may prevent ball bearing 304 from allowing undesirable slippage of band 104 when band 104 is closed around cables/wires, in a manner similar to that described above for sphere 306 (e.g., by occupying a space between ball bearing 304 and stop of housing 108 .
[0033] FIGS. 6A-6C are cross-sectional side views of cable tie 100 according to other, different implementations. FIG. 6A shows the cross-sectional view of cable tie 100 according to one implementation. In this implementation, ball bearing 604 , square/cube 606 and side portions 602 - 1 through 602 - 3 replace ball bearing 304 , sphere 306 , and side portions 110 - 1 through 110 - 3 , respectively, illustrated in FIGS. 4A-4C . Furthermore, each of ball bearing 604 , resilient cube 606 , side portions 602 - 1 through 602 - 3 has a functional role corresponding to the role of bearing 304 , sphere 306 , and side portions 110 - 1 through 110 - 3 , respectively. In addition, resilient cube 606 acts as a spring between bearing 604 and side portion 110 - 1 . Cube 606 exerts a pressure on bearing 604 by pushing against side portion 602 - 1 and bearing 604 . This prevents bearing 604 from moving away substantially from portion 602 - 3 , and reducing the force on section 116 - 3 when section 116 - 3 is fully inserted in housing 108 .
[0034] In a typical implementation, resilient cube 606 may be made of stainless steel wire mesh. Depending on the implementation, resilient cube 606 may be replaced by a stainless steel mesh of another shape, such as a round ball, cylinder, rectangular box/prism, etc. In contrast to portions 110 in FIGS. 4A-4C , portions 602 may be longer or shorter—that is, portions 603 may extend to properly accommodate resilient cube 606 .
[0035] FIG. 6B shows the cross-sectional view of cable tie 100 according to yet another implementation. In this implementation, ball bearing 608 and sphere 610 and side portions 612 - 1 through 612 - 3 replace ball bearing 304 , sphere 306 , and side portions 110 - 1 through 110 - 3 , respectively, illustrated in FIGS. 4A-4C . Each of ball bearing 608 , sphere 610 , side portions 612 - 1 through 612 - 3 has a functional role similar to the role of bearing 304 , sphere 306 , and side portions 110 - 1 through 110 - 3 , respectively. In this implementation, ball bearing 608 is smaller (i.e., has a smaller diameter) than sphere 610 such that ball bearing 608 occupies slack/room in housing 108 . Ball bearing 608 and sphere 610 prevents each other from “sloshing” in housing 108 (by occupying the space in housing 108 ), and thus from reducing the force exerted by bearing 608 and/or sphere 610 on section 116 - 3 when section 116 - 3 is fully inserted in housing 108 .
[0036] Portions 612 may be dimensioned to properly accommodate ball bearing 608 and sphere 610 . In some implementations, both ball bearing 608 and sphere 610 may be composed of the same or similar materials (e.g., stainless steel).
[0037] FIG. 6C shows the cross-sectional view of cable tie 100 according to still yet another implementation. In this implementation, sphere 614 and replaces ball bearing 304 and sphere 306 , and portions 616 - 1 through 616 - 3 replace portions 110 - 1 through 110 - 3 illustrated in FIGS. 4A-4C . In FIG. 6C , portions 616 - 1 , 612 - 1 , and 616 - 3 are shaped/cut such that portions 616 - 1 and/or 616 - 2 (“housing 108 ” or buckle) act as backstop against sphere 614 . Once inserted into housing 108 , section 116 - 3 acts as a leaf spring on sphere 614 and pushes sphere 614 against portions 616 - 1 through 616 - 3 . That is, when section 116 - 3 of cable tie 100 is inserted in housing/buckle 108 , sphere 614 is pressed against portions 616 (e.g., especially portions 616 - 1 and 616 - 2 ) by section 116 - 3 . When section 116 - 3 is being pulled back out of housing 108 , sphere 614 is pulled toward portion 616 - 3 , which increases the force applied by section 116 - 3 against sphere 614 . This causes sphere 614 to increase its force on portion 616 - 3 , preventing section 116 - 3 from being pulled out of housing 108 . In this implementation, section 116 - 3 's leaf-spring action against sphere 614 and the shape of portions 616 prevent sphere 614 from moving substantially away from portion 616 - 3 . This causes sphere 614 to maintain constant pressure on section 116 - 3 and not allow section 116 - 3 to slip away from within housing 108 .
[0038] In some implementations, interior position 308 may include a “dimple” or a hole. In other implementations, interior portion 308 excludes (i.e., is without) a dimple or a hole. If a hole or a dimple exists on interior position 308 , when section 116 - 3 is fully inserted into housing 108 bearing/sphere (e.g., any one of bearing 304 , sphere 306 , cylinder 502 , cube 606 , bearing 608 , sphere 610 , or sphere 614 )) may drive the area (of section 116 - 3 ) bearing sits into the hole (on interior portion 308 ) underneath section 116 - 3 . In this way, the dimple or hole on interior position 308 may further stabilize the bearing/sphere, when section 116 - 3 is locked by the bearing/sphere.
[0039] The foregoing description of implementations provides illustration, but is not intended to be exhaustive or to limit the implementations to the precise form disclosed. Modifications and variations are possible in light of the above teachings or may be acquired from practice of the teachings. For example, in some implementations, housing 108 may be shaped differently than that illustrated in FIGS. 1-6C . Furthermore, in some implementations, more than a single sphere 306 , cylinder 502 , or block 504 may be placed within housing 108 to prevent ball bearing 304 from “sloshing” and allowing slippage of band 104 in the closed configuration. In some implementations, in place of sphere 306 or cylinder 502 , or block 504 , a spring or spring-like component may be places in housing 108 to prevent slippage. Furthermore, depending on the implementation, a different type of band 104 may be used in place of band 104 (e.g., thicker band, narrower band, etc.). In still other implementations, top surface 118 - 1 of band 104 , the interior surfaces of housing 108 and/or ball bearing 304 may include ridges to increase the friction between top surface 118 - 1 of band 104 , the interior surfaces of housing 108 , and/or ball bearing 304 .
[0040] Although different implementations have been described above, it is expressly understood that it will be apparent to persons skilled in the relevant art that the implementations may be modified without departing from the spirit of the invention. Various changes of form, design, or arrangement may be made to the invention without departing from the spirit and scope of the invention. Therefore, the above mentioned description is to be considered exemplary, rather than limiting, and the true scope of the invention is that defined in the following claims.
[0041] It should be emphasized that the term “comprises/comprising” when used in this specification is taken to specify the presence of stated features, integers, steps or components but does not preclude the presence or addition of one or more other features, integers, steps, components, or groups thereof.
[0042] No element, act, or instruction used in the present application should be construed as critical or essential to the implementations described herein unless explicitly described as such. Also, as used herein the article “a” is intended to include one or more items. Further, the phrase “based on” is intended to mean “based, at least in part, on” unless explicitly stated otherwise.
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A cable tie includes a band that extends lengthwise from a first end to a second end. The cable tie also includes a housing, affixed near the second end, with a first opening to receive the first end of the band when the first end of the band is brought toward the housing in a loop. The housing includes: walls that enclose a space and have a stop toward the second end of the band; a first mass in the space; and a second mass placed in the space and between the first mass and the stop. When the first end is inserted into the housing, the first end passes under the first mass and the second mass and exerts a pull on the first mass toward the second mass. When the first mass is pulled toward the second mass, the second mass acts as a spring between the first mass and the stop and prevents the first mass from hitting the stop. After the first end is inserted into the housing and when the first end is being pulled out of the housing, due to a force exerted by the second mass to the first mass and the walls, the first mass squeezes the first end against the bottom of the housing and locks the first end in the housing.
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FIELD OF THE INVENTION
The present invention relates to novel antidiabetic compounds, their tautomeric forms, their derivatives, their analogues, their stereoisomers, their polymorphs, their pharmaceutically acceptable salts, their pharmaceutically acceptable solvates and pharmaceutically acceptable compositions containing them. This invention particularly relates to novel azolidinediones of the general formula (I), their analogues, their derivatives, their tautomeric forms, their stereoisomers, their polymorphs, their pharmaceutically acceptable salts, pharmaceutically acceptable solvates and pharmaceutical compositions containing them.
The present invention also relates to a process for the preparation of the above said novel azolidinedione compounds, derivatives, analogues, tautomeric forms, stereoisomers, polymorphs, pharmaceutically acceptable salts, and pharmaceutically acceptable solvates; and pharmaceutical compositions containing them.
This invention also relates to novel intermediates, processes for preparing the intermediate and processes for using the intermediates.
The azolidinediones of the general formula (I) defined above of the present invention are useful for the treatment and/or prophylaxis of hyperlipidemia, hypercholesterolemia, hyperglycemia, osteoporosis, obesity, glucose intolerance, insulin resistance and also diseases or conditions in which insulin resistance is the underlying pathophysiological mechanism. Examples of these diseases and conditions are type II diabetes, impaired glucose tolerance, dyslipidaemia, hypertension, coronary heart disease and other cardiovascular disorders including atherosclerosis. The azolidinediones of formula (I) are useful for the treatment of insulin resistance associated with obesity and psoriasis. The azolidinediones of the formula (I) can also be used to treat diabetic complications and can be used for treatment and/or prophylaxis of other diseases and conditions such as polycystic ovarian syndrome (PCOS), certain renal diseases including diabetic nephropathy, glomerulonephritis, glomerular sclerosis, nephrotic syndrome, hypertensive nephrosclerosis, end-stage renal diseases and microalbuminuria as well as certain eating disorders, as aldose reductase inhibitors and for improving cognitive functions in dementia.
BACKGROUND OF THE INVENTION
Insulin resistance is the diminished ability of insulin to exert its biological action across a broad range of concentrations. In insulin resistance, the body secretes abnormally high amounts of insulin to compensate for this defect; failing which, the plasma glucose concentration inevitably rises and develops into diabetes. Among the developed countries, diabetes mellitus is a common problem and is associated with a variety of abnormalities including obesity, hypertension, hyperlipidemia (J. Clin. Invest., (1985) 75: 809-817; N. Engl. J. Med. (1987) 317: 350-357; J. Clin. Endocrinol. Metab., (1988) 66: 580-583; J. Clin. Invest., (1975) 68: 957-969) and other renal complications (See patent application Ser. No. WO 95/21608). It is now increasingly being, recognized that insulin resistance and relative hyperinsulinemia have a contributory role in obesity, hypertension, atherosclerosis and type 2 diabetes mellitus. The association of insulin resistance with obesity, hypertension and angina has been described as a syndrome having insulin resistance as the central pathogenic link-Syndrome-X. In addition, polycystic ovarian syndrome (patent application Ser. No. WO 95/07697), psoriasis (patent application Ser. No. WO 95/35108), dementia (Behavioral Brain Research (1996) 75: 1-11) etc. may also have insulin resistance as a central pathogenic feature. Recently, it has also been reported that insulin sensitizers improve the bone mineral density and thus may be useful for the treatment of osteoporosis (EP-783888).
A number of molecular defects have been associated with insulin resistance. These include reduced expression of insulin receptors on the plasma membrane of insulin responsive cells and alterations in the signal transduction pathways that become activated after insulin binds to its receptor including glucose transport and glycogen synthesis.
Since defective insulin action is thought to be more important than failure of insulin secretion in the development of non-insulin dependent diabetes mellitus and other related complications, this raises doubts about the intrinsic suitability of antidiabetic treatment that is based entirely upon stimulation of insulin release. Recently, Takeda has developed a new class of compounds which are the derivatives of 5-(4-alkoxybenzyl)-2,4-thiazolidinediones of the formula (II) (Ref. Chem. Pharm. Bull. 1982, 30, 3580-3600). In the formula (II), V represents substituted or unsubstituted divalent aromatic group B represents a sulfur atom or an oxygen atom and U represents various groups which have been reported in various patent documents.
By way of examples, U may represent the following groups:
(i) a group of the formula (IIa) where R 1 is hydrogen or hydrocarbon residue or heterocyclic residue which may each be substituted, R 2 is hydrogen or a lower alkyl which may be substituted by hydroxy group, X is an oxygen or sulphur atom, Z is a hydroxylated methylene or a carbonyl, m is 0 or 1, n is an integer of 1-3. These compounds have been disclosed in the European Patent Application No. 0 177 353
An example of these compounds is shown in formula (IIb)
(ii) a group of the formula (IIc) wherein R 1 and R 2 are the same or different and each represents hydrogen or C 1 -C 5 alkyl, R 3 represents hydrogen, acyl group, a (C 1 -C 6 ) alkoxycarbonyl group or aralkyloxycarbonyl group, R 4 -R 5 are same or different and each represent hydrogen, C 1 -C 5 alkyl or C 1 -C 5 alkoxy or R 4 , R 5 together represent C 1 -C 4 alkenedioxy group, n is 1, 2, or 3, W represents CH 2 , CO, CHOR 6 group in which R 6 represents any one of the items or groups defined for R 3 and may be the same or different from R 3 . These compounds are disclosed in the European Patent Application No. 0 139 421.
An example of these compounds is shown in (IId)
iii) A group of formula (IIe) where A 1 represents substituted or unsubstituted aromatic heterocyclic group, R 1 represents a hydrogen atom, alkyl group, acyl group, an aralkyl group wherein the aryl moiety may be substituted or unsubstituted, or a substituted or unsubstituted aryl group, n represents an integer in the range from 2 to 6. These compounds are disclosed in European Patent No. 0 306 228.
An example of this compound is shown in formula (IIf)
iv) A group of formula (IIg) where Y represents N or CR 5 , R 1 , R 2 , R 3 , R 4 and R 5 represents hydrogen, halogen, alkyl and the like and R 6 represents hydrogen, alkyl, aryl and the like, n represents an integer of 0 to 3. These compounds are disclosed in European Patent Application No. 0 604 983.
An example of this compound is shown in formula (IIh)
v) a group of formula (IIi), where R is (C 1 -C 6 ) alkyl groups, cycloalkyl group, furyl, thienyl, substituted or unsubstituted phenyl group, X is hydrogen, methyl, methoxy, chloro or fluoro. These compounds have been disclosed in the U.S. Pat. No. 5,037,842.
An example of these compounds is shown in formula (IIj).
(vi) a group of formula (IIk) wherein A 1 represents a substituted or unsubstituted aromatic heterocyclyl group; R 1 represents a hydrogen atom, an alkyl group, an acyl group, an aralkyl group, wherein the aryl moiety may be substituted or unsubstituted or a substituted or unsubstituted aryl group, n represents an integer in the range of from 2 to 6. These compounds have been disclosed in the patent application Ser. No. WO 92/02520.
An example of these compounds is shown in formula (IIl).
Some of the above referenced hitherto known antidiabetic compounds seem to possess bone marrow depression, liver and cardiac toxicities and modest potency and consequently, their regular use for the treatment and control of diabetes is becoming limited and restricted.
SUMMARY OF THE INVENTION
With an objective of developing new compounds for the treatment of type II diabetes [non-insulin-dependent-diabetes mellitus (NIDDM)] which could be more potent at relatively lower doses and having better efficacy with lower toxicity, we focused our research efforts in a direction of incorporating safety and to have better efficacy, which has resulted in the development of novel azolidinedione compounds having the general formula (I) as defined above.
The main objective of the present invention is therefore, to provide novel azolidinediones, their derivatives, their analogues, their tautomeric forms, their stereoisomers, their polymorphs, their pharmaceutically acceptable salts, their pharmaceutically acceptable solvates and pharmaceutical compositions containing them and mixtures thereof.
Another objective of the present invention is to provide novel azolidinedione compounds, their derivatives, their analogues, their tautomeric forms, their stereoisomers, their polymorphs, their pharmaceutically acceptable salts, their pharmaceutically acceptable solvates and pharmaceutical compositions containing them and mixtures thereof having enhanced activities, no toxic effect or reduced toxic effect.
Yet another objective of the present invention is to provide a process for the preparation of novel azolidinediones of the formula (I) as defined above, their tautomeric forms, their analogues, their derivatives, their stereoisomers, their polymorphs, their pharmaceutically acceptable salts and their pharmaceutically acceptable solvates.
Still another objective of the present invention is to provide pharmaceutical compositions containing compounds of the general formula (I), their tautomers, their stereoisomers, their derivatives, their analogues, their polymorphs, their salts, solvates or mixtures thereof in combination with suitable carriers, solvents, diluents, excipients and other media normally, employed in preparing such compositions.
Yet another objective of the present invention is to provide novel intermediates of the formula (III)
where G represents —CHO, —NO 2 , —NH 2 or —CH 2 CH(J)—COOR, where J represents halogen atom such as chlorine, bromine or iodine and R represents H or lower alkyl group such as (C 1 -C 6 ) alkyl group, preferably a (C 1 -C 3 ) alkyl group such as methyl, ethyl, or propyl; and R 1 , R 2 , R 3 , R 4 , R 5 , R 6 , X, W, n and Ar are defined as in formula (I).
Still another objective of the present invention is to provide a process for the preparation of the novel intermediates of the formula (III)
where G represents —CHO, —NO 2 , —NH 2 or —CH 2 CH(J)—COOR, where J represents halogen atom such as chlorine, bromine or iodine and R represents H or lower alkyl group such as (C 1 -C 6 ) alkyl group, preferably a (C 1 -C 3 ) alkyl group such as methyl, ethyl, or propyl; and R 1 , R 2 , R 3 , R 4 , R 5 , R 6 , X, W, n and Ar are defined as in formula (I).
DETAILED DESCRIPTION OF THE INVENTION
Azolidinediones of the present invention have the general formula (I)
In the above formula (I), X represents O or S; the groups R 1 , R 2 , R 3 , R 4 may be same or different and represent hydrogen, halogen, hydroxy, cyano, nitro; optionally substituted groups selected from alkyl, cycloalkyl, alkoxy, cycloalkyloxy, aryl, aralkyl, heteroaryl, heteroaralkyl, heterocyclyl, aryloxy, alkoxycarbonyl, aryloxycarbonyl, aralkoxycarbonyl, alkylamino, arylamino, amino, aminoalkyl, hydroxyalkyl, alkoxyalkyl, thioalkyl, alkylthio, acyl, acylamino, aryloxycarbonylamino, aralkoxycarbonylamino, alkoxycarbonylamino, carboxylic acid or its derivatives, acyloxy, sulfonic acid or its derivatives; W represents O, S or a group NR 9 ; R 6 and R 9 may be same or different and represent hydrogen; or optionally substituted alkyl, cycloalkyl, aryl, aralkyl, heterocyclyl, heteroaryl, heteroaralkyl, acyl, hydroxyalkyl, aminoalkyl, alkoxycarbonyl, aryloxycarbonyl, aralkoxycarbonyl, alkoxyalkyl, alkylthio, or thioalkyl groups; R 5 represents hydrogen, hydroxy, or halogen atom or optionally substituted alkyl, aryl, heteroaryl, acyl, alkoxy, aralkyl, or aralkoxy; n is an integer ranging from 1-4; Ar represent an optionally substituted divalent aromatic or heterocyclic group; R 7 and R 8 may be same or different and individually represents hydrogen atom, halogen, hydroxy, lower alkyl, optionally substituted aralkyl group or together form a bond; and B represents an oxygen atom or a sulfur atom.
Suitable groups represented by R 1 , R 2 , R 3 , R 4 may be selected from hydrogen, halogen atom such as fluorine, chlorine, bromine, or iodine; hydroxy, cyano, nitro; substituted or unsubstituted (C 1 -C 12 )alkyl group, especially, linear or branched (C 1 -C 6 )alkyl group, such as methyl, ethyl, n-propyl, isopropyl, n-butyl, iso-butyl, t-butyl, n-pentyl, isopentyl, hexyl and the like; cycloalkyl group such as cyclopropyl, cyclobutyl, cyclopentyl, cyclohexyl and the like, cycloalkyl group may be substituted; cycloalkyloxy group such as cyclopropyloxy, cyclobutyloxy, cyclopentyloxy, cyclohexyloxy and the like, cycloalkyloxy group may be substituted; aryl group such as phenyl or naphthyl, the aryl group may be substituted; aralkyl such as benzyl or phenethyl, the aralkyl group may be substituted; heteroaryl group such as pyridyl, thienyl, furyl, pyrrolyl, oxazolyl, thiazolyl, imidazolyl, oxadiazolyl, tetrazolyl, benzopyranyl, benzofuranyl and the like, the heteroaryl group may be substituted; heteroaralkyl wherein the heteroaryl moiety as defined earlier and is attached to (C 1 -C 3 ) alkylene group such as furanmethyl, pyridinemethyl, oxazolemethyl, oxazolethyl, and the like, the heteroaralkyl group may be substituted; heterocyclyl groups such as aziridinyl, pyrrolidinyl, morpholinyl, piperidinyl, piperazinyl and the like, the heterocyclyl group may be substituted; aryloxy such as phenoxy, naphthyloxy, the aryloxy group may be substituted; alkoxycarbonyl such as methoxycarbonyl or ethoxycarbonyl, the alkoxycarbonyl group may be substituted; aryloxycarbonyl group such as optionally substituted phenoxycarbonyl or naphthyloxycarbonyl; substituted or unsubstituted aralkoxycarbonyl wherein the aryl moiety is phenyl or naphthyl, such as benzyloxycarbonyl, phenethyloxycarbonyl, naphthylmethyloxycarbonyl and the like; linear or branched (C 1 -C 6 ) alkylamino; arylamino group such as HNC 6 H 5 ; —NCH 3 C 6 H 5 , —NHC 6 H 4 —CH 3 , —NHC 6 H 4 -halo and the like, amino group; amino(C 1 -C 6 )alkyl; hydroxy(C 1 -C 6 )alkyl; (C 1 -C 6 )alkoxy; alkoxyalkyl such as methoxymethyl, ethoxymethyl, methoxyethyl and the like; thio(C 1 -C 6 )alkyl; (C 1 -C 6 )alkylthio; acyl group such as acetyl, propionyl or benzoyl, the acyl group may be substituted; acylamino groups such as NHCOCH 3 , NHCOC 2 H 5 , NHCOC 3 H 7 , NHCOC 6 H 5 , aralkoxycarbonylamino group such as NHCOOCH 2 C 6 H 5 —NHCOOCH 2 CH 2 C 6 H 5 , —NCH 3 COOCH 2 C 6 H 5 ,—NC 2 H 5 COOCH 2 C 6 H 5 ,—NHCOOCH 2 C 6 H 4 CH 3 , —NHCOOCH 2 C 6 H 4 OCH 3 and the like, alkoxycarbonyl amino group such as NHCOOC 2 H 5 , NHCOOCH 3 and the like; aryloxycarbonylamino group such as NHCOOC 6 H 5 , —NCH 3 COOC 6 H 5 , —NC 2 H 5 COOC 6 H 5 , —NHCOOC 6 H 4 CH 3 , —NHCOOC 6 H 4 OCH 3 and the like; carboxylic acid or its derivatives such as amides, like CONH 2 , CONHMe, CONMe 2 , CONHEt, CONEt 2 , CONHPh and the like, the carboxylic acid derivatives may be substituted; acyloxy group such as MeCOO, EtCOO, PhCOO and the like, which may optionally be substituted; sulfonic acid or its derivatives such as SO 2 NH 2 , SO 2 NHMe, SO 2 NMe 2 , SO 2 NHCF 3 and the like, the sulfonic acid derivatives may be substituted.
The alkoxy, alkylamino, arylamino, amino, aminoalkyl, hydroxyalkyl alkoxyalkyl, thioalkyl, alkylthio, acylamino, aryloxycarbonylamino, aralkoxycarbonylamino, and alkoxycarbonylamino groups may also be substituted.
When the groups represented by R 1 , R 2 , R 3 , R 4 are substituted, the substituents may be selected from halogen, hydroxy, cyano, or nitro or optionally substituted groups selected from alkyl, cycloalkyl, alkoxy, cycloalkoxy, aryl, aralkyl, heterocyclyl, heteroaryl, heteroaralkyl, acyl, acyloxy, hydroxyalkyl, amino, acylamino, arylamino, aminoalkyl, aryloxy, alkoxycarbonyl, alkylamino such as NHCH 3 , N(CH 3 ) 2 , NCH 3 (C 2 H 5 ), NHC 2 H 5 and the like; alkoxyalkyl such as methoxymethyl, ethoxymethyl, methoxyethyl and the like; alkylthio, thioalkyl groups, carboxylic acid or its derivatives, or sulfonic acid or its derivatives.
These groups are as defined above for R 1 -R 4 .
It is preferred that R 1 -R 4 represent hydrogen; halogen atom such as fluorine, chlorine, bromine; alkyl group such as methyl, ethyl, isopropyl, n-propyl, n-butyl; and the like which may be halogenated; optionally halogenated groups selected from cycloalkyl group such as cyclopropyl; aryl group such as phenyl; aralkyl group such as benzyl; (C 1 -C 3 )alkoxy, aryloxy group such as benzyloxy; hydroxy group, acyl or acyloxy groups. Acyl and acyloxy groups are as defined above.
Suitable R 6 and R 9 are selected from hydrogen, substituted or unsubstituted (C 1 -C 12 )alkyl group, especially, linear or branched (C 1 -C 6 )alkyl group, such as methyl, ethyl, n-propyl, isopropyl, n-butyl, iso-butyl, t-butyl, n-pentyl, isopentyl, hexyl and the like; substituted or unsubstituted cycloalkyl group such as cyclopropyl, cyclobutyl, cyclopentyl, cyclohexyl and the like; aryl group such as phenyl or naphthyl, the aryl group may be substituted; aralkyl group such as benzyl or phenethyl, the aralkyl group may be substituted; heteroaryl group such as pyridyl, thienyl, furyl and the like, the heteroaryl group may be substituted; substituted or unsubstituted heterocyclyl such as aziridinyl, pyrrolidinyl, morpholinyl, piperidinyl and the like; substituted or unsubstituted heteroaralkyl such as pyridinemethyl, furanmethyl, oxazolemethyl, oxazolethyl and the like; substituted or unsubstituted alkoxyalkyl such as methoxymethyl, ethoxymethyl, ethoxyethyl, methoxyethyl and the like; substituted or unsubstituted alkylthio such as SCH 3 , SC 2 H 5 , SC 3 H 7 and the like; substituted or unsubstituted alkoxycarbonyl such as methoxycarbonyl or ethoxycarbonyl; aryloxycarbonyl group such as optionally substituted phenoxycarbonyl or naphthyloxycarbonyl; substituted or unsubstituted aralkoxycarbonyl group such as benzyloxycarbonyl, napthylmethoxycarbonyl; amino(C 1 -C 6 )alkyl; hydroxy(C 1 -C 6 )alkyl; thio(C 1 -C 6 )alkyl; and acyl group such as acetyl, propionyl or benzoyl. The acyl, aminoalkyl, hydroxyalkyl and thioalkyl groups may be substituted.
When the groups represented by R 6 , R 9 are substituted, the preferred substituents are halogen such as fluorine, chlorine; hydroxy, acyl, acyloxy, and amino groups.
The acyl and acyloxy groups are as defined above.
Suitable R 5 may be hydrogen, halogen, hydroxy or optionally substituted (C 1 -C 6 )alkyl group which may be linear or branched, aryl, heteroaryl, (C 1 -C 6 )alkoxy, aralkyl, aralkoxy, or acyl groups.
R 5 may be substituted by hydroxy, halogen, linear or branched (C 1 -C 6 ) alkyl group, acyl or acyloxy group.
These groups are as defined above.
n is an integer ranging from 1-4. It is preferred that n be 1 or 2.
It is preferred that the group represented by Ar be substituted or unsubstituted groups selected from divalent phenylene, naphthylene, pyridyl, quinolinyl, benzofuryl, dihydrobenzofuryl, benzopyranyl, indolyl, indolinyl, azaindolyl, azaindolinyl, pyrazolyl, benzothiazolyl, benzoxazolyl and the like. The substituents on the group represented by Ar may be selected from linear or branched (C 1 -C 6 )alkyl, (C 1 -C 3 )alkoxy, halogen, acyl, amino, acylamino, thio or carboxylic or sulfonic acids and their derivatives.
It is more preferred that Ar represents substituted or unsubstituted divalent phenylene, naphthylene, benzofuryl, indolyl, indolinyl, quinolinyl, azaindolyl, azaindolinyl, benzothiazolyl or benzoxazolyl.
It is still more preferred that Ar represents divalent phenylene or naphthylene, which may be optionally substituted by methyl, halomethyl, methoxy or halomethoxy groups.
Suitable R 7 includes hydrogen, hydroxy, lower alkyl group such as (C 1 -C 6 )alkyl such as methyl, ethyl or propyl; substituted or unsubstituted aralkyl group such as benzyl, phenethyl CH 2 C 6 H 4 -Halo, CH 2 C 6 H 4 -OCH 3 , CH 2 C 6 H 4 CH 3 , CH 2 CH 2 C 6 H 4 CH 3 and the like; halogen atom such as fluorine, chlorine, bromine or iodine; or R 7 together with R 8 represents a bond.
It is preferred that R 7 represents hydrogen or a bond together with R 8 .
Suitable R 8 represents hydrogen, hydroxy, lower alkyl group such as (C 1 -C 6 )alkyl such as methyl, ethyl or propyl; substituted or unsubstituted aralkyl group such as benzyl, phenethyl, CH 2 C 6 H 4 -Halo, CH 2 C 6 H 4 -OCH 3 , CH 2 C 6 H 4 CH 3 , CH 2 CH 2 C 6 H 4 CH 3 and the like; halogen atom such as fluorine, chlorine, bromine or iodine; or together with R 7 forms a bond.
When R 7 or R 8 is lower alkyl, the lower alkyl may be substituted by groups such as halogen, methyl or oxo group.
Suitable B group includes a hetero atom selected from O or S.
Suitable ring structure comprising B include 2,4-dioxooxazolidinyl, 2,4-dioxothiazolidinyl groups.
It is more preferred that the ring structure comprising B is a 2,4-dioxothiazolidinyl group.
The groups represented by R 1 -R 9 and any substituents on these groups may be defined as disclosed anywhere in the specification.
Pharmaceutically acceptable salts forming part of this invention include salts of the azolidinedione moiety such as alkali metal salts like Li, Na, and K salts, alkaline earth metal salts like Ca and Mg salts, salts of organic bases such as lysine, arginine, guanidine, diethanolamine, choline and the like, ammonium or substituted ammonium salts, salts of carboxy group wherever appropriate, such as aluminum, alkali metal salts; alkaline earth metal salts, ammonium or substituted ammonium salts. Salts may include acid addition salts which are, sulphates, nitrates, phosphates, perchlorates, borates, hydrohalides, acetates, tartrates, maleates, citrates, succinates, palmoates, methanesulfonates, benzoates, salicylates, hydroxynaphthoates, benzenesulfonates, ascorbates, glycerophosphates, ketoglutarates and the like. Pharmaceutically acceptable solvates may be hydrates or comprising other solvents of crystallization such as alcohols.
Particularly useful compounds according to the present invention include:
5-[4-[[4-Oxo-3,4-dihydro-(2H)-1,3-benzoxazine-2-yl]methoxy]phenyl methyl]thiazolidin-2,4-dione;
5-[4-[[3-Methyl-4-oxo-3,4-dihydro-(2H)-1,3-benzoxazine-2-yl]methoxy]phenyl methyl]thiazolidin-2,4-dione;
5-[4-[[3-Ethyl-4-oxo-3,4-dihydro-(2H)-1,3-benzoxazine-2-yl]methoxy]phenyl methyl]thiazolidin-2,4-dione;
5-4-[[2, 5-[4-[[4-Oxo-3,4-dihydro-(2H)-1,3-benzoxazine-2-yl]methoxy]phenyl methyl]thiazolidin-2,4-dione;
5-[4-[[2,3-Dimethyl-4-oxo-3,4-dihydro-(2H)-1,3-benzoxazine-2-yl]methoxy]phenyl methyl]thiazolidin-2,4-dione;
5-[4-[[4-Oxo-3,4-dihydro-(2H)-1,3-benzoxazine-2-yl]methoxy]phenyl methyl]thiazolidin-2,4-dione, sodium salt;
5-[4-[[3-Methyl-4-oxo-3,4-dihydro-(2H)-1,3-benzoxazine-2-yl]methoxy]phenyl methyl]thiazolidin-2,4-dione, sodium salt;
5-[4-[[1,3-Dimethyl-4-oxo-1,2,3,4-tetrahydro-2-quinazolinyl]methoxy]phenyl methylene]thiazolidin-2,4-dione;
5-[4-[[3-Methyl-4-oxo-1,2,3,4-tetrahydro-2-quinazolinyl]methoxy]phenyl methylene]thiazolidin-2,4,dione;
5-[4-[[3-Dimethyl-4-oxo-1,2,3,4-tetrahydro-2-quinazolinyl]methoxy]phenyl methyl]thiazolidin-2,4-dione;
5-[4-[[3-Methyl-4-oxo-1,2,3,4-tetrahydro-2-quinazolinyl]methoxy]phenyl methyl]thiazolidin-2,4-dione;
5-[4-[[3-Ethyl-1-methyl-4-oxo-1,2,3,4-tetrahydro-2-quinazolinyl]methoxy]phenyl methyl]thiazolidin-2,4-dione;
5-[4-[[1-Methyl-4-oxo-1,2,3,4-tetrahydro-2-quinazolinyl]methoxy]phenyl methyl]thiazolidin-2,4-dione;
5-[4-[[1,3-Dimethyl-4-oxo-1,2,3,4-tetrahydro-2-quinazolinyl]methoxy]phenyl methyl]thiazolidin-2,4-dione, sodium salt;
5-[4-[[4-Oxo-1,2,3,4-tetrahydro-2-quinazolinyl]methoxy]phenyl methyl]thiazolidin-2,4-dione;
5-[4-[[1,3-Diethyl-4-oxo-1,2,3,4-tetrahydro-2-quinazolinyl]methoxy]phenyl methyl]thiazolidin-2,4-dione;
5-[4-[[1-Ethyl-3-methyl-4-oxo-1,2,3,4-tetrahydro-2-quinazolinyl]methoxy]phenyl methyl]thiazolidin-2,4-dione; and
5-[4-[[1-Ethyl-4-oxo-1,2,3,4-tetrahydro-2-quinazolinyl]methoxy]phenyl methyl]thiazolidin-2,4-dione.
The invention also includes an intermediate of formula (III)
wherein X represents O or S; the groups R 1 , R 2 , R 3 , R 4 may be same or different and represent hydrogen, halogen, hydroxy, cyano, nitro; optionally substituted groups selected from alkyl, cycloalkyl, alkoxy, cycloalkyloxy, aryl, aralkyl, heteroaryl, heteroaralkyl, heterocyclyl, aryloxy, alkoxycarbonyl, aryloxycarbonyl, aralkoxycarbonyl, alkylamino, arylamino, amino, aminoalkyl, hydroxyalkyl, alkoxyalkyl, thioalkyl, alkylthio, acyl, acylamino, aryloxycarbonylamino, aralkoxycarbonylamino, alkoxycarbonylamino, carboxylic acid or its derivatives, acyloxy, sulfonic acid or its derivatives; W represents O, S or a group NR 9 ; R 6 and R 9 may be same or different and represent hydrogen or optionally substituted alkyl, cycloalkyl, aryl, aralkyl, heterocyclyl, heteroaryl, heteroaralkyl, acyl, hydroxyalkyl, aminoalkyl, alkoxycarbonyl, aryloxycarbonyl, aralkoxycarbonyl, alkoxyalkyl, alkylthio, or thioalkyl groups; R 5 represents hydrogen, hydroxy or halogen or optionally substituted alkyl, aryl, heteroaryl, acyl, alkoxy, aralkyl, or aralkoxy; n is an; integer ranging from 1-4; Ar represents an optionally substituted divalent aromatic or heterocyclic group; G represents CHO, NO 2 , —NH 2 or —CH 2 CH(J)—COOR, where J represents a halogen atom and R represents H or lower alkyl group.
According to a feature of the present invention, there is provided a process for the preparation of novel intermediate of the general formula (III)
where R 1 , R 2 , R 3 , R 4 , R 5 , R 6 , X, W, n, and Ar are as defined earlier, G represents —CHO or —NO 2 group which comprises, reacting a compound of the general formula (IV)
wherein, R 1 , R 2 , R 3 , R 4 , R 5 , R 6 , X, W, and n are as defined earlier, with a compound of general formula (V)
L 1 —Ar—G (V)
where L 1 is a halogen atom such as fluorine or chlorine, G is a CHO or a NO 2 group and Ar is as defined earlier.
The reaction of a compound of formula (IV) with a compound of formula (V) to produce a compound of formula (III) may be carried out in the presence of solvents such as THF, DMF, DMSO, DME and the like or mixtures thereof. The inert atmosphere may be maintained by using inert gases such as N 2 , Ar or He. The reaction may be effected in the presence of a base such as K 2 CO 3 , Na 2 CO 3 , NaH and the like. Mixture of bases may be used. The reaction temperature may range from 20° C. to 150° C., preferably at a temperature in the range of 30° C. to 100° C. The duration of the reaction may range from 1 to 24 hours, preferably from 2 to 6 hours.
In another embodiment of the present invention, the novel intermediate of general formula (III), where G is a CHO or NO 2 group, can also be prepared by the reaction of compound of general formula (VI)
where R 1 , R 2 , R 3 , R 4 , R 5 , R 6 , X, W, and n are as defined earlier and L 2 may be a halogen atom such as Cl, Br, I or a leaving group such as methanesulfonate, trifluoromethanesulfonate, p-toluenesulfonate with a compound of general formula (VII)
HO—Ar—G (VII)
where G is a CHO or NO 2 group and Ar is as defined earlier.
The reaction of a compound of formula (VI) with a compound of formula (VII) to produce a compound of the formula (III) may be carried out in the presence of solvents such as THF, DMF, DMSO, DME and the like or mixtures thereof. The reaction may be carried out in an inert atmosphere which may be maintained by using inert gases such as N 2 , Ar, or He. The reaction may be effected in the presence of a base such as K 2 CO 3 , Na 2 CO 3 or NaH or mixtures thereof. The reaction temperature may range from 20° C.-120° C., preferably at a temperature in the range of 30° C.-100° C. The duration of the reaction may range from 1-12 hours, preferably from 2 to 6 hours.
Alternatively, a compound of general formula (III) can also be prepared by the reaction of compound of general formula (IV) defined earlier with a compound of general formula (VII) defined earlier.
The reaction of compound of general formula (IV) with a compound of general formula (VII) may be carried out using suitable coupling agents such as dicyclohexyl urea, triarylphosphine/dialkylazadicarboxylate such as PPh 3 /DEAD and the like. The reaction may be carried out in the presence of solvents such as THF, DME, CH 2 Cl 2 , CHCl 3 , toluene, acetonitrile, carbontetrachloride and the like. The inert atmosphere may be maintained by using inert gases such as N 2 , Ar, and He. The reaction may be effected in the presence of DMAP, HOBT and they may be used in the range of 0.05 to 2 equivalents, preferably 0.25 to 1 equivalents. The reaction temperature may be in the range of 0° C. to 100° C., preferably at a temperature in the range of 20° C. to 80° C. The duration of the reaction may range from 0.5 to 24 hours, preferably from 6 to 12 hours.
The present invention provides a process for the preparation of novel azolidinedione derivatives of general formula (I), their tautomeric forms, their stereoisomers, their polymorphs, their pharmaceutically acceptable salts and their pharmaceutically acceptable solvates wherein R 1 , R 2 , R 3 , R 4 , R 5 , R 6 , X, W, n, Ar and B are as defined earlier and R 7 together with R 8 represent a bond which comprises:
reacting the novel intermediate of the general formula (III) obtained above where G represents CHO group with 2,4-thiazolidinedione or 2,4-oxazolidinedione and removing the water formed during the reaction by conventional methods to yield a compound of general formula (VIII)
where R 1 , R 2 , R 3 , R 4 , R 5 , R 6 , X, W, n, and Ar are as defined earlier and B represents sulfur or oxygen. The compound of general formula (VIII) represents a compound of general formula (I), wherein R 7 and R 8 together represent a bond and all other symbols are as defined earlier.
The reaction of compound of the general formula (III) where G is a CHO group with 2,4-thiazolidinedione or 2,4-oxazolidinedione, to yield compound of general formula (VIII), may be carried out neat in the presence of sodium acetate or in the presence of a solvent such as benzene, toluene, methoxyethanol or mixtures thereof. The reaction temperature may range from 80° C. to 140° C. depending upon the solvents employed and in the range from 80° C. to 180° C. when the reaction is carried out neat in the presence of sodium acetate. Suitable catalyst such as piperidinium acetate or benzoate, sodium acetate or mixtures of catalysts may also be employed. Sodium acetate can be used in the presence of solvent, but it is preferred that sodium acetate is used neat. The water produced in the reaction may be removed, for example, by using Dean Stark water separator or by using water absorbing agents like molecular seives. Oxazolidine-2-oxo-4-thione may be used instead of 2,4-oxazolidinedione, wherein the thio group may be converted to oxo group by oxidation using agents such as hydrogen peroxide or peroxyacids like mCPBA.
The compound of the general formula (VIII) obtained above is converted into its pharmaceutically acceptable salts, or its pharmaceutically acceptable solvates by conventional methods.
The compound of the general formula (VIII) obtained in the manner described above is reduced by known methods to obtain the compound of general formula (IX).
wherein R 1 , R 2 , R 3 , R 4 , R 5 , R 6 , X, W, n, Ar and B are as defined earlier. The compound of general formula (IX) represents a compound of general formula (I), wherein R 7 and R 8 represent hydrogen atoms and other symbols are as defined earlier.
The reduction of compound of the formula (VIII) to yield a compound of the general formula (IX) may be carried out in the presence of gaseous hydrogen and a catalyst such as Pd/C, Rh/C, Pt/C, Raney nickel, and the like. Mixtures of catalysts may be used. The reaction may also be conducted in the presence of solvents such as dioxane, acetic acid, ethyl acetate and the like or mixtures thereof. A pressure between atmospheric pressure and 80 psi may be employed. The catalyst may be 5-10% Pd/C and the amount of catalyst used may range from 50-300% w/w. The reaction may also be carried out by employing metal solvent reduction such as magnesium in methanol or sodium amalgam in methanol. The reaction may also be carried out with alkali metal borohydrides such as LiBH 4 , NaBH 4 , KBH 4 and the like in the presence of cobalt salt such as CoCl 2 and ligands, preferably bidentated ligands such as 2, 2′-bipyridyl, 1, 10-phenanthroline, bisoximes and the like.
The compound of the general formula (IX) obtained above is converted into its pharmaceutically acceptable salts, or its pharmaceutically acceptable solvates by conventional methods.
In yet another embodiment of the present invention, the compound of the general formula (I) can also be prepared by reacting a compound of the general formula (VI) defined above with a compound of general formula (X)
where R 7 , R 8 , B and Ar are as defined earlier and R 10 is hydrogen or a nitrogen protecting group which is removed after the reaction.
The reaction of compound of formula (VI) with compound of formula (X) to produce a compound of the formula (I) may be carried out in the presence of solvents such as THF, DMF, DMSO, DME and the like or mixtures thereof. The reaction may be carried out in an inert atmosphere which may be maintained by using inert gases such as N 2 , Ar or He. The reaction may be effected in the presence of a base such as K 2 CO 3 , Na 2 CO 3 or NaH or mixtures thereof. The reaction temperature may range from 20° C.-150° C., preferably at a temperature in the range of 30° C.-80° C. The duration of the reaction may range from 1-12 hours, preferably from 2 to 6 hours.
Alternatively, compound of the general formula (I) can also be prepared by reacting a compound of general formula (IV) defined earlier with a compound of general formula (X) defined above.
The reaction of compound of general formula (IV) with a compound of general formula (X) may be carried out using suitable coupling agents such as dicyclohexyl urea, triarylphosphine/dialkylazadicarboxylate such as PPh 3 /DEAD and the like. The reaction may be carried out in the presence of solvents such as THF, DME, CH 2 Cl 2 , CHCl 3 , toluene, acetonitrile, carbontetrachloride and the like. The inert atmosphere may be maintained by using inert gases such, as N 2 , Ar, He. The reaction may be effected in the presence of DMAP, HOBT and they may be used in the range of 0.05 to 2 equivalents, preferably 0.25 to 1 equivalents. The reaction temperature may be in the range of 0° C. to 100° C., preferably at a temperature in the range of 20° C. to 80° C. The duration of the reaction may range from 0.5 to 24 hours, preferably from 6 to 12 hours.
In another embodiment of the present invention, the compound of general formula (I), where R 1 , R 2 , R 3 , R 4 , R 5 , R 6 , X, W, n, and Ar are as defined earlier and R 7 and R 8 represent hydrogen atoms, B represents S can be prepared by the reaction of compound of general formula (XI)
where R 1 , R 2 , R 3 , R 4 , R 5 , R 6 , X, W, n, and Ar are as defined earlier, J is a halogen atom like chlorine, bromine or iodine and R is a lower alkyl group with thiourea followed by treatment with an acid.
The reaction of compound of general formula (XI) with thiourea is normally carried out in the presence of alcoholic solvent such as methanol, ethanol, propanol, isobutanol, 2-methoxybutanol and the like or DMSO or sulfolane. The reaction may be conducted at a temperature in the range between 20° C. and the reflux temperature of the solvent used. Bases such as NaOAc, KOAc, NaOMe, NaOEt and the like may be used. The reaction is normally followed by treatment with a mineral acid such as hydrochloric acid at 20° C.-100° C.
The compound of general formula (XI) where all the symbols are as defined earlier can be prepared by the diazotization of the amino compound of the general formula (XII)
where all symbols are as defined earlier, using alkali metal nitrites followed by treatment with acrylic acid esters in the presence of hydrohalo acids and catalytic amount of copper oxide or copper halide.
The compounds of general formula (XII) can in turn be prepared by the conventional reduction of the novel intermediate (III) where G is NO 2 group and other symbols are as defined earlier.
In yet another embodiment of the present invention, the compound of general formula (I), can also be prepared by reacting the compound of general formula (XIII)
where R 1 , R 2 , R 3 , R 4 , R 6 , X, and W are as defined earlier, with a compound of general formula (XIV)
where Ar, R 5 , R 7 , R 8 , B and n are as defined earlier, and R 11 may be a linear or branched (C 1 -C 5 ) alkyl group such as methyl, ethyl, propyl, isopropyl, t-butyl and the like.
The reaction of compound of general formula (XIV) with compound of general formula (XIII) to produce a compound of general formula (I) may be carried out in neat or in the presence of solvents such as THF, CHCl 3 , benzene, toluene, hexane, dioxane and the like or mixture thereof The reaction may be carried out at a temperature in the range of 0° C. to 250° C. preferably at a temperature in the range of 10° C. to 150° C. The reaction may be carried out in the presence of an acid or a base. The selection of acid or base is not critical. The examples of such acids include H 2 SO 4 , HCl, pTsOH, PPE (polyphosphoric ethyl ester) and the like. Examples of bases include pyrrolidine, piperidine and the like. The reaction may be carried out in an inert atmosphere which may be maintained by using inert gases such as N 2 , Ar or He. The duration of the reaction may range from 0.25 to 24 h preferably, from 1 to 12 h.
In another embodiment of the present invention, there is provided a process for the preparation of novel intermediate of general formula (XIV) as defined above, where all the symbols are as defined earlier which comprises, reacting a compound of the general formula (XV)
(R 11 O) 2 CR 5 —(CH 2 ) n —L 1 (XV)
where all symbols are defined earlier with a compound of general formula (X) where R 7 , R 8 , B and Ar are as defined earlier and R 10 is hydrogen or a nitrogen protecting group which is removed after the reaction.
The reaction of compound of formula (XV) with compound of formula (X) to produce a compound of the formula (XIV) may be carried out in the presence of solvents such as THF, DMF, DMSO, DME and the like or mixtures thereof. The reaction may be carried out in an inert atmosphere which may be maintained by using inert gases such as N 2 , Ar or He. The reaction may be effected in the presence of a base such as K 2 CO 3 , Na 2 CO 3 or NaH or mixtures thereof. The reaction temperature may range from 20° C.-120° C., preferably at a temperature in the range of 30° C.-80° C. The duration of the reaction may range from 1-12 hours, preferably from 2 to 6 hours.
In still another embodiment of the present invention, the compound of general formula (XIV) where R 7 and R 8 represents hydrogen atom and all other symbols are as defined earlier can be prepared from the compound of general formula (XVI)
where all the symbols are as defined above, by reducing under known methods.
The reduction of compound of the formula (XVI) to yield a compound of the general formula (XIV) may be carried out in the presence of gaseous hydrogen and a catalyst such as Pd/C, Rh/C, Pt/C, and the like. Mixtures of catalysts may be used. The reaction may also be conducted in the presence of solvents such as dioxane, acetic acid, ethyl acetate and the like. A pressure between atmospheric pressure and 80 psi may be employed. The catalyst may be 5-10% Pd/C and the amount of catalyst used may range from 50-200% w/w. The reaction may also be carried out by employing metal solvent reduction such as magnesium in methanol or sodium amalgam in methanol.
The reaction may also be carried out with Raney Nickel in the presence of hydrogen gas or alkali metal borohydrides such as LiBH 4 , NaBH 4 , KBH 4 and the like in the presence of cobalt salt such as CoCl 2 and ligands, preferably bidentated ligands such as 2, 2′-bipyridyl, 1, 10-phenanthroline, bisoximes and the like.
The present invention also provides a process for the preparation of novel intermediate of general formula (XVI) where all the symbols are as defined earlier, which comprises reacting the intermediate (XVII)
(R 11 O) 2 CR 5 —(CH 2 ) n —O—Ar—G (XVII)
where G represents CHO group, and all the symbols are as defined earlier, with 2,4-thiazolidinedione or 2,4-oxazolidinedione and removing the water formed during the reaction by conventional methods.
The reaction between the compound of the general formula (XVII) where G is a CHO group with 2,4-thiazolidinedione or 2,4-oxazolidinedione, to yield compound of general formula (XVI) wherein B represents a sulfur or an oxygen atom respectively, may be carried out neat in the presence of sodium acetate or in the presence of a solvent such as benzene, toluene, methoxyethanol or mixtures thereof. The reaction temperature may range from 80° C. to 140° C. depending upon the solvents employed and in the range from 80° C. to 180° C. when the reaction is carried out neat in the presence of sodium acetate. Suitable catalyst such as piperidinium acetate or benzoate, sodium acetate or mixtures of catalysts may also be employed. Sodium acetate can be used in the presence of solvent, but it is preferred that sodium acetate is used neat. The water produced in the reaction may be removed, for example, by using Dean Stark water separator or by using water absorbing agents like molecular seives. Oxazolidine-2-oxo-4-thione may be used instead of 2,4-oxazolidinedione, wherein the thio group may be converted to oxo group by oxidation using agents such as hydrogen peroxide or peroxyacids like mCPBA.
The compound of formula (XVII) is in turn prepared by reacting a compound of formula (XV)
(R 11 O) 2 CR 5 —(CH 2 ) n —L 1 (XV)
where all symbols are as defined earlier and L 1 is a leaving group, with a compound of formula (VII)
HO—Ar—G (VII)
where G is a CHO group and Ar is as defined earlier.
The reaction of a compound of formula (XV) with a compound of formula (VII) to produce a compound of the formula (XVII) may be carried out in the presence of solvents such as THF, DMF, DMSO, DME and the like or mixtures thereof. The reaction may be carried out in an inert atmosphere which may be maintained by using inert gases such as N 2 , Ar, or He. The reaction may be effected in the presence of a base such as K 2 CO 3 , Na 2 CO 3 or NaH or mixtures thereof. The reaction temperature may range from 20° C.-120° C., preferably at a temperature in the range of 30° C.-100° C. The duration of the reaction may range from 1-12 hours, preferably from 2 to 6 hours.
In another embodiment of the present invention the compound of formula (I) where R 7 and R 8 together represent a bond and all other symbols are as defined earlier may be prepared by reacting a compound of general formula (XVI) with a compound of general formula (XIII) using similar conditions as that followed for the reaction of compound of formula (XIII) with a compound of formula (XIV) as described earlier.
In yet another embodiment of the present invention, the compound of general formula (I) where R 5 is hydrogen atom, W represents NH and all other symbols are as defined earlier can also be prepared by reducing the compound of general formula (XVIII) (disclosed in copending U.S. application Ser. Nos. 08/777,627 and 08/884,816).
where R 7 and R 8 represents hydrogen atom or together form a bond and all other symbols are as defined earlier.
The reduction of compound of the formula (XVIII) to yield a compound of the general formula (I) may be carried out in the presence of gaseous hydrogen and a catalyst such as Pd/C, Rh/C, Pt/C and the like. Mixture of catalysts may be used. The reaction may also be carried out in the presence of solvents such as dioxane, acetic acid, ethyl acetate and the like. A pressure between atmospheric pressure and 80 psi may be employed. The catalyst may be 5-10% Pd/C and the amount of catalyst used may range from 30-50 w/w. The duration of the reaction may range from 12 to 24 h and the temperature of the reaction may range from 25° C. to 80° C.
The compound of general formula (VI) defined earlier may be prepared from compound of general formula (IV) defined earlier using conventional organic transformations that one skilled in the art would use.
The compound of general formula (VI) and of general formula (IV) defined earlier may be prepared by the reaction of compound of general formula (XIII) defined earlier with a compound of formula (XIX)
(R 11 O) 2 CR 5 —(CH 2 ) n —Z (XIX)
where R 11 , R 5 and n are as defined earlier and Z represents hydroxy or a leaving group L 1 such as chloride, bromide, p-toluenesulfonate, methanesulfonate, trifluoromethanesulfonate and the like.
The reaction of compound of (XIII) with a compound of formula (XIX) to yield a compound of formula (VI) or (IV) may be carried out using similar conditions described for the reaction of formula (XIII) with the compound of general formula (XIV).
The pharmaceutically acceptable salts are prepared by reacting the compound of formula (I) with 1 to 4 equivalents of a base such as sodium hydroxide, sodium methoxide, sodium hydride, potassium t-butoxide, calcium hydroxide, magnesium hydroxide and the like, in solvents like ether, THF, methanol, t-butanol, dioxane, isopropanol, ethanol etc. Mixture of solvents may be used. Organic bases like lysine, arginine, diethanolamine, choline, guanidine and their derivatives etc. may also be used. Alternatively, acid addition salts are prepared by treatment with acids such as hydrochloric acid, hydrobromic acid, nitric acid, sulfuric acid, phosphoric acid, p-toluenesulphonic acid, methanesulfonic acid, acetic acid, citric acid, maleic acid, salicylic acid, hydroxynaphthoic acid, ascorbic acid, palmitic acid, succinic acid, benzoic acid, benzenesulfonic acid, tartaric acid and the like in solvents like ethyl acetate, ether, alcohols, acetone, THF, dioxane etc. Mixture of solvents may also be used.
The term neat as used in this application means the reaction is carried out without the use of a solvent.
The stereoisomers of the compounds forming part of this invention may be prepared by using reactants in their single enantiomeric form in the process wherever possible or by conducting the reaction in the presence of reagents or catalysts in their single enantiomeric form or by resolving the mixture of stereoisomers by conventional methods. Some of the preferred methods include use of microbial resolution, resolving the diastereomeric salts formed with chiral acids such as mandelic acid, camphorsulfonic acid, tartaric acid, lactic acid and the like or chiral bases such as brucine, cinchona alkaloids and their derivatives and the like.
Various polymorphs of compound of general formula (I) forming part of this invention may be prepared by crystallization of compound of formula (I) under different conditions. For example, using different solvents commonly used or their mixtures for recrystallization; crystallizations at different temperatures; various modes of cooling, ranging from very fast to very slow cooling during crystallizations. Polymorphs may also be obtained by heating or melting the compound followed by gradual or fast cooling. The presence of polymorphs may be determined by solid probe nmr spectroscopy, ir spectroscopy, differential scanning calorimetry, powder X-ray diffraction or such other techniques.
The present invention also provides a pharmaceutical composition, containing the compounds of the general formula (I), as defined above, their tautomeric forms, their stereoisomers, their polymorphs, their pharmaceutically acceptable salts, their pharmaceutically acceptable solvates or mixtures thereof in combination with the usual pharmaceutically employed carriers, diluents and the like, useful for the treatment and/or prophylaxis of hyperlipidemia, hypercholesterolemia, hyperglycemia, osteoporosis, obesity, glucose intolerance, insulin resistance and also diseases or conditions in which insulin resistance is the underlying pathophysiological mechanism such as type II diabetes, impaired glucose tolerance, dyslipidaemia, hypertension, coronary heart disease and other cardiovascular disorders including atherosclerosis; insulin resistance associated with obesity and psoriasis, for treating diabetic complications and other diseases such as polycystic ovarian syndrome (PCOS), certain renal diseases including diabetic nephropathy, glomerulonephritis, glomerular sclerosis, nephrotic syndrome, hypertensive nephrosclerosis, end-stage renal diseases and microalbuminuria as well as certain eating disorders, as aldose reductase inhibitors and for improving cognitive functions in dementia.
The pharmaceutical composition may be in the forms normally employed, such as tablets, capsules, powders, syrups, solutions, suspensions and the like, may contain flavourants, sweeteners etc. in suitable solid or liquid carriers or diluents, or in suitable sterile media to form injectable solutions or suspensions. Such compositions typically contain from 1 to 20%, preferably 1 to 10% by weight of active compound, the remainder of the composition being pharmaceutically acceptable carriers, diluents, excipients, or solvents.
A typical tablet production method is exemplified below:
Tablet Production Example:
a)
1) Active ingredient
10 g
2) Lactose
110 g
3) Corn starch
35 g
4) Carboxymethyl cellulose
44 g
5) Magnesium stearate
1 g
200 g
for 1000 tablets
The ingredients 1 to 3 are uniformly blended with water and granulated after drying under reduced pressure. The ingredient 4 and 5 are mixed well with the granules and compressed by tabletting machine to prepare 1000 tablets each containing 10 mg of active ingredient.
b)
1) Active ingredient
10 g
2) Calcium phosphate
90 g
3) Lactose
50 g
4) Corn starch
45 g
5) Polyvinyl pyrrolidone
3.5 g
6) Magnesium stearate
1.5 g
200 g
for 1000 tablets
The ingredients 1 to 4 are uniformly moistened with an aqueous solution of ingredient 5 and granulated after drying under reduced pressure. Ingredient 6 is added and granules are compressed by a tabletting machine to prepare 1000 tablets containing 10 mg of active ingredient 1.
The compound of the formula (I) as defined above are clinically administered to mammals, including man, via either oral or parenteral routes. Administration by the oral route is preferred, being more convenient and avoiding the possible pain and irritation of injection. However, in circumstances where the patient cannot swallow the medication, or absorption following oral administration is impaired, as by disease or other abnormality, it is essential that the drug be administered parenterally. By either route, the dosage is in the range of about 0.10 mg to about 200 mg/kg body weight of the subject per day or preferably about 0.10 mg to about 30 mg/kg body weight per day administered singly or as a divided dose. However, the optimum dosage for the individual subject being treated will be determined by the person responsible for treatment, generally smaller doses being administered initially and thereafter increments made to determine the most suitable dosage.
Suitable pharmaceutically acceptable carriers include solid fillers or diluents and sterile aqueous or organic solutions. The active compound will be present in such pharmaceutical compositions in the amounts sufficient to provide the desired dosage in the range as described above. Thus, for oral administration, the compounds can be combined with a suitable solid or liquid carrier or diluent to form capsules, tablets, powders, syrups, solutions, suspensions and the like. The pharmaceutical compositions, may, if desired, contain additional components such as flavourants, sweeteners, excipients and the like. For parenteral administration, the compounds can be combined with sterile aqueous or organic media to form injectable solutions or suspensions. For example, solutions in sesame or peanut oil, aqueous propylene glycol and the like can be used, as well as aqueous solutions of water-soluble pharmaceutically-acceptable acid addition salts or salts with base of the compounds. The injectable solutions prepared in this manner can then be administered intravenously, intraperitoneally, subcutaneously, or intramuscularly, with intramuscular administration being preferred in humans.
The invention is explained in detail in the examples given below which are provided by way of illustration only and therefore should not be construed to limit the scope of the invention.
PREPARATION 1
4-[[2-Methyl-4-oxo-3,4-dihydro-(2H)-1,3-benzoxazine-2-yl]methoxy]nitrobenzene
Step A: Preparation of 4-[2-oxo-propoxy]nitrobenzene—To stirred suspension of K 2 CO 3 (50.0 g, 0.36 mol) in dry DMF (500 mL) was added 4-nitrophenol (25.0 g, 0.18 mol) and stirred for 30 min at 25° C. Chloroacetone (21.5 mL, 0.27 mol) was added to the reaction mixture and stirred for 24 h at 25-30° C. The reaction mixture was filtered through a buchner funnel. The filtrate was poured into water (500 mL) and extracted with ethyl acetate (3×300 mL). The combined organic layers were washed with brine, dried over anhydrous Na 2 SO 4 and concentrated. The crude compound was purified by column chromatography using EtOAc:Pet. ether (1:2) as eluent to yield the title compound (11.0 g, 31%) as a colourless liquid.
1 H NMR (CDCl 3 ): δ 8.22 (d, J=9.17 Hz, 2H), 6.95 (d, J=9.17 Hz, 2H), 4.67 (s, 2H), 2.30 (s, 3H).
Step B:
To a stirred mixture of salicylamide (6.85 g, 50 mmol) and 4-[2-oxo-propoxy]nitrobenzene (9.75 g, 50 mmol) in benzene (500 mL) was added piperidine (0.52 mL, 5 mmol). The reaction mixture was immersed in a pre-heated oil bath (˜100° C.) and refluxed for 10 h with continuous removal of water using Dean-Stark water separator. The reaction mixture was cooled to room temperature End the precipitated brown coloured solid was filtered, washed with benzene and dried to afford the title compound (13.5 g, 86%).
1 H NMR (CDCl 3 ): δ 8.76 (bs, 1H, D 2 O exchangeable), 8.14 (d, J=9.20 Hz, 2H), 7.82 (d, J=7.50 Hz, 1H), 7.42 (t, J=7.50 Hz, 1H), 7.06 (t, J=7.50 Hz, 1H), 6.99 (d, J=9.20 Hz, 2H), 6.88 (d, J=7.50 Hz, 1H), 4.30 (d, J=10.33 Hz, 1H), 4.14 (d, J=10.33 Hz, 1H), 1.72 (s, 3H).
PREPARATION 2
4-[[2,3-Dimethyl-4-oxo-3,4-dihydro-(2H)-1,3-benzoxazine-2-yl]methoxy]nitrobenzene
To a stirred mixture of 4-[[2-methyl-4-oxo-3,4-dihydro-(2H)-1,3-benzoxazine-2-yl]methoxy]nitrobenzene (5.0 g, 15.9 mmol) obtained in preparation 1 and K 2 CO 3 (6.6 g, 47.7 mmol) in acetone (60 mL) was added CH3I (9.9 mL, 159 mmol) and refluxed for 12 h. The reaction mixture was cooled to room temperature, filtered through buchner funnel to remove all the inorganic salts and acetone was removed at 40° C. The residue was poured into water (50 mL) and extracted with ethyl acetate (3×50 mL). The organic extracts were washed with brine, dried over anhydrous Na 2 SO 4 and concentrated to afford the title compound (5.1 g, 98%).
1 H NMR (CDCl 3 ): δ 8.19 (d, J=9.10 Hz, 2H), 7.94 (d, J=7.50 Hz, 1H), 7.42 (t, J=7.50 Hz, 1H), 7.11 (t, J=7.50 Hz, 1H), 6.95 (d, J=9.10 Hz, 2H), 6.88 (d, J=7.50 Hz, 1H), 4.30−4.10 (m, 2H), 3.22 (s, 3H), 1.88 (s, 3H).
PREPARATION 3
4-[[2,3-Dimethyl-4-oxo-3,4-dihydro-(2H)-1,3-benzoxazine-2-yl]methoxy]aniline
A solution of 4-[[2,3-dimethyl-4-oxo-3,4-dihydro-(2H)-1,3-benzoxazine-2-yl]methoxy]nitrobenzene (5.0 g, 15.2 mmol) obtained in preparation 2, in 1,4-dioxane (100 mL) was reduced with hydrogen in the presence of 10% palladium charcoal (500 mg) at 40 psi for 16 h. The reaction mixture was filtered through a bed of celite and washed with dioxane and evaporated to dryness under reduced pressure to yield the title compound (4.2 g, 93%), mp: 162-164° C.
1 H NMR (CDCl 3 ): δ 7.92 (d, J=7.35 Hz, 1H), 7.40 (t, J=7.35 Hz, 1H), 7.05 (t, J=7.35 Hz, 1H), 6.87 (d, J=7.35 Hz, 1H), 6.68−6.52 (m, 4H), 4.12−3.98 (m, 2H), 3.18 (s, 3H), 1.8 (s, 3H).
PREPARATION 4
Ethyl 2-bromo-3-[4-[[2,3-dimethyl-4-oxo-3,4-dihydro-(2H)-1,3-benzoxazine-2-yl]methoxy]phenyl]propionate
To a stirred solution of 4-[[2,3-dimethyl-4-oxo-3,4-dihydro-(2H)-1,3-benzoxazine-2-yl]methoxy]aniline (2.5 g, 8.4 mmol) obtained from preparation 3, in acetone (20 mL) was added aq HBr (6 mL, 33.6 mmol, 47%) and stirred for 20 min at 0-10° C. A solution of NaNO 2 (638 mg, 9.24 mmol) in water (1.5 mL) was added slowly dropwise at 0-10° C. and stirred further for 30 min at 0-15° C. To the reaction mixture, ethyl acrylate (5.5 mL, 50.4 mmol) was added and allowed to warm to 30° C. Catalytic amount of cuprous oxide (200 mg) was added in one portion and the reaction mixture was stirred further for 1 h at 30° C. Acetone was removed under reduced pressure. The resultant residue was extracted with ethyl acetate (3×25 mL). The combined organic layers were washed with ethyl acetate (3×25 mL), dilute NH 3 solution, water, followed by brine, dried over anhydrous Na 2 SO 4 . The solvent was evaporated under reduced pressure and the residue was purified by flash chromatography using EtOAc:pet. ether (4:6) as an eluent to yield the title compound (1.5 g, 39%).
1 H NMR (CDCl 3 ): δ 7.95 (d, J=7.50 Hz, 1H), 7.41 (t, J=7.50 Hz, 1H), 7.09 (d, J=8.30 Hz, 2H), 7.05 (d, J=7.50 Hz, 1H), 6.85 (d, J=7.50 Hz, 1H), 6.71 (d, J=8.30 Hz, 2H), 4.29 (dd, J=8.50, 7.05 Hz, 1H), 4.23−4.02 (m, 4H), 3.38 (dd, J=13.70, 7.05 Hz, 1H), 3.20 (s, 3H), 3.15 (dd, J=13.70, 8.50 Hz, 1H), 1.88 (s, 3H), 1.22 (t, J=7.30 Hz, 3H).
PREPARATION 5
4-[(2,2-diethoxy]ethoxy]benzaldehyde
To a stirred suspension of sodium hydride (2.5 g, 100 mmol, 98%) in DMF (100 mL) was added a solution of 4-hydroxy benzaldehyde (10.0 g, 82 mmol) in DMF (100 mL) slowly dropwise at 25-30° C. and stirred for 30 min at 25-30° C. 2,2-diethoxy-1-bromoethane (19.7 g, 100 mmol) was added to the reaction mixture. The reaction mixture was immersed in a preheated oil bath at 60° C. and stirring was continued for 48 h at 60° C. The reaction mixture was cooled to room temperatures, quenched with water (200 mL) and extracted with ethyl acetate (3×300 mL). The combined organic layers were washed with brine, dried over anhydrous Na 2 SO 4 and concentrated. The crude compound was purified by column chromatography using EtOAc:pet. ether (1:2) as eluent to yield the title compound (12.65 g, 58%) as a brown coloured liquid.
1 H NMR (CDCl 3 ): δ 9.88 (s, 1H), 7.82 (d, J=8.63 Hz, 2H), 7.02 (d, J=8.63 Hz, 2H), 4.85 (t, J=5.17 Hz, 1H), 4.08 (d, J=7.17 Hz, 2H), 3.88−3.50 (m, 4H), 1.24 (t, J=7.03 Hz, 6H).
EXAMPLE 1
5-[4-[(2,2-Diethoxy)ethoxy]phenyl methylene]thiazolidin-2,4-dione
A mixture of 4-[(2,2-diethoxy]ethoxy]benzaldehyde (10.6 g, 44.53 mmol), thiazolidin-2,4-dione (5.21 g, 44.53 mmol), benzoic acid (0.70 g, 5.78 mmol) and piperidine (0.64 mL, 6.7 mmol) in toluene (150 mL) was refluxed for 2 h with continuous removal of water. The reaction mixture was cooled to room temperature and diluted with EtOAc (150 ml). The mixture was washed with water, brine, dried over anhydrous Na 2 SO 4 and concentrated. The crude compound was purified by column chromatography using EtOAc:pet. ether (1:2) as eluent to afford the title compound (12.54 g, 70%) as a brown coloured liquid.
1 H NMR (CDCl 3 ): δ 8.70 (bs, 1H, D 2 O exchangeable), 7.80 (s, 1H), 7.45 (d, J=8.72 Hz, 2H), 7.02 (d, J=8.72 Hz, 2H), 4.87 (t, J=5.21 Hz, 1H), 4.08 (d, J=5.21 Hz, 2H), 3.90−3.52 (m, 4H), 1.26 (t, J=7.02 Hz, 6H).
EXAMPLE 2
5-[4-[(2,2-Diethoxy)ethoxy]phenyl methyl]thiazolidin-2,4-dione
A solution of 5-[4-[(2,2-diethoxy)ethoxy]phenyl methylene]thiazolidin-2,4-dione (8.0 g, 23.7 mmol) obtained in example 1, in 1,4-dioxane (100 mL) was reduced with hydrogen in the presence of 10% palladium on charcoal (16.0 g) at 60 psi for 60 h. The mixture was filtered through a bed of celite. The filtrate was evaporated to dryness under reduced pressure; purified by column chromatography using EtOAc:pet. ether (1:1) as an eluent to afford the title compound (8.04 g, 67%) as a colourless liquid.
1 H NMR (CDCl 3 ): δ 8.75 (bs, 1H, D 2 O exchangeable), 7.14 (d, J=8.63 Hz, 2H), 6.87 (d, J=8.63 Hz, 2H), 4.84 (t, J=5.25 Hz, 1H), 4.49 (dd, J=9.46, 3.83 Hz, 1H), 3.99 (d, J=5.25 Hz, 2H), 3.88−3.52 (m, 4H), 3.45 (dd, J=14.11, 3.83 Hz, 1H), 3.10 (dd, J=14.11, 9.46 Hz, 1H), 1.25 (t, J=7.03 Hz, 6H).
EXAMPLE 3
5-[4-[[4-Oxo-3,4-dihydro-(2H)-1,3-benzoxazine-2-yl]methoxy]phenyl methyl]thiazolidin-2,4-dione
To a stirred solution of polyphosphonate ethyl ester (PPE) (3.15 g, 7.29 mmol) in chloroform (4.0 mL) was added salicylamide (0.5 g, 3.65 mmol) followed by addition of a solution of 5-[4-[(2,2-diethoxy)ethoxy]phenyl methyl]thiazolidin-2,4-dione (1.36 g, 4.0 mmol) obtained in example 2, in chloroform (10 mL) dropwise at 25-30° C. The reaction mixture was immersed in a preheated oil bath and refluxed for 3 h. The reaction mixture was cooled to room temperature and CHCl 3 was removed under reduced pressure. To the resultant residue aq. sat. NaHCO 3 solution (25 mL) was added and stirred for 30 min. at 25-30° C. The precipitated brown coloured solid was filtered and purified by column chromatography using EtOAc:pet. ether (1:1) to yield the title compound (1.15 g, 81%). mp: 134° C.-138° C.
1 H NMR (CDCl 3 ): δ 11.80 (bs, 1H, D 2 O exchangeable), 8.40 (bs, 1H, D 2 O exchangeable), 7.9 (d, J=7.50 Hz, 1H), 7.15 (d, J=8.30 Hz, 2H), 7.05 (t, J=7.50 Hz, 1H), 6.90 (d, J=7.50 Hz, 1H), 6.80 (d, J=8.30 Hz, 2H), 5.80 (t, J=5.30 Hz, 1H), 4.42 (dd, J=9.50, 3.80 Hz, 1H), 4.30−4.10 (m, 2H), 3.34 (dd, J=14.10, 3.80 Hz, 1H), 3.02 (dd, J=14.10, 9.50 Hz, 1H).
EXAMPLE 4
5-[4-[[3-Methyl-4-oxo-3,4-dihydro-(2H)-1,3-benzoxazine-2-yl]methoxy]phenyl methyl]thiazolidin-2,4-dione
The title compound (0.4 g, 60%) was obtained from N-methyl salicylamide (250 mg, 1.66 mmol), 5-[4-[(2,2-diethoxy)ethoxy]phenyl methyl]thiazolidin-2,4-dione (620 mg, 1.82 mmol) obtained in example 2 and PPE (1.40 g, 3.32 mmol), by a similar procedure to that described in example 3. mp: 187° C.
1 H NMR (CDCl 3 ): δ 8.23 (bs, 1H, D 2 O, exchangeable), 7.95 (d, J=7.50 Hz, 1H), 7.43 (t, J=7.50 Hz, 1H), 7.12 (d, J=8.54 Hz, 2H), 7.08 (t, J=7.50 Hz, 1H), 6.93 (d, J=7.50 Hz, 1H), 6.77 (d, J=8.54 Hz, 2H), 5.62 (t, J=5.39 Hz, 1H), 4.48 (dd, J=9.04, 3.74 Hz, 1H), 4.32−4.08 (m, 2H), 3.45 (dd, J=14.05, 3.74 Hz, 1H), 3.21 (d, J=3.83 Hz, 3H), 3.10 (dd, J=14.05, 9.04 Hz, 1H).
EXAMPLE 5
5-[4-[[3-Ethyl-4-oxo-3,4-dihydro-(2H)-1,3-benzoxazine-2-yl]methoxy]phenyl methyl]thiazolidin-2,4-dione
The title compound (0.51 g, 69%) was obtained from N-ethyl salicylamide (300 mg, 1.82 mmol) and 5-[4-[(2,2-diethoxy)ethoxy]phenyl methyl]thiazolidin-2,4-dione (677 mg, 1.99 mmol) obtained in example 2 and PPE (1.57 g, 3.64 mmol) by a similar procedure to that described in example 3. mp: 70-72° C.
1 H NMR (CDCl 3 ): δ 8.10 (bs, 1H, D 2 O exchangeable), 7.96 (d, J=7.50 Hz, 1H), 7.41 (t, J=7.50 Hz, 1H), 7.11 (d, J=8.40 Hz, 2H), 7.05 (t, J=7.50 Hz, 1H), 6.91 (d, J=7.50 Hz, 1H), 6.72 (d, J=8.40 Hz, 2H), 5.62 (t, J=5.40 Hz, 1H), 4.48 (dd, J=9.03, 3.87 Hz, 1H), 4.42−3.90 (m, 3H), 3.50−3.02 (m, 3H), 1.28 (t, J=7.05 Hz, 3H).
EXAMPLE 6
Step A
5-[4-[[2,3-Dimethyl-4-oxo-3,4-dihydro-(2H)-1,3-benzoxazin-2-yl]methoxy]phenyl methyl]-2-iminothiazolidin-4-one
A mixture of ethyl 2-bromo-3-[4-[[2,3-dimethyl-4-oxo-3,4-dihydro-(2H)-1,3-benzoxazine-2-yl]methoxy]phenyl]propionate (1.5 g, 3.25 mmol) obtained in preparation 4, fused sodium acetate (884 mg, 6.5 mmol) and thiourea (493 mg, 6.5 mmol) in ethanol (12 mL) was refluxed for 12 h. The reaction mixture was cooled to room temperature and ethanol was removed under reduced pressure. The resultant residue was diluted with ethyl acetate and washed with water. Ethyl acetate layer was dried over anhydrous Na 2 SO 4 and concentrated. The crude compound was chromatographed on silica gel using EtOAc:pet. ether (1:1) as eluent to obtain the title compound (1.1 g, 82%).
1 H NMR (DMSO-d 6 ): δ 7.91 (d, J=7.50 Hz, 1H), 7.40 (t, J=7.50 Hz, 1H), 7.05 (d, J=8.30 Hz, 2H), 7.02 (t, J=7.50 Hz, 1H), 6.88 (d, J=7.50 Hz, 1H), 6.70 (d, J=8.30 Hz, 2H), 4.41 (dd, J=9.50, 3.75 Hz, 1H), 4.11 (s, 2H), 3.45 (dd, J=14.12, 3.75 Hz, 1H), 3.18 (s, 3H), 2.92 (dd, J=14.12, 9.50 Hz, 1H), 1.82 (s, 3H).
Step B
5-[4-[[2,3-Dimethyl-4-oxo-3,4-dihydro-(2H)-1,3-benzoxazine-2-yl]methoxy]phenyl methyl]thiazolidin-2,4-dione
To a stirred solution of the compound (1 g, 2.43 mmol) obtained above in ethanol (20 mL) was added 2N HCl (5 mL) and refluxed for 12 h. The reaction mixture was cooled to room temperature and ethanol was removed under reduced pressure. The aqueous layer was neutralised with saturated aqueous NaHCO 3 solution and extracted with EtOAc (2×50 mL). The combined organic layers were washed with brine, dried over anhydrous Na 2 SO 4 and concentrated. The crude compound was chromatographed on silica gel using EtOAc:pet. ether (1:1) as eluent to yield tie title compound (450 mg, 45%). mp: 58-60° C.
1 H NMR (CDCl 3 ): δ 7.92 (d, J=8.30 Hz, 1H), 7.42 (t, J=8.30 Hz, 1H), 7.12 (d, J=8.50 Hz, 2H), 7.06 (t, J=8.30 Hz, 1H), 6.87 (d, J=8.30 Hz, 1H), 6.76 (d, J=8.50 Hz, 2H), 4.50 (s, 2H), 4.48 (dd, J=9.30, 3.90 Hz, 1H), 3.40 (dd, J=14.11, 3.90 Hz, 1H), 3.18 (d, J=4.24 Hz, 3H), 3.08 (dd, J=14.11, 8.30 Hz, 1H), 1.85 (s, 3H).
EXAMPLE 7
5-[4-[[4-Oxo-3,4-dihydro-2H)-1,3-benzoxazine-2-yl]methoxy]phenyl methyl]thiazolidin-2,4-dione, sodium Salt
To a stirred suspension of 5-[4-[[4-oxo-3,4-dihydro-(2H)-1,3-benzoxazine-2-yl]methoxy]phenyl methyl]thiazolidin-2,4-dione (250 mg, 0.65 mmol) obtained from example 3, in methanol (4 mL) was added a solution of sodium methoxide (55 mg, 1.0 mmol) in methanol (1 mL) dropwise at 25-30° C. During this period the suspension slowly dissolved completely and a white solid precipitated out which was stirred further for 1 h. The solid was filtered and washed with methanol (2 mL) and dried to afford the title compound (250 mg, 95%). mp: 280° C.
1 H NMR (DMSO-d 6 ): δ 7.70 (d, J=7.50 Hz, 1H), 7.35 (t, J=7.50 Hz, 1H), 7.10 (d, J=8.30 Hz, 2H), 7.00 (d, J=7.50 Hz, 1H), 6.85 (d, J=7.50 Hz, 1H), 6.75 (d, J=8.30 Hz, 2H), 5.70 (t, J=5.30 Hz, 1H), 4.05 (dd, J=8.95, 3.90 Hz, 1H), 3.90−3.80 (m, 2H), 3.23 (dd, J=13.80, 3.90 Hz, 1H), 2.65 (dd, J=13.80, 8.95 Hz, 1H).
EXAMPLE 8
5-[4-[[3-Methyl-4-oxo-3,4-dihydro-(2H)-1,3-benzoxazine-2-yl]methoxy]phenyl methyl]thiazolidin-2,4-dione, sodium salt
The title compound (136 mg, 81%) was obtained from 5-[4-[[3-methyl-4-oxo-3,4-dihydro-(2H)-1,3-benzoxazine-2-yl]methoxy]phenyl methyl]thiazolidin-2,4-dione (150 mg, 0.39 mmol) obtained in example 4, by a similar procedure to that described in example 7. mp: 205-298° C.
1 H NMR (CDCl 3 +DMSO-d 6 ): δ 7.78 (d, J=7.50 Hz, 1H), 7.48 (t, J=7.50 Hz, 1H), 7.35−6.95 (m, 4H), 6.75 (d, J=8.30 Hz, 2H), 5.86 (t, J=4.98 Hz, 1H), 4.20 (d, J=4.98 Hz, 2H), 4.06 (dd, J=10.38, 3.23 Hz, 1H), 3.24 (dd, J=13.70, 3.23 Hz, 1H), 3.09 (s, 3H), 2.64 (dd, J=13.70, 10.38 Hz, 1H).
EXAMPLE 9
5-[4-[[1,3-Dimethyl-4-oxo-1,2,3,4-tetrahydro-2-quinazolinyl]methoxy]phenyl methylene]thiazolidin-2,4-dione
The title compound was obtained from N,N′-dimethylanthranilamide (500 mg, 3.04 mmol), 5-[4-[(2,2-diethoxy)ethoxy]phenyl methylene]thiazolidin-2,4-dione (1.13 g, 3.35 mmol) obtained in example 1 and PPE (2.63 g, 6.10 mmol) by a similar procedure to that described in example 3. mp: 236-240° C.
1 H NMR (DMSO-d 6 ): δ 7.72 (d, J=7.47 Hz, 1H), 7.57 (s, 1H), 7.50−7.30 (m, 3H), 6.96 (d, J=8.30 Hz, 2H), 6.90−6.60 (m, 2H), 5.23 (t, J=5.30 Hz, 1H), 4.22 (d, J=5.30 Hz, 2H), 3.14 (s, 3H), 3.07 (s, 3H).
EXAMPLE 10
5-[4-[[3-Methyl-4-oxo-1,2,3,4-tetrahydro-2-quinazolinyl]methoxy]phenyl methylene]thiazolidin-2,4,-dione
The title compound (800 mg, 65%) was obtained from N-methyl anthranilamide (500 mg, 3.3 mmol), 5-[4-[(2,2-diethoxy)ethoxy]phenyl methylene]thiazolidin-2,4-dione (1.23 g, 3.66 mmol) obtained from example 2 and PPE (2.85 g, 6.6 mmol) by a similar procedure to that described in example 3. mp: 66-68° C.
1 H NMR (DMSO-d 6 ): δ 7.67 (s, 1H), 7.63 (d, J=7.80 Hz, 1H), 7.51 (d, J=8.60 Hz, 2H), 7.23 (t, J=7.80 Hz, 1H), 7.03 (d, J=8.60 Hz, 2H), 6.80−6.60 (m, 2H), 5.12 (t, J=5.30 Hz, 1H), 4.14 (d, J=5.30 Hz, 2H), 3.08 (s, 3H).
EXAMPLE 11
5-[4-[[1,3-Dimethyl-4-oxo-1,2,3,4-tetrahydro-2-quinazolinyl]methoxy]phenyl methyl]thiazolidin-2,4-dione
Method A
The title compound (3.84 g, 82%) was obtained from N, N′-methylanthranilamide (1.87 g, 11.4 mmol), 5-[4-[(2,2-diethoxy)ethoxy]phenyl methyl]thiazolidin-2,4-dione (2.0 g, 5.8 mmol) obtained in example 2 and PPE (9.86 g, 22.8 mmol) by a similar procedure to that described in example 3. mp: 201.9° C.
Method B
The title compound (340 mg, 64%) was obtained from 5-[4-[[1,3-dimethyl-4-oxo-1,2,3,4-tetrahydro-2-quinazolinyl]methoxy]phenyl methylene]thiazolidin-2,4-dione (500 mg) obtained in example 9 by a similar procedure to that described in example 2.
1 H NMR (CDCl 3 ): δ 8.76 (bs, 1H, D 2 O exchangeable), 7.94 (d, J=7.50 Hz, 1H), 7.38 (t, J=7.50 Hz, 1H), 7.10 (d, J=8.30 Hz, 2H), 6.86 (t, J=7.50 Hz, 1H), 6.71 (d, J=8.30 Hz, 2H), 6.62 (d, J=7.50 Hz, 1H), 4.87 (t, J=5.81 Hz, 1H), 4.45 (dd, J=9.04, 3.83 Hz, 1H), 4.20−4.00 (m, 2H), 3.38 (dd, J=14.02, 3.83 Hz, 1H), 3.23 (s, 3H), 3.12 (s, 3H), 3.10 (dd, J=14.02, 9.04 Hz, 1H).
EXAMPLE 12
5-[4-[[3-Methyl-4-oxo-1,2,3,4-tetrahydro-2-quinazolinyl]methoxy]phenyl methyl]thiazolidin-2,4-dione
Method A:
The title compound (0.96 g, 95%) was prepared from 5-[4-[[3-methyl-4-oxo-3,4-dihydro-2-quinazolinyl]methoxy]phenyl methylene]thiazolidin-2,4-dione (1.0 g) (preparation described in copending U.S. application Ser. Nos. 08/777,627 and 08/884,816), by a similar procedure to that described in example 2.
Method B:
The title compound (350 mg, 44%) was obtained from N-methyl anthranilamide (272 mg, 2.0 mmol) and 5-[4-[(2,2-diethoxy)ethoxy]phenyl methyl]thiazolidin-2,4-dione (746 mg, 2.2 mmol) obtained from example 2 and PPE (1.73 g, 4.0 mmol) by a similar procedure to that described in example 3. mp: 86-90° C.
Method C:
The title compound (480 mg, 96%) was prepared from 5-[4-[[3-methyl-4-oxo-3,4-dihydro-2-quinazolinyl]methoxy]phenyl methyl]thiazolidin-2,4-dione (500 mg) (preparation described in copending U.S. application Ser. Nos. 08/777,627 and 08/884,816), by a similar procedure to that described in example 2.
Method D:
The title compound (440 mg, 88%) was prepared from 5-[4-[[3-methyl-4-oxo-1,2,3,4-tetrahydro-2-quinazolinyl]methoxy]phenyl methylene]thiazolidin-2,4-dione (500 mg) obtained in example 10, by a similar procedure to that described in example 2.
1 H NMR (CDCl 3 ): δ 8.23 (bs, 1H, D 2 O exchangeable), 7.95 (d, J=7.50 Hz, 1H), 7.43 (t, J=7.50 Hz, 1H), 7.12 (d, J=8.54 Hz, 2H), 7.08 (t, J=7.50 Hz, 1H), 6.93 (d, J=7.50 Hz, 1H), 6.77 (d, J=8.54 Hz, 2H), 5.62 (t, J=5.39 Hz, 1H), 4.48 (dd, J=9.04, 3.74 Hz, 1H), 4.32−4.08 (m, 2H), 3.45 (dd, J=14.05, 3.74 Hz, 1H), 3.20 (d, J=3.83 Hz, 3H), 3.10 (dd, J=14.05, 9.04 Hz, 1H).
EXAMPLE 13
5-[4-[[3-Ethyl-1-methyl-4-oxo-1,2,3,4-tetrahydro-2-quinazolinyl]methoxy]phenyl methyl]thiazolidin-2,4-dione
The title compound (1.6 g, 65%) was obtained from 2-(N-methyl)amino-N-ethyl benzamide (1.08 g, 6.06 mmol) and 5-[4-[(2,2-diethoxy)ethoxy]phenyl methyl]thiazolidin-2,4-dione (2.26 g, 6.68 mmol) obtained in example 2 and PPE (5.23 g, 12.13 mmol) by a similar procedure to that described in example 3. mp: 72-74° C.
1 H NMR (CDCl 3 ): δ 11.99 (bs, 1H, D 2 O exchangeable), 7.69 (d, J=7.50 Hz, 1H), 7.36 (t, J=7.50 Hz, 1H), 7.09 (d, J=8.30 Hz, 2H), 6.78 (t, J=7.50 Hz, 1H), 6.76 (d, J=8.30 Hz, 2H), 6.68 (d, J=7.50 Hz, 1H), 5.18 (t, J=5.30 Hz, 1H), 4.84 (dd, J=8.62, 4.47 Hz, 1H), 4.05 (q, J=7.05 Hz, 2H), 4.12−3.80 (m, 2H), 3.36 (dd, J=14.05, 4.47 Hz, 1H), 3.06 (s, 3H), 3.13 (dd, J=14.05, 8.62 Hz, 1H), 1.18 (t, J=7.05 Hz, 3H).
EXAMPLE 14
5-[4-[[1-Methyl-4-oxo-1,2,3,4-tetrahydro-2-quinazolinyl]methoxy]phenyl methyl]thiazolidin-2,4-dione
The title compound (450 mg, 23%) was obtained from 2-(N-methyl)amino benzamide (750 mg, 5.0 mmol) and 5-[4-[(2,2-diethoxy)ethoxy]phenyl methyl]thiazolidin-2,4-dione (1.87 g, 5.51 mmol) obtained in example 2 and PPE (4.33 g, 10.02 mmol) by a similar procedure to that described in example 3. mp: 108-110° C.
1 H NMR (CDCl 3 ): δ 10.10 (bs, 1H, D2O exchangeable), 7.93 (d, J=7.50 Hz, 1H), 7.42 (t, J=7.50 Hz, 1H), 7.09 (d, J=8.53 Hz, 2H), 6.84 (t, J=7.50 Hz, 1H), 6.73 (d, J=8.53 Hz, 2H), 6.64 (d, J=7.50 Hz, 1H), 4.98 (t, J=4.56 Hz, 1H), 4.43 (dd, J=8.90, 3.97 Hz, 1H), 4.20−3.82 (m, 2H), 3.37 (dd, J=14.11, 3.97 Hz, 1H), 3.12 (dd, J=14.11, 8.90 Hz, 1H), 3.10 (s, 3H).
EXAMPLE 15
5-[4-[[1,3-Dimethyl-4-oxo-1,2,3,4-tetrahydro-2-quinazolinyl]methoxy]phenyl methyl]thiazolidin-2,4-dione, sodium salt
The title compound (150 mg, 95%) was obtained from 5-[4-[[1,3-dimethyl-4-oxo-1,2,3,4-tetrahydro-2-quinazolinyl]methoxy]phenyl methyl]thiazolidin-2,4-dione (150 mg, 0.36 mmol) obtained in example 11, by a similar procedure described in example 7. mp: 281-237° C.
1 H NMR (CDCl 3 ): δ 7.72 (d, J=7.50 Hz, 1H), 7.40 (t, J=7.50 Hz, 1H), 7.10 (d, J=8.30 Hz, 2H), 6.90−6.66 (m, 4H), 5.20 (t, J=5.30 Hz, 1H), 4.20−4.05 (m, 3H), 3.32 (dd, J=13.53, 3.23 Hz, 1H), 3.13 (s, 3H), 3.07 (s, 3H), 2.62 (dd, J=13.52, 10.70 Hz, 1H).
EXAMPLE 16
5-[4-[[4-Oxo-1,2,3,4-tetrahydro-2-quinazolinyl]methoxy]phenyl methyl]thiazolidin-2,4-dione
The title compound (0.42 g, 50%) was obtained from anthranilamide (0.3 g, 2.2 mmol) and 5-[4-[(2,2-diethoxy]ethoxy]phenyl methyl]thiazolidin-2,4-dione (0.82 g, 2.42 mmol) obtained in example 2 and PPE (1.91 g, 4.4 mmol) by a similar procedure to that described in example 3. m.p: 81-83° C.
1 H NMR (CDCl 3 ): δ 8.59 (bs, 1H, D 2 O exchangeable), 7.89, (d, J=7.70 Hz, 1H), 7.35 (t, J=7.50 Hz, 1H), 7.15 (d, J=8.62 Hz, 2H), 6.95−6.75 (m, 3H), 6.69 (d, J=7.50 Hz, 1H), 5.20 (t, J=5.70 Hz, 1H), 4.65 (bs, 1H, D 2 O exchangeable), 4.49 (dd, J=9.03, 4.06 Hz, 1H), 4.20−4.10 (m, 1H), 4.10−3.92 (m, 1H), 3.40 (dd, J=14.12, 4.06 Hz, 1H), 3.18 (dd, J=14.12, 9.03 Hz, 1H).
EXAMPLE 17
5-[4-[[1,3-Diethyl-4-oxo-1,2,3,4-tetrahydro-2-quinazolinyl]methoxy]phenyl methyl]thiazolidin-2,4-dione
The title compound (0.4 g, 53%) was obtained from N, N′-diethylanthranilamide (0.32 g, 1.66 mmol) and 5-[4-[(2,2-diethoxy]ethoxy]phenyl methyl]thiazolidin-2,4-dione (0.62 g, 1.83 mmol) obtained in example 2 and PPE (1.44 g, 3.37 mmol) by a similar procedure to that described in example 3. m.p: 74-76° C.
1 H NMR (CDCl 3 ): δ 8.60 (bs, 1H, D 2 O exchangeable), 7.95, (d, J=7.50 Hz, 1H), 7.36 (t, J=7.50 Hz, 1H), 7.09 (d, J=8.60 Hz, 2H), 6.86 (t, J=7.57 Hz, 1H), 6.75 (d, J=7.50 Hz, 1H), 6.71 (d, J=8.60 Hz, 2H), 4.92 (t, J=5.81 Hz, 1H), 4.46 (dd, J=9.13, 3.73 Hz, 1H), 4.20−3.90 (m, 3H), 3.90−3.00 (m, 5H), 1.45−1.15 (m, 6H).
EXAMPLE 18
5-[4-[[1-Ethyl-3-methyl-4-oxo-1,2,3,4-tetrahydro-2-quinazolinyl]methoxy]phenyl methyl]thiazolidin-2,4-dione
The title compound (575 mg, 52%) was obtained from N-ethyl-N′-methylanthranilamide (460 mg, 2.58 mmol) and 5-[4-[(2,2-diethoxy]ethoxy]phenyl methyl]thiazolidin-2,4-dione (963 mg, 2.8 mmol) obtained in example 2 and PPE (1.91 g, 4.4 mmol) by a similar procedure to that described in example 3. m.p: 165° C.
1 H NMR (CDCl 3 ): δ 8.30 (bs, 1H, D 2 O exchangeable), 7.96 (d, J=7.50 Hz, 1H), 7.38 (t, J=7.50 Hz, 1H), 7.11 (d, J=8.50 Hz, 2H), 6.88 (t, J=7.50 Hz, 1H), 6.76 (d, J=7.50 Hz, 1H), 6.72 (d, J=8.50 Hz, 2H), 4.89 (t, J=5.80 Hz, 1H), 4.47 (dd, J=8.36, 3.78 Hz, 1H), 4.10−3.95 (m, 2H), 3.70−3.50 (m, 1H), 3.50−3.30 (m, 2H), 3.24 (d, J=3.72, 3H), 3.20−3.00 (m, 1H), 1.30 (t, J 7.06 Hz, 3H).
EXAMPLE 19
5-[4-[[1-Ethyl-4-oxo-1,2,3,4-tetrahydro-2-quinazolinyl]methoxy]phenyl methyl]thiazolidin-2,4-dione
The title compound (240 mg, 43%) was obtained from N-ethyl anthranilamide (300 mg, 1.83 mmol) and 5-[4-[(2,2-diethoxy]ethoxy]phenyl methyl]thiazolidin-2,4-dione (680 mg, 2.0 mmol obtained in example 2 and PPE (1.58 g, 3.65 mmol) by a similar procedure to that described in example 3. m.p: 77-79° C.
1 H NMR (CDCl 3 ): δ 9.40 (bs, 1H, D 2 O exchangeable), 7.95 (d, J=7.50 Hz, 1H), 7.39 (t, J=7.50 Hz, 1H), 7.09 (d, J=8.50 Hz, 2H), 6.95−6.65 (m, 4H), 4.99 (t, J=5.70 Hz, 1H), 4.44 (dd, J=8.30, 3.00 Hz, 1H), 4.15−3.90 (m, 2H), 3.75−3.50 (m, 1H), 3.50−3.25 (m, 2H), 3.20−3.00 (m, 1H), 1.30 (t, J=7.48 Hz, 3H).
Mutation in colonies of laboratory animals and different sensitivities to dietary regimens have made the development of animal models with non-insulin dependent diabetes associated with obesity and insulin resistance possible. Genetic models such as db/db and ob/ob (See Diabetes, (1982) 31(1): 1-6) in mice and fa/fa and zucker rats have been developed by the various laboratories for understanding the pathophysiology of disease and testing the efficacy of new antidiabetic compounds (Diabetes, (1983) 32: 830-838; Annu. Rep. Sankyo Res. Lab. (1994) 46: 1-57). The homozygous animals, C57 BL/KsJ-db/db mice developed by Jackson Laboratory, U.S., are obese, hyperglycemic, hyperinsulinemic and insulin resistant (J. Clin. Invest., (1990) 85: 962-967), whereas heterozygous are lean and normoglycemic. In db/db model, mouse progressively develops insulinopenia with age, a feature commonly observed in late stages of human type II diabetes when blood sugar levels are insufficiently controlled. The state of pancreas and its course vary according to the models. Since this model resembles that of type II diabetes mellitus, the compounds of the present invention were tested for blood sugar and triglycerides lowering activities.
The compounds of the present invention showed blood sugar and triglycerides lowering activities through improved insulin resistance. This was demonstrated by the following in vivo experiments.
Male C57BL/KsJ-db/db mice of 8 to 14 weeks age, having body weight range of 35 to 60 grams, procured from the Jackson Laboraotory, U.S.A., were used in the experiment. The mice were provided with standard feed (National Institute of Nutrition, Hyderabad, India) and acidified water, ad libitum. The animals having more than 300 mg/dl blood sugar were used for testing. The number of animals in each group was 4.
The random blood sugar and triglyceride levels were measured by collecting blood (100 μl) through orbital sinus, using heparinised capillary in tubes containing EDTA which was centrifuged to obtain plasma. The plasma glucose and triglycerides levels were measured spectrometrically, by glucose oxidase and glycerol-3-PO 4 oxidase/peroxidase enzyme (Dr. Reddy's Lab. Diagnostic Division Kits, Hyderabad, India) methods respectively. On 6th day the blood samples were collected one hour after administration of test compounds/vehicle for assessing the biological activity.
Test compounds were suspended on 0.25% carboxymethyl cellulose and administered to test group at a dose of 1 mg to 100 mg/kg through oral gavage daily for 6 days. The control group received vehicle (dose 10 ml/kg). Troglitazone (100 mg/kg, daily dose) was used as a standard drug which showed 28% reduction in random blood sugar level on 6th day.
The blood sugar and triglycerides lowering activities of the test compound was calculated according to the formula: Blood sugar / triglycerides lowering activity ( % ) = 1 - DT / DC TC / ZC × 100
ZC=Zero day control group value
DC=Zero day treated group value
TC=Control group value on test day
DT=Treated group value on the test day
No adverse effects were observed for any of the mentioned compounds of invention in the above test. The compounds of the present invention also showed cholesterol lowering activity in the experimental animals used.
Dose
Maximum reduction in
Triglyceride
Compound
(mg/kg/day)
blood glucose level (%)
lowering (%)
Example 12
3
55
35
Example 11
1
34
28
Example 4
10
48
42
Example 3
10
41
48
The experimental results from the db/db mice suggest that the novel compounds of the present invention also possess therapeutic utility as a prophylactic or regular treatment for obesity, cardiovascular disorders such as hypertension, hyperlipidaemia and other diseases; as it is known from the literature that such diseases are interrelated to each other.
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The present invention relates to novel antidiabetic compounds, their tautomeric forms, their derivatives, their analogues, their stereoisomers, their polymorphs, their pharmaceutically acceptable salts, their pharmaceutically acceptable solvates and pharmaceutically acceptable compositions containing them. This invention particularly relates to novel azolidinediones of the general formula (I), their analogues, their derivatives, their tautomeric forms, their stereoisomers, their polymorphs, their pharmaceutically acceptable salts, pharmaceutically acceptable solvates and pharmaceutical compositions containing them
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BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to an electric oil pump that can greatly improve the operation, increase the endurance, and extend the service life of an Oldham's coupling connecting a drive shaft that rotates a rotor in a pump housing and a motor output shaft in a motor housing.
2. Description of the Related Art
Electric oil pumps comprising a combination of a pump housing having a drive shaft provided with a rotor of an inner contact gear type and a motor housing having a motor for rotating the drive shaft mounted on the rotor have been used as pumps in lubrication systems of automobiles or the like. A specific example of such electric oil pump is described in Japanese Patent Application Laid-open No. H11-173278. The essence of the invention disclosed in this application is that a hydraulic gear pump and a motor are connected via a bracket. A drive shaft on the side of the hydraulic gear pump and a rotor shaft on the side of the motor are connected via a coupling, and an Oldham's coupling is disclosed as an example of the coupling.
The construction of the Oldham' coupling disclosed in Japanese Patent Application Laid-open No. H11-173278 enables the rotation transfer even when the input shaft and output shaft are not coaxial. A plate-shaped protrusion is formed on the distal end of the output shaft of the motor, and a groove for inserting the protrusion is formed on the input shaft side of the pump housing. The output shaft of the motor rotates and the rotor shaft rotates in a state where the plate shaped protrusion is inserted into the groove. In this case, the rotation is transferred even though the input shaft and output shaft are not coaxial, but the plate-shaped protrusion and the groove rub against each other and the surfaces thereof wear each other in long-term usage, thereby decreasing the strength of the coupling. It is an object of the present invention to increase the endurance and extend the service life of the Oldham's coupling connecting the output shaft and input shaft.
SUMMARY OF THE INVENTION
With the foregoing in view, the inventors have conducted a comprehensive study aimed at the resolution of the above-described problems, and the invention of claim 1 resolves the problems by providing an electric oil pump comprising a pump housing comprising a rotor and a drive shaft for rotatably supporting the rotor, and a motor housing connected to the pump housing and having an output shaft connected to the drive shaft via an Oldham's coupling, wherein a coupling chamber for accommodating the Oldham's coupling and a linking channel for transporting the leaked oil from a rotor chamber of the pump housing where a rotor is accommodated to the coupling chamber are provided in the pump housing.
The invention of claim 2 resolves the problems by providing an electric oil pump comprising a pump housing having a cover section having a bearing hole formed therein, a pump body section having a rotor chamber formed therein, and a base section having a shaft through hole and a coupling chamber connected to the shaft through hole and opened outwardly, a drive shaft rotatably supported by the bearing hole and shaft through hole and protruding into the coupling chamber, a rotor accommodated in the rotor chamber, and a motor housing comprising an output shaft connected by an Oldham's coupling to the drive shaft protruding into the coupling chamber, wherein an annular drain groove is formed between the cover section and the pump body section or between the pump body section and the base section, surrounding the rotor chamber; and a linking channel for linking the annular drain groove and the coupling chamber is formed in the pump body section and the base section.
Furthermore, the invention of claim 3 resolves the problems by providing the electric oil pump of the above-described configuration, wherein an annular drain groove surrounding the rotor chamber is formed between the cover section and pump body section and between the pump body section and base section.
The invention of claim 4 resolves the problems by providing the electric oil pump of the above-described configuration, comprising a discharge channel leading from the linking channel to an oil pan, wherein the position of the coupling chamber is below the position of a discharge section provided in the oil pan. The invention of claim 5 resolves the problems by providing the electric oil pump of the above-described configuration, wherein a linking channel is formed between the bearing hole and the annular drain groove in the cover section.
With the invention of claim 1 , a linking channel for transporting the leaked oil from a rotor chamber of the pump housing where a rotor is accommodated to the coupling chamber is provided in the Oldham's coupling. Therefore, the oil constantly spreads to the rubbing zone in the Oldham's coupling accommodated in the coupling chamber, good and stable rotation transfer is carried out from the output shaft of the motor housing to the drive shaft of the pump housing, and excellent endurance can be attained.
Furthermore, with the invention of claim 2 , because an annular drain groove surrounding the rotor chamber is formed between the cover section and the pump body section, the leaked oil from the rotor chamber can be reliably removed by the annular drain groove and the leaked oil can be effectively pumped, practically without any waste, to the coupling chamber. Other effects are almost identical to those of the invention of claim 1 . Furthermore, with the invention of claim 3 , forming annular drain grooves on both sides in the axial direction of the pump body section makes it possible to remove the leaked oil from both surfaces of the rotor chamber and to conduct rapid oil supply to the coupling chamber.
With the invention of claim 4 , providing a discharge channel leading from the linking channel to the oil pan makes it possible to pump the oil from the coupling chamber to the oil pan when the amount of leaked oil increases and pressure rises. Furthermore, because the coupling chamber is positioned below the discharge section provided in the oil pan, the coupling chamber can be maintained in a state where it is filled with oil.
With the invention of claim 5 , a linking channel is formed between the bearing hole and the annular drain groove. As a result, oil penetrates to the periphery of the shaft and lubrication can be ensured between the shaft and the bearing hole or the bearing, e.g., the shaft through hole. Furthermore, because the bearing holes in both end sections of the shaft and the coupling chamber are linked by the linking channel, they have the same pressure, the shaft is not displaced axially by the difference in pressure between the two end sections of the shaft, and stable rotation operation of the shaft can be ensured.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a side view with partial vertical cut-out illustrating the configuration of the present invention;
FIG. 2(A) is a front view of the cover section, (B) is a sectional side view of (A);
FIG. 3(A) is a front view of the pump body section, (B) is a sectional side view of (A);
FIG. 4(A) is a front view of the base section, (B) is a sectional side view of (A), (C) is a cross-sectional view of the main portion of (A);
FIG. 5 is an exploded perspective view of an Oldham's coupling;
FIG. 6 is an exploded side view with a partial vertical section illustrating the present invention;
FIG. 7 illustrates schematically the operation in which an electric oil pump in accordance with the present invention is mounted on an oil pan and the leaked oil is discharged from the discharge section into the oil pan;
FIG. 8 is a graph comparing the performance of the pump in accordance with the present invention and the conventional pump.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
Embodiments of the present invention will be described below based on the appended drawings. As shown in FIG. 1 and FIG. 6 , the electric oil pump in accordance with the present invention comprises a pump housing A, a motor housing B, a rotor 21 , and a drive shaft 22 . The rotor 21 and drive shaft 22 are mounted inside the pump housing A. The pump housing A comprises a cover section A 1 , a pump body section A 2 , and a base section A 3 , and those cover section A 1 , pump body section A 2 , and base section A 3 are joined via a fastener such as bolts and screws along the axial direction of the drive shaft 22 contained therein.
As shown in FIG. 1 and FIG. 6 , the cover section A 1 mainly comprises a cover body 1 and a bearing hole 2 . The bearing hole 2 is formed on the side of the surface of the cover body 1 where it is joined to the pump body section A 2 . The bearing hole 2 serves to support the drive shaft 22 inserted therein. Furthermore, as shown in FIG. 2 , port recesses 3 , 4 are formed around the bearing hole 2 . As shown in FIG. 4(A) , the port recesses 3 , 4 correspond to the positions of an intake port 15 and a discharge port 16 formed in the base section A 3 and have almost the same shape in the plane thereof as those intake port 15 and discharge port 16 . Furthermore, the port recesses 3 , 4 are in the form of shallow grooves.
Furthermore, as shown in FIG. 2 , an annular drain groove 5 is formed so as to surround the port recesses 3 , 4 . Furthermore, a seal groove 6 is formed on the outside of the annular drain groove 5 . A drain hole section 7 is formed between the annular drain groove 5 and seal groove 6 . The annular drain groove 5 is formed to surround from the outside the region of a rotor chamber 10 formed in the pump body section A 2 , and makes it possible to remove the leaked oil. The drain hole section 7 is formed to be located specifically in the lower portion of the cover section A 1 and crosses the annular drain groove 5 on the lower side thereof. The leaked oil flowing in the annular drain groove 5 is collected in the drain hole section 7 (see FIG. 2(B) ). As shown in FIG. 1 and FIG. 2 , this drain hole section 7 comprises a hole opening 7 a and a feed guide recess 7 b . The leaked oil that flowed out from the hole opening 7 a can be transferred in a stable state thereof along the feed guide recess 7 b to the main oil hole section 11 of the below-described pump body section A 2 .
The drain hole section 7 and bearing hole 2 are linked together via a first linking channel 8 . The first linking channel 8 passes through inside the cover body 1 of the corner section A 1 and serves to pump out the oil that leaked to the bearing hole 2 into the drain hole section 7 . The linking location of the first linking channel 8 and the bearing hole 2 comprises an axial linking passage 8 a with an inner diameter less than the bearing hole 2 and matching the linking location in the axial direction of the bearing hole 2 and a drain-side linking passage 8 b linked to the drain hole section 7 , and the channel is formed by the intersection of the axial linking passage 8 a and drain-side linking passage 8 b (see FIG. 2(B) ).
Furthermore, the pump body section A 2 is disposed between the cover section A 1 and base section A 3 , as shown in FIG. 6 . The rotor chamber 10 in the form of a through hole accommodating the rotor 21 is formed in a body main unit 9 . The main oil hole section 11 is formed in the position corresponding to the drain hole section 7 on the side of the surface of the pump body section A 2 that is joined to the cover section A 1 , and a second linking channel 12 is formed so as to pass from the main oil hole section 11 toward the surface of the pump body section A 2 that is joined to the base section A 3 .
The inner diameter of the main oil hole section 11 is formed larger than the inner diameter of the second linking channel 12 . The main oil hole section 11 serves to receive the leaked oil from the drain hole section 7 of the cover section A 1 and feed the leaked oil to the second linking channel 12 . Thus, the second linking channel 12 is linked to the first linking channel 8 and annular drain groove 5 formed in the cover section A 1 via the drain hole section 7 , and this second linking channel 12 transfers the oil that flowed in from the annular drain groove 5 of the cover section A 1 and the first linking channel 8 to a coupling chamber 20 formed in the base section A 3 .
As shown in FIG. 6 , in the base section A 3 , a shaft through hole 14 is formed in a base main unit 13 . Together with the bearing hole 2 formed in the cover section A 1 , the shaft through hole 14 serves as a bearing rotatably supporting the drive shaft 22 . As shown in FIGS. 4(A) and (C), the intake port 15 and discharge port 16 are formed around the shaft through hole 14 of the base main unit 13 . Those intake port 15 and discharge port 16 are formed to match the positions of the port recesses 3 , 4 when the pump body section A 2 and base section A 3 are joined together (see FIG. 1 ). The intake port 15 passes through to an oil pan 30 disposed on the outside of the pump housing A (see FIG. 1 and FIG. 7 ).
A third linking channel 17 is formed in the base main unit 13 . The third linking channel 17 is configured to be linked to the second linking channel 12 when the pump body section A 2 and base body A 3 are joined together. As shown in FIG. 1(A) and FIG. 4(B) , the third linking channel 17 is linked to the shaft through hole 14 . More specifically, a drain opening section 17 a is formed in the location where the shaft through hole 14 and the third linking channel 17 intersect. The drain opening section 17 a is formed as a zone expanding radially in part of the shaft through hole 14 and makes it possible to pump out the sufficient amount of oil transported from the third linking channel 17 to the shaft through hole 14 in the drain opening section 17 a .
Furthermore, a discharge channel 18 linked to the oil pan 30 is formed in the third linking channel 17 . As shown in FIG. 7 , the discharge channel 18 is linked to a discharge section 31 provided in the oil pan 30 . Furthermore, the position of the discharge section 31 provided in the oil pan 30 is set to be higher than the coupling chamber 20 . Owing to such a configuration, when the amount of leaked oil increased and pressure rises, the oil can be pumped out to the oil pan 30 via the discharge section 31 and also via the coupling chamber 20 . Furthermore, because the coupling chamber 20 is positioned below the discharge section 31 of the oil pan 30 , the coupling chamber 20 can be almost constantly maintained in a state in which it is filled with oil. A second annular drain groove 19 is formed in the surface of the base section A 3 where the base section is joined to the pump body section A 2 . The second annular drain groove 19 crosses the third linking channel 17 , and the oil present in the second annular drain groove 19 is caused to flow into the third linking channel 17 . Forming the two drain grooves makes it possible to remove the leaked oil from both surfaces of the rotor chamber and supply the rapidly flowing oil to the coupling chamber 20 .
Furthermore, as shown in FIG. 4(B) , the coupling chamber 20 is formed in the base main unit 13 of the base section A 3 in the joint surface thereof with the motor housing B. The coupling chamber 20 is formed as an almost cylindrical receding zone in the joining outer wall surface of the base main unit 13 . The coupling chamber 20 is linked to the shaft through hole 14 . The coupling chamber 20 comprises a leaked oil pool section 20 a with an inner diameter slightly larger than that of the shaft through hole 14 and a guide section 20 b serving as a guide for joining to the motor housing B. The leaked oil is accumulated in the leaked oil pool section 20 a and part of the guide section 20 b . The drive shaft 22 is disposed inside the coupling chamber 20 of the bump housing A. Furthermore, the drive shaft 22 is connected to an output shaft 26 of the monitor housing B via an Oldham's coupling 23 .
As shown in FIG. 6 , in the above-described cover section A 1 , pump body section A 2 , and base section A 3 , a rotor 21 constituting a pump with internal contact gears such as torodial gears is contained in the rotor chamber 10 of the pump body section A 2 , and the drive shaft 22 is mounted on the rotor 21 on the drive side thereof via a key or the like. Rotational support is provided by the bearing hole 2 on the side of the cover section A 1 and the shaft through hole 14 on the side of the base section A 3 . More specifically, one end of the drive shaft 22 in the axial direction is the portion fixedly attached to the rotor 21 and supported in the bearing hole 2 . The other end side of the drive shaft 22 in the axial direction thereof becomes an input side and serves for connection to the output shaft 26 of the motor housing B. The end portion 22 a on the input side of the drive shaft 22 is connected to the output shaft of the motor housing B via the Oldham's coupling 23 . A shaft seal 29 is provided on the motor section side in the coupling chamber 20 to seal the oil located inside the coupling chamber 20 .
In the motor housing B, the motor section is mounted inside a housing main unit 24 , and the output shaft 26 of the motor section. Furthermore, the output shaft 26 of the motor section is disposed inside a flange section 27 . The flange section 27 is connected to the base section A 3 of the pump housing A via a fastener such a screw or a bolt. A second coupling chamber 28 enabling the Oldham's coupling 23 to be inserted and disposed therein is also provided in the flange section 27 .
As shown in FIG. 5 , the Oldham's coupling 23 comprises insertion groove sections 23 a and insertion plate sections 23 b . The insertion plate sections 23 b are formed in the end portion 22 a on the input side of the drive shaft 22 and the distal end portion of the output shaft 26 , and the insertion groove sections 23 a are formed on both sides in the axial direction of a joint member 23 c . The insertion plate sections 23 b of the drive shaft 22 and output shaft 26 are configured to be inserted into respective insertion groove sections 23 a formed in the joint member 23 c.
A configuration is also possible in which respective insertion grooves 23 a are formed in the drive shaft 22 and output shaft 26 , and the insertion plate sections 23 b , 23 b are formed in both sides in the axial direction of the joint member 23 c . Furthermore, the joint members 23 c are disposed in the coupling chamber 20 of the pump housing A and the second coupling chamber 28 of the motor housing B, the Oldham's coupling 23 of the drive shaft 22 and output shaft 26 is configured, while inserting the insertion plate sections 23 b into the insertion grooves 23 a , and the pump housing A and motor housing B are joined.
FIG. 8 is a graph illustrating the amount of wear in the Oldham's coupling 23 with and without lubrication. The figure shows that feeding the leaked oil to the coupling chamber 20 in accordance with the present invention reduced the amount of wear in the rubbing zone of the Oldham's coupling 23 .
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An object of the invention is to provide an electric oil pump with greatly improved operation, increased endurance, and extended service life of an Oldham's coupling connecting a drive shaft that rotates a rotor in a pump housing and a motor output shaft in a motor housing.
The electric pump comprises a pump housing having a rotor and a drive shaft for rotatably supporting the rotor, and a motor housing connected to the pump housing and having an output shaft connected to the drive shaft via an Oldham's coupling. The pump housing is provided with a coupling chamber for accommodating the Oldham's coupling, and a linking channel for transporting the leaked oil from a rotor chamber accommodating the rotor of the pump housing to the coupling chamber.
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BACKGROUND
[0001] Videoconferencing entails exchange of audio, video, and other information between at least two participants. Generally, a videoconferencing endpoint at each participant location will include a camera for capturing images of the local participant and a display device for displaying images of remote participants. The videoconferencing endpoint can also include additional display devices for displaying digital content. In scenarios where more than two endpoints participate in a videoconferencing session, a multipoint control unit (MCU) can be used as a conference controlling entity. The MCU and endpoints typically communicate over a communication network, the MCU receiving and transmitting video, audio, and data channels from and to the endpoints.
[0002] FIG. 1 depicts an exemplary multipoint videoconferencing system 100 . System 100 can include network 110 , one or more multipoint control units (MCU) 106 , and a plurality of endpoints 1 - 5 101 - 105 . Network 110 can be, but is not limited to, a packet switched network, a circuit switched network, or a combination of the two. Endpoints 1 - 5 101 - 105 may send and receive both audio and video data. Communications over the network can be based on communication protocols such as H.320, H.324, H.323, SIP, etc., and may use compression standards such as H.263, H.264, etc. MCU 106 can initiate and manage videoconferencing sessions between two or more endpoints. Generally, MCU 106 can mix audio data received from one or more endpoints, generate mixed audio data, and send mixed audio data to appropriate endpoints. Additionally, MCU 106 can receive video streams from one or more endpoints. One or more of these video streams may be combined by the MCU 106 into combined video streams. Video streams, combined or otherwise, may be sent by the MCU 106 to appropriate endpoints to be displayed on their respective display screens. As an alternative, MCU 106 can be located at any one of the endpoints 1 - 5 101 - 105 .
[0003] Combining the video streams is typically based on a specified layout. A layout can be specified for various states and configurations of the video call. For example, the near end display layout for a 2-way call can include the video streams of the only far end videoconferencing device; however, a 3-way video call near end display may include various permutations and combinations of the two far end video streams. Historically, the layouts generated by the MCU for various call scenarios have been either hard-coded into the software running the MCU or have been configured by a system administrator of the MCU. In some cases, a layout is maintained regardless of the roster count (number of sites on a call). In many cases, the admin configuration may be inconsistent with what a user would desire to see in a particular scenario. Historically, changes to the layouts have been cumbersome or impossible for a user to make.
[0004] Moreover, whatever user-configurable layout changes were availble were not at all persistent, whether within a call, within calls made on the same device, or within calls made on different devices throughout a particular system, for example, all videoconferencing MCUs belonging to an organization. For example, users may have been able to configure certain layout variables such as dual monitor emulation (DME). Often this was done by toggleing through existing layouts. Unfortunatly, these selections would be lost when another site joined the call. Alternatively, in a bridge call, users might be able to use a far-end camera control feature or a touch screen to manually select the current layout, but it would not scale to the roster number. Additionally, whatever user-configurable layout parameters were available were device-specific, i.e., were stored locally only on the endpoint and/or MCU currently being used by the user. Thus, there has been no way for an admin to create a layout policy or for a user to have his layout preferences follow him from system to system.
SUMMARY
[0005] Disclosed herein are methods, systems, and techniques for creating media conferencing layouts that are intelligent (i.e., based on some underlying principle to enhance user-perceived conference quality) and persistent (i.e., consistent within a call and from one call to the next).
BRIEF DESCRIPTION OF THE DRAWINGS
[0006] Exemplary embodiments of the present invention will be more readily understood from reading the following description and by reference to the accompanying drawings, in which:
[0007] FIG. 1 illustrates an exemplary system in which various endpoints can communicate with each other and the multipoint control unit (MCU) over a communication network.
[0008] FIGS. 2A-2D illustrate various conferencing layouts.
[0009] FIG. 3 illustrates an exemplary block diagram of an endpoint including an MCU.
[0010] FIG. 4 illustrates a flowchart of an automated layout technique.
[0011] FIGS. 5-8 illustrate various conference layout parameter selection menus and associated conferencing layouts.
DETAILED DESCRIPTION
[0012] FIG. 3 illustrates an exemplary block diagram of an endpoint 301 , which includes a multipoint control unit MCU. Inclusion of an MCU allows the endpoint 301 to initiate, control, and maintain videoconferences in addition to performing the functionality of a typical videoconferencing endpoint. It is understood that the MCU portion of the endpoint 301 can be located outside the endpoint at the near end or across the network, as a standalone entity that communicates to all the endpoints (e.g., Endpoint 1 - 5 101 - 105 of FIG. 1 ) over the network.
[0013] The endpoint 301 can include and endpoint module 302 , which, in turn, includes the necessary hardware and software associated with a typical videoconferencing endpoint. For example, the endpoint module 302 can include a user interface 304 , which allows the user to input commands for controlling the operation of the endpoint module 302 , or even the entire endpoint 301 . The user interface 304 can include a keypad, keyboard, mouse, touchscreen, etc. and the associated software for accepting the user input. The user interface 304 can also include one or more displays, light emitting diodes (LEDs), etc., for providing status indications and other videoconferencing related data to the user. The user interface 304 can also provide such data visually on the monitors 313 - 315 . The user interface 304 can communicate with an endpoint processor 306 to send user commands and receive user data to be communicated to the user.
[0014] The endpoint processor 306 can control the operation of various components of the endpoint 301 as well as control communications between the endpoint module 302 and the MCU 303 or other endpoints over the network 110 . The end point processor 306 can be a microprocessor, microcontroller, a field programmable gate array (FPGA), an application specific integrated circuit (ASIC), or a combination thereof. The endpoint processor 306 can be coupled to a memory, which can be volatile (e.g., RAM) or non-volatile (e.g., ROM, FLASH, hard-disk drive, etc.). The memory can store all or portion of the software and data associated with the endpoint module 302 . The endpoint processor 306 can control the settings and orientation of the pan-tilt-zoom (PTZ) camera 311 , the display settings of the monitors (Monitor 1 313 , Monitor 2 314 , and Monitor 3 315 ), the (one or more) speaker 311 , and the microphone array 316 .
[0015] The audio and video codec module 305 can include audio and video encoders and decoders as well as communication protocols. For example, the codec module 305 can include audio codecs such as MPEG, G.722, etc. and video codecs such as MPEG-4, H.264, etc. The audio codec can encode audio signals received from the microphone array 316 and generate audio streams and can decode audio streams received from the MCU module 303 or from the network 110 for reproduction by the speaker 311 . The video codec can encode video frames captured by the camera 312 and generate video streams and can decode video streams received from the MCU 303 or over the network for reproduction on the monitors 313 - 315 . The audio and video streams generated by the codec 306 can be communicated to the MCU module 303 or to far end endpoints and MCUs over the network 110 . Communication over the network can be carried out via the network interface and communication module 310 .
[0016] As mentioned above, the MCU module 303 can initiate, control, and maintain videoconference sessions that can include the near end endpoint 301 and far end endpoints over the network 110 . The MCU module 303 can include various components as described in the H.323 specification, which is incorporated by reference in its entirety, and are not described further. The MCU module 303 can also include a presentation and layout manager 307 , which is responsible for deciding how video images related to a video conferencing session are presented to far end endpoints to the near end endpoint 301 on monitors 313 - 315 . As discussed in further detail below, the presentation and layout module 307 bases its decisions on various videoconferencing state and configuration changes, external commands, and external definition files.
[0017] The video and audio subsystem 308 receives data and instructions from the presentation module 307 and carries out audio and video mixing to generate audio and video streams that are sent to various far end and near end endpoints. The subsystem 308 can include various audio and video codecs for encoding and decoding audio and video streams received from various endpoints participating in a videoconferencing session.
[0018] The MCU processor 309 can control the operations of the MCU module 303 .
[0019] However, the MCU processor 309 can also include the functionality of the EP processor 306 for controlling the various components of the endpoint 301 . As such, the MCU processor 309 and the EP processor 306 can be implemented on the same processor. The MCU processor 309 can also communicate with the user interface 304 to receive MCU related commands from the user, and present MCU related indications and data to the user.
[0020] Operation details of Presentation and Layout Manager 307 will now be described, with particular reference to a new technique for layout management and persistence. However, before doing so, it is useful to describe the various elements that make up a layout. A first element that makes up a layout is illustrated in FIG. 2A . This element is the self-view or picture in picture. This element shows the local camera view to the local participant.
[0021] A second element that can make up the layout is a content view, illustrated in FIG. 2B . Content can include any variety of items that are not live people video. For example, content can be a shared document, such as a presentation, spreadsheet, etc. that is shown from a computer connected to the conferencing system. Additionally, content could be a view from a document camera. Some videoconferencing systems also include facilities to allow content to be shown from a USB memory device or other storage device connected to the conferencing system. In some cases, the content view can replace the self view and swap itself with the self view. This will be more readily understood in conjunction with the various layouts described below.
[0022] FIG. 2C illustrates a typical layout for a point-to-point call, i.e., a call with two participants whose videoconferencing terminals are directly connected. The video of a remote participant is illustrated in the main window 201 , with the self view illustrated as a picture-in-picture view 202 in the lower right portion of the remote participant view. FIG. 2D illustrates a typical layout for a multi-point call, i.e., a call with more than two participants connected via a multipoint control unit (MCU). The MCU can either be part of one of the participant endpoints or can be a separate device. In the example of FIG. 2D , six remote and one local participant (not shown) are on the call. In one embodiment the active speaker (i.e., the speaker who is currently talking) can be illustrated in a larger window 203 , while the other participants are illustrated in a plurality of smaller windows 204 - 208 . In some embodiments, the active speaker can also be highlighted, illustrated conceptually by the light shading of the background of active speaker view 203 . Other forms of highlighting, such as colored frames, etc. can also be used.
[0023] The various display elements referenced above can be advantageously combined in a variety of ways to present useful displays for a variety of conferencing scenarios. Preferably, conferencing and layout manager 307 can implement a variety of rules to provide consistency to the user experience. One exemplary set of rules is as follows:
Rule 1: Layouts are persistent over call scenarios. Thus, each time the user changes a layout for a certain number of endpoints in the call, the next time the user is in a call with the same number of endpoints, the same layout will be used. As an example, if a user is on a three way call and a fourth participant joins, then the layout will change to the layout used in the last four-way call. Rule 2: Rule 1 is followed only up to the number of displayable sites given the current monitor configuration. Each monitor configuration has a maximum number of sites that it can display. For example, a single monitor system may be limited to displaying four remote sites, while a dual monitor system may be limited to displaying five remote sites and a three-monitor system may be limited to six remote sites. Other limits are also possible. Additionally, the MCU may composite the video streams from a multiple sites into a single stream that can be treated as one remote site by the displaying endpoint. These techniques are generally known in the art and will not be discussed in detail herein. Rule 3: There are two layout tracks or “styles.” These are described herein as “full screen” and “dual monitor emulation” (DME). It is to be understood that DME mode can also include multi-monitor emulation for emulation of more than three monitors. In some embodiments, the system can remain on a given track or style within a call. Thus, for example, if the user is in a three way DME call, and a fourth participant joins the conference, the system can go to a four way DME layout (as opposed to a single monitor four way layout). Rule 4: The self view (discussed above) is persistent regardless of the number of sites on the call. Thus, for example, if a two way call with self view enabled is joined by a third participant, the self view remains enabled. Similarly, self view can be persistent from call to call. Thus, if self view is on and in a predetermined position in one call, it will be in the same position during the next call.
[0028] A flowchart for implementing these rules to create persistent layouts for a user is illustrated in FIG. 4 . The process begins at step 401 , which can coincide with call initiation. At that point the system can determine the current call type ( 402 ). This can include whether it is a point-to-point or multipoint call, the number of participants, whether dual monitor emulation (or multi-monitor emulation) is in use, etc. Once the call type is determined, the parameters for the last call of that type can be retrieved ( 403 ) from storage 404 . These retrieved parameters are then used ( 405 ) to configure a layout for a display 406 . The system can then check for a parameter change from the user ( 407 ). This might include any variety of setting changes, such as toggling the self view on and off, changing the location of the self view (see FIG. 5 ), etc. If there has been a user driven change of parameter, the new parameters for the current call type can be stored ( 408 ) in storage 404 . The system can then determine whether the call has ended ( 404 ). If so, then the call ends ( 410 ), if not, the process can repeat with determining the current call type ( 402 ). The call type may change during the call, for example, if a new participant joins or drops off the call, or if content is now being presented (or not), etc.
[0029] FIG. 5 illustrates conceptually a user toggle menu for self view state. There are a plurality of choices 501 - 509 . Options 501 - 505 are what are known as full screen views. These views include self view off ( 501 ), bottom right ( 502 ), top right ( 503 ), and top left ( 504 ). Options 506 - 509 are what are known as dual monitor emulation (DME) or multi-monitor emulation modes. These include bottom left ( 505 ), side-by-side ( 506 ), side-by-side reduced ( 507 ), below reduced ( 508 ), and above reduced ( 509 ). Also note the selection box indicating the current mode which is picture-in-picture bottom left, as indicated in the conferencing screen in front of which the menu appears. Similar menus may be presented for other layout options as further described below.
[0030] Another menu may be presented to a user allowing them to choose a layout or have the system choose a layout for them. One example of such a menu is illustrated in FIG. 6 . The menu allows the user to select automatic layout mode 601 (in which the system will preselect a layout type based on rules like those described above. Alternatively, the user can select discussion mode 602 , which shows all participants (up to the maximum number displayable) in separate regions of the screen in what is known as a “Hollywood Squares” layout. In this mode, the active speaker can be highlighted, or in variations of this mode, the active speaker may appear in a larger region. As yet another alternative, the user can select a full screen mode 603 , in which the current speaker is displayed full screen, with the optional self view shown or not (as selected using a menu like that of FIG. 5 .)
[0031] Numerous other combinations of these view elements are possible. Without limitation some of these various views are illustrated in FIGS. 7A-7B . For example, FIG. 7A represents a four site, full screen, no content view, with self view enabled. The self view 701 thus appears in one of the four regions. The overlaying menu for selecting various layouts includes full screen picture-in-picture ( 702 ), the currently selected view of full screen with self view, and various multi monitor emulation modes in which the self view and non-active speakers are presented in various positions relative to the active speaker in the larger window ( 703 - 705 ). FIG. 7B illustrates a selection of four person call arrangement but with content.
[0032] As the number of participants increases, the display arrangements become somewhat more complicated, but the same principles apply. As alluded to above, most videoconferencing endpoints have a maximum number of separate conference streams that can be displayed on a given display. However, for calls involving more participants, an MCU can composite multiple endpoints' streams into a single stream, thereby overcoming this limitation. Historically, these settings have been configured by an administrator of the MCU and were not typically accessible by users connected to the MCU. However, in accordance with the systems described herein, a menu, such as that illustrated in FIG. 8 may be presented to the user, which allows the user to tell the MCU how many sites he would like to view (based on compositing done by the MCU). As can be seen, increasingly large numbers of sites can be displayed, even on a single monitor, by judicious arrangement in the compositing process.
[0033] In addition to persistently arranging the layouts based on rules like those discussed above, layout rules may also be specified based on the “role” of the stream in a conference. The role may be included as part of an identifier of a stream. Roles may include such items as whether the steam is live people video or content. Additionally, people or content streams may be identified as various different types, such as presenter, active speaker, passive participant, etc. These roles may be permanent, semi-permanent (i.e., unchanging for the duration of a call), or may change during the call.
[0034] As one example, during a CEO presentation or a remote instruction scenario, it might be desirable for the CEO's or teacher's endpoint to claim the “presenter” role so that their video is always displayed to all participants. Additionally content associated with the presenter could receive priority over other streams. Conversely, passive participants in those roles might not be displayed to remote participants. However, during a call if a participant has a question for the presenter, that passive participant stream might be denoted as active speaker so that other participants could see who was asking a question of the nominal presenter. Any number of roles and rules based on those roles can be defined based on the needs of a particular conferencing system.
[0035] In addition to the foregoing, roles (and rules based thereon) can be assigned not just to media streams, but also to monitors. For example, a particular monitor could be assigned a role as the content displaying monitor or as only a people-displaying monitor. One or both of those scenarios might be applicable to a telepresence room, which as dedicated content monitors and in which displaying content on the people monitors might be disruptive to the telepresence experience. Such might not be true in the case of a small group room, in which the monitors of necessity do double duty.
[0036] Additionally, roles (and rules based thereon) might be assigned on an enterprise basis, e.g., the CEO might always have priority in all calls. Alternatively, roles and associated rules might be changeable on a call-to-call basis. In some instances, it may be desirable to present the user with a choice as to whether or not the default enterprise role should be changed for the present call. Additional information on role-based media stream, layout, and conference management can be found in provisional patent application Ser. No. 13/918,226, filed Jun. 14, 2013, entitled “Layout and Presentation Manager for a Videoconferencing Multipoint Control Unit,” which is hereby incorporated by reference in its entirety.
[0037] The data and rules for the layout preferences can be stored in one or more data files that can be created and/or modified by an administrator or by the user. In some embodiments, an administrator can create a default layout preference file (or files) that can be distributed to users and modified by those users, if so desired. In some embodiments, such files can be downloaded, and distributed across multiple systems and multiple platforms. This can allow a user to retrieve his preferences when using new equipment within the organization. If a user can login or check-in to a system, layout preferences can be associated with that user can be automatically retrieved upon said log in or check-in. Future logins or check-ins can automatically retrieve the preferences either from a last used MCU or from some other centralized server.
[0038] The above description is illustrative and not restrictive. Many variations of the invention will become apparent to those skilled in the art upon review of this disclosure. The scope of the invention should therefore be determined not with reference to the above description, but instead with reference to the appended claims along with their full scope of equivalents.
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Disclosed herein are methods, systems, and techniques for creating media conferencing layouts that are intelligent (i.e., based on some underlying principle to enhance user-perceived conference quality) and persistent (i.e., consistent within a call and from one call to the next).
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TECHNICAL FIELD
This invention pertains to enhancing the efficiency of an internal combustion engine by rapid heating of circulating engine oil though preferential circulation of previously-heated oil. Mixing of the previously-heated oil and cold oil in the engine sump is discouraged through the use of a selectively-permeable screen which only promotes mixing when the sump oil attains a preselected viscosity.
BACKGROUND OF THE INVENTION
The text of this background section is to prepare the reader for understanding practices described in this disclosure. The text is not presented with a consideration of whether it discloses prior art.
Multi-cylinder, reciprocating piston, internal combustion engines for automotive vehicles typically contain an oil circulation system for lubrication of valves, cylinder walls, pistons, connecting rods, cranking mechanisms, and the like. Generally, a predetermined quantity of lubricating oil (e.g., four to six quarts) is stored in bucket-like sump container attached to the engine below the cranking mechanism. When the engine is operating, an oil pumping mechanism, often driven off the engine, draws lubrication oil from the sump container and pumps it upwardly over all moving engine parts. The oil is drawn through an oil pick-up or inlet tube positioned below the surface of the sump oil. The oil flows in an oil circulation path, as intended and provided, over engine parts requiring lubrication. As it completes its flow, the oil drains downwardly back into the sump container. Typically, less than half of the stored volume of oil is in circulation at any moment of engine operation. In this way an adequate supply of oil is assured despite irregular motion of the vehicle, or leakage of the oil or burning of some of the oil as it is exposed on cylinder walls.
The oil is heated during engine operation, often to temperatures of about 90° C. to about 110° C. and at this temperature the oil has a viscosity and flow properties well suited for lubrication of engine surfaces. But when engine operation has ceased, the stored and now quiescent oil is cooled to the ambient temperature in which the vehicle is situated. Since this temperature may be well less than about 30° C., temperature-dependent properties of the oil are often less than desired for engine operation. So the oil may be relatively cold and viscous as its circulation is commenced immediately following an engine cold start. Sometimes vehicles intended for cold climates have special oil heaters located in the sump container for keeping the oil at a desired temperature between intermittent usages of the engine. Most vehicles do not have such an oil heater. But there is a need to reheat the circulating oil for better engine operation and less engine wear. A difficulty is that the total volume of oil is considerably larger than the amount being circulated and heated by the engine at any operating moment.
SUMMARY OF THE INVENTION
In accordance with practices of this invention, the oil storage volume in the sump container is divided into two volumes using a separator which may be a thin metal sheet with many small holes or small mesh metal screen member. The size of the small holes in the sheet or the mesh openings in the screen are determined to impede flow-through by a cold viscous oil but to permit passage of the same oil heated for engine operation.
The sheet or screen separator member is shaped, located, and fixed in the sump container to catch and contain circulated, returning engine oil from a started and operating engine and direct it to an oil pick-up in the sump for continued circulation. The cold oil-retaining separator member is also shaped and located to enclose a volume of oil from the total stored oil volume, the enclosed volume lying between the separator and the sump walls and bottom. The circulating oil is drawn from and returned to the free volume defined by the separator. The remaining portion of the oil in the sump container volume is outside the circulated oil volume and contained within the screen member enclosed volume. For example, in a five or six quart oil capacity engine, the circulating volume of oil within the separator defined space may be about one and one-half quarts, or about 25 to 30% of the total oil volume, with the remaining cold oil contained within the enclosed volume.
Thus, immediately following an engine cold-start, a selected portion of the oil from the overall sump container volume is pumped upwardly into the oil circulation paths through the engine, and this volume of circulating oil is drained back into the free storage volume defined within the screen or sheet member. This smaller portion of oil is determined for adequate lubrication of the parts of the engine. But this smaller portion is also more rapidly heated by engine operation from the stored oil's ambient temperature to its preferred operation temperature, somewhat above 90° C.
So, during a period of a few minutes following an engine cold start, the total oil volume within the sump container has been divided by the screen or sheet member into two portions. The smaller free portion contained within an upper and central volume (with respect to the return drain path of the circulated oil) is being heated as it is circulated through the engine. The larger oil volume contained within the sump vessel, but temporarily and partially excluded from circulation by the separator member, is cooler. But the separation of the warming circulating oil from the excluded outer oil volume in the sump container is temporary.
The screen or shell member is formed of a metal or other suitable thermally conductive material so that heat is transferred through the member from the engine heated oil to the temporarily non-circulated oil. Further, the small screen or sheet openings of the separator become less resistant to oil flow as the oil is heated. The screen mesh opening or sheet perforations are sized to permit easy passage of heated oil (e.g., at 60° C. or higher) while slowing and impeding passage of colder oil through the perforations. It is in this way that the perforated sheet or screen member temporarily excludes much of the cold oil from the enclosed volume defined by the shell member. But some circulated and warming oil can enter the enclosed volume as it is returned to the circulating oil volume. As engine operation continues, oil flow through the perforations in the sheet member permits heating of the total oil volume, and the temporarily separated oil volumes are, in effect, recombined by easy flow of heated oil through the perforations in the separator shell member.
Thus, the openings in the screen or sheet are sized to permit a slow flow of relatively cold oil and to permit easy flow of hot oil. As described the function of the screen or perforated sheet is simply to permit the recirculation of a loosely confined portion of the total oil volume to hasten heating of the oil following an engine cold start. But the goal is to continually heat and circulate all of the stored oil during continued engine operation so that the screen or sheet presents only a modest resistance to flow of heated oil. The sheet serves its task mainly following an engine cold-start and reduces the time required to heat some oil to its effective lubricating temperature. Thereafter, during continued engine operation, the rest of the stored oil is heated. But the duration of the cold start period with less effective lubrication is reduced.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 shows, in cross-section, an internal combustion engine schematically illustrating the circulating path followed by the lubricating oil.
FIG. 2 shows, in sectional view, a schematic representation of oil flow in a portion of a schematic, but representative engine oil sump with an associated oil intake. The oil in the sump is partitioned into two volumes by a temperature-sensitive separator, and the oil flow shown is representative of the initial oil flow expected during practice of the invention immediately after a cold engine start when the oil is at a temperature of less than about 60° C.
FIG. 3 shows a representation of the oil flow in the engine oil sump portion of FIG. 2 after some period of engine operation during which one of the oil volumes has attained a temperature of greater than 60° C. while the bulk of the second oil volume remains at a temperature of below about 60° C.
FIG. 4 shows a representation of the oil flow in the engine oil sump portion of FIGS. 2 and 3 after both oil volumes have attained a temperature of greater than about 60° C.
FIGS. 5A and 5B show two exemplary separators. FIG. 5A shows a perspective view of a portion of a sheet separator incorporating a plurality of openings; FIG. 5B shows a woven mesh separator. Both separators are suited to prevent or restricting passage of lubricating oil at a temperature of less than about 60 20 C. while allowing passage of lubricating oil at temperatures of greater than 60° C.
FIGS. 6A-C show, in cross-section, several orifice configurations and indicate the difference in flow capacity of these orifice configurations.
FIG. 7 shows a representative curve showing the difference between the circulating oil temperature in an engine adapted for practice of the invention and a conventional engine with a conventional sump after a cold start. The result illustrates the increase in oil temperature and hence the reduction in viscosity and associated fuel economy enhancement obtainable through practice of the invention.
DESCRIPTION OF PREFERRED EMBODIMENTS
Lubricating oils in internal combustion engines, in common with most liquids, become less viscous as their temperature increases. Although such oils commonly include, as part of a more extensive additive package, a viscosity modifier, this will only reduce, not eliminate, the extent of the viscosity reduction. Hence an oil formulated to develop an appropriate viscosity for effective lubrication at normal engine operating temperatures of 90-110° C. or so will exhibit a higher viscosity as the engine, and its lubricating oil, is warming to its steady-state operating temperature after a cold start. This higher viscosity results in increased friction and reduced vehicle fuel economy during the 800-1200 seconds or so required for the engine to reach its operating temperature. It is an object of this invention to mitigate the negative impact of cold starts on vehicle fuel economy.
FIG. 1 shows, in schematic cross-section, an engine 5 suitable for use in a motor vehicle. Oil 11 is stored in sump 10 for delivery to the engine. Oil is withdrawn from sump 10 at oil pick-up 14 under the urging of oil pump 15 and flows as flow 22 through tube 18 to filter 17 . After passing through filter 17 the oil is distributed under pressure by an appropriate arrangement of channels and orifices to all regions of the engine requiring lubrication. These lubricated elements include rocker arm 13 and the valve system located at the topmost location of the engine as well as bearings 19 , 21 and 23 . After performing its lubrication function the oil returns to sump 10 as droplets 24 under the influence of gravity.
An exemplary embodiment of the invention is shown in FIG. 2 which is a schematic sectional view of a portion of a sump 10 of an internal combustion engine like that shown in FIG. 1 , showing the oil pick-up 14 contained within oil pan 12 . Oil fills the oil pan 12 to a predetermined level 16 and oil entering oil pick-up 14 is conveyed to the engine through tube 18 by an oil pump (not shown). Oil flow within the sump is shown by arrows 20 and the aggregated oil flow within tube 18 by arrows 22 . Heated oil which has previously passed through the engine and is returning, under the action of gravity to sump 10 is shown as droplets 24 . Individual droplets may also deposit on some of the unseen sump surfaces and consolidate into flow 26 directed into the oil pan.
In an embodiment the oil in oil pan 12 is sequestered into two layers 28 and 30 by separator 32 . Separator 32 is a generally planar and horizontally mounted below the oil surface indicated by oil level 16 . Separator 32 has an opening surrounding oil pick-up 14 allowing upper oil layer 30 free access to pick-up 14 . The opening is bounded by a downwardly extending flange 40 extending to inner bottom surface 36 of oil pan 12 . It is intended that separator 32 seal against the surfaces of oil pan 12 wherever the perimeter edges or flange edges of the separator contact the oil pan to prevent passage of oil from one volume to the other at the oil pan interior surfaces. Lower oil layer 28 is contained between the inner surface 34 of separator 32 and the inner bottom surface 36 and the sidewalls 38 of oil pan 12 . It will be appreciated that the respective volumes of upper oil layer 30 and lower oil layer 28 may not be readily estimated from this figure since the lateral extent of the oil pan, shown in the section, is much less than its longitudinal extent. Thus the volume of oil accessible to oil pick-up 14 is disproportionately emphasized in lateral section.
Separator 32 comprises a plurality of openings in a thin sheet or a fine mesh screen. Commonly such a sheet would be metal, but any material which may be fabricated as a thin sheet and not react with hot oil or any of the fuel or water-based or other impurities in the oil pan would be suitable. However it is preferred that the separator possess good thermal conductivity to promote heat flow from heated oil on one side of the separator to colder oil on the other side. Thus metallic separators may be commonly used. Such separators may be fabricated of those metals and alloys, optionally coated, currently in use for oil pans since these have clearly demonstrated durability in an engine oil environment.
An exemplary arrangement of orifices in a sheet is shown in FIG. 5A . Commonly such orifices may be circular in plan view as shown, but alternate geometries, such as ovals, slits or regular or irregular polygons may be employed provided at least one dimension of the orifice does not exceed a characteristic dimension. The characteristic dimension is selected so that the orifices severely impede the flow of higher viscosity oil, that is oil at a temperature of about 60° C. or less, but enable flow of the same oil at a temperature of greater than about 60° C. or so when it is in a lower viscosity state. The particular characteristic dimension will vary with the particular lubricating oil but will generally range from about 100-300 micrometers. An exemplary polygonal opening will generally obtain in woven wire mesh separators such as that shown in FIG. 5B in which openings 76 of dimension ‘d’ are defined by the spacings between arrays of interwoven arrays of orthogonal wires 72 , 74 . Opening shapes other than the generally square openings shown in FIG. 5B may be developed under more complex weaves.
Referring to FIG. 5A it will be noted that orifices 60 , only some of which are shown extending through sheet 62 for clarity, are arranged in a hexagonal arrangement highlighted at 64 . This particular arrangement enables close packing but it is intended to be illustrative rather than limiting and other arrangements of the orifices may be used without limitation. The orifices are shown as spaced apart to avoid unduly weakening supporting sheet 62 . As shown the orifices may be spaced apart by a distance ‘d’ substantially equal to the diameter ‘d’ of the orifices but other suitable spacings may also be used.
The area density of orifices should be sufficient to enable an oil flow rate substantially equal to or greater than the oil flow rate through the engine. As an example, an array of orifices 200 micrometers in diameter arranged as shown in FIG. 5A on a separator with an area of 100 square inches or so, may pass up to about 30 gallons per minute under a 1 inch head. This flow rate is sufficient for a high performance V8 engine for a sports car. The more open weave mesh of FIG. 5B enables yet greater flow.
The flow characteristics of the interface may be enhanced by shaping the exit geometry of the orifice. The calculated results referred to above were representative of the orifice of FIG. 6A , that is an orifice in a very thin sheet of thickness (indicated as ‘t’ in FIG. 5A ) of less than one quarter of the orifice diameter. For the 200 micrometer orifice discussed above this would imply that the sheet be a foil of 50 micrometers or so. Such a foil may require that it be mounted on a frame or similar support structure to support the loads which might be applied to it, for example by sloshing oil on cornering or abruptly stopping the vehicle. It may be noted that use of this thin foil exacts a flow performance penalty of about 25% over the use of the thicker sheet shown in FIG. 6B .
Increasing the sheet thickness to between two and three times the orifice dimension as shown in FIG. 6B enables, for a two hundred micron orifice, a sheet thickness of between 0.2 and 0.3 millimeters enabling the sheet to be self-supporting eliminating and eliminating any need for a frame or support structure. As noted, the thicker sheet enables greater fluid flow than the thinner sheet. While such theory is not relied on it appears that the extended channel length may result in a more organized flow pattern and induce less backpressure.
Yet further modification of the orifice, while maintaining the same exit diameter, is shown in FIG. 6C . Again the orifice extends to between two and three times the orifice dimension, but, in addition, the orifice inlet is tapered, resulting in a smoother flow transition and a further increase in flow by about 18% over the straight-sided orifice of FIG. 6B . For ease of manufacture, preferably the tapered geometry of FIG. 6C is developed on a foil, as in FIG. 6A , again raising the issues of the mechanical stability of the foil under applied loads. Also, as will become apparent in consideration of the oil flow paths the direction in which the flared section extends from the sheet may need to be modified consistent with the anticipated oil flow paths.
The straight-sided orifices of FIGS. 6A and 6B may be made by drilling using conventional microdrills or by spark machining or laser drilling. The orifice geometry of FIG. 6C may be developed by piercing and flaring using a tapered point cylindrical punch which will, when the point penetrates the sheet, flare the surrounding material provided the sheet's ductility is sufficient to resist flange cracking
The influence of separator 32 on the oil flow paths in the oil pan 12 may be appreciated by consideration of FIGS. 2, 3 and 4 which are illustrative of the evolution in oil flow path as the engine, after a cold start, progressively heats up to its operating temperature.
As illustrated in FIG. 2 , immediately after cold start up, the oil of lower oil layer 28 , at a temperature of less that 60° C. is initially prevented from accessing oil pick-up 14 by separator 32 . Oil pick-up 14 therefore draws oil substantially exclusively from upper layer oil 30 conveying it to the engine (not shown) as aggregated flow 22 under the urging of an oil pump (not shown). The oil, now heated after its passage though the engine, returns to the sump as droplets 24 and consolidated flow 26 . The oil of upper oil layer 30 , though warmed by the engine-heated returning oil remains below 60° C. and so substantially cannot pass through separator 32 . Oil in upper oil layer 30 therefore flows parallel to the surface of separator 32 as indicated by arrows 20 and returns to oil pick-up 14 without significantly mixing with the oil of lower oil layer 28 . The individual oil flows 20 , on converging at the oil pick-up 14 are aggregated into oil flow 22 and conveyed into engine.
FIG. 3 is illustrative of the oil flow at a later stage in the engine warm-up. The oil of the upper oil layer 30 upper layer continually heated by returning heated returning oil droplets 24 and returning consolidated oil flow 26 achieves a temperature of about 60° C. or so at which it may pass through separator 32 . However, because of its lower density than the cooler oil of lower oil layer 28 , the preponderance of flow is still parallel to separator 32 as indicated by arrows 20 . But passage of heated oil flow 20 serves to warm separator 32 and elevate the temperature of some volume of the oil of lower oil layer 30 in contact with inner surface 34 of the separator. When the temperature of the volume of oil in contact with inner surface 34 is sufficient to enable flow through separator 32 some volume of oil from lower oil layer 28 may pass though separator 32 as flow 120 to merge and mingle with flow 20 as it merges into aggregated flow 22 . The volume of oil corresponding to flow 120 may be replaced by leakage of some oil from the upper oil layer into lower oil volume 28 via flow 20 ′. Continued engine operation will further elevate the temperature of the oil of upper oil layer 30 and promote further heating of, and flow into and out of lower oil volume 28 .
When all oil, in both the upper and lower oil layers, achieves a temperature above about 60° C. or so, rendering separator 32 fully permeable to all of the oil, the flow will be as shown in FIG. 4 . Flow 20 in upper oil layer 30 will continue but the volume of flow 20 ′ from the upper oil layer 30 to lower oil layer 28 and the volume of flow 120 from the lower oil layer to the upper oil layer will both increase, promoting full circulation and engaging all the oil in the sump.
The effectiveness of this approach is shown in FIG. 7 , a representative curve illustrating the difference in oil temperature with time after cold start resulting from practice of this invention. The curve shows the difference in circulating oil temperature recorded for an engine with an oil pan containing a separator as described and an engine with a conventional oil pan without a separator. In both cases the oil attains its normal operating temperature about 800-1000 seconds after cold start, leading to a temperature differential of substantially zero. But the engine with the separator enables a rise in circulating oil temperature during the warmup period. The temperature difference rise develops immediately after start-up and increases rapidly to a maximum value of about 10-12° C. at about 200 seconds or so after engine start, before starting to decline as the circulating oil in both engines progresses to its steady-state normal operating temperature after about 800-1000 seconds or so.
The relative partitioning of the total oil volume may depend on the specifics of a particular engine but the volume should be informed by the need to not starve the engine of oil during warm-up, particularly during the first 10-20 seconds after start-up. During this initial period the gravitational return flow of the still-cool, viscous oil to the sump may be delayed resulting in an initial circulating oil volume which is greater than would occur at steady-state.
The volume of oil participating in engine lubrication should also be informed by its ability to temporarily accept and hold contaminants, such as water and unburned fuel, from the combustion chamber, which blow by the piston rings. Such contaminants may exist as vapors in a hot engine and be eliminated by the positive crankcase ventilation system of the engine. In cold engine and during warm-up they will condense and temporarily dissolve and be dispersed in the cold oil. Thus another constraint on the oil volume partition effected by the separator is that the circulating oil volume be sufficient to accommodate the oil contaminants produced on cold start without prejudicing its lubricating properties. All of these requirements may be met if the sump is so partitioned as to enable an initial circulating oil flow of at least one and one-half quarts. This will correspond to about 25 to 30% of the total oil volume in a conventional engine whose normal oil requirement is for five or six quarts.
While preferred embodiments of the invention have been described as illustrations, these illustrations are not intended to limit the scope of the invention.
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The volume of lubricating oil stored in the sump of an internal combustion engine for a vehicle is in significant excess of the volume of oil circulating through the engine at any one time. The circulating oil, drawn from the sump, may be rapidly heated during its passage through the engine, but the excess volume remaining in the sump dilutes and cools the circulating oil as it returns to the sump. By separating the oil volume into a portion which is circulated through the engine and a second portion which has only limited opportunity to mix with and cool the circulating oil the circulating oil may attain its operating temperature more rapidly. Once the stored volume of oil in the engine has also reached its operating temperature the circulating oil and stored oil may be recombined.
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CROSS REFERENCE
This application is a continuation of U.S. application Ser. No. 08/880,099, filed Jun. 20, 1997, now U.S. Pat. No. 5,976,565.
TECHNICAL FIELD
A delivery device in the form of patch, and method of its manufacture, is provided for the topical treatment of acne and acneiform diseases.
BACKGROUND ART
Acne afflicts 90% of all teenagers but also men and women in their twenties or thirties or may persist throughout adulthood. The process by which acne develops has been described in “New Approaches to Acne Treatment” by W. J. Cunliffe, ed. Martin Dunitz, London, 1989.
Acne vulgaris is a chronic disorder of the pilosebaceous follicles (apparatus) characterized by comedones (blackheads), papules, pustules, cysts, nodules, and often scars, that appear on the most visible areas of the skin particularly on the face, chest, back and occasionally neck, and upper arms.
The pilosebaceous apparatus is largely under the control of endogenous hormones (mainly androgens) which are present in unusually high concentrations in the blood during adolescence and puberty giving rise to an excessive production of sebum. The condition may worsen by a simultaneous increase in the rate of keratinization of the skin's horny layer (the stratum corneum). As the horny cells proliferate, they can form an occlusive plug or comedone which coupled with the increased production of the sebum, represents an ideal medium for the proliferation of the skin resident strains, such as the Gram positive anaerobic bacterium, Propionibacterium acnes.
Eventually, the plugged follicles rupture and allow the discharge of their contents causing local swelling and inflammation. The exposed follicles may darken from the deposition of pigment from damaged cells in the deeper layer of skin.
Acne is a multistage condition and in most severe form leads to hospitalization of the patient and extensive discomfort with long term scarring of the skin. There is a need for improved treatments for acne that will effectively prevent the condition developing to its most severe form and that can be used by majority of the sufferers without adverse effects.
At this time there are numerous treatments available for treating acne but each treatment has unfortunate limitations which it would be desirable to overcome. In most part, treatment of acne is by topical formulations in the form of creams, gels, emulsions or lotions which contain selected agents. These agents include hormones or hormone agonists and antagonists (EP A1 0 563 813 and U.S. Pat. No. 5,439,923), antimicrobial agents (U.S. Pat. No. 4,446,145, GB 2,088,717, GB 2,090,135, GB 1,054,124, U.S. Pat. No. 5,409,917), salicylic acid (U.S. Pat. No. 4,514,385, U.S. Pat. No. 4,355,028, EP A1 0 052 705, FR-A 2,581,542, and FR-A 2,607,498). The problems associated with topical treatment of acne with creams, gels, emulsions and lotions include the lack of precision of application and associated lack of control over precise dose at the target site. Application of a cream, gel, emulsion or lotion results in exposure of an area considerably in excess of that covered by lesion thereby exposing normal healthy skin to the anti-acne formulation. For example salicylic acid is an irritant to normal skin over prolonged exposure and particularly in high concentrations.
Oral administration of anti-acne agents is currently provided for severe cases of acne. These are reviewed in “Acne, A Review of Optimum Treatment” by Sykes N. I. and Webster G. F in Drugs 48, 59-70 (1994). Numerous side effects have been described using oral administration of anti-acne drugs. For example, isotretinoin which is a derivative of vitamin A has associated risks of teratogenicity and may be a risk for women of childbearing age. Oral administration of antibiotics suited for treating acne, may induce the appearance of adverse effects which include abdominal cramps, black tongue, cough, diarrhea, fatigue, irritation of the mouth and other undesirable symptoms.
Salicylic acid in the form of a tacky hydrophilic gel dressing (U.S. Pat. No. 5,258,421) and in combination with pantothenic acid or pantothenic acid derivative in a cleansing pad (PCT WO 93/21899) has been used for treating acne.
In addition, a patch containing cephalosporin has been described in the U.S. Pat. No. 5,409,917 for the treatment of acne using a method for making nicotine patches. Since the patch was not optimized for the special circumstances associated with acne including optimizing the anti-acne agent content and placement of the patch at multiple locations on exposed skin such as the face, the patch has not been adopted as an anti-acne formulation delivery modality.
There is a need therefore for methods and devices for treating patients with acne that have minimum adverse effects, have maximum efficacy and may be simple and comfortable to use.
OBJECTIVES OF INVENTION
The present invention addresses the need for treating acne and acneiform diseases so as to minimize adverse effects and to maximize efficacy of treatment. The present invention is directed to a topical delivery device, in the form of a patch, having a size and thickness suited for prolonged delivery of an anti-acne formulation at a selected site characterized as acneiform. The patch contains at least two agents suited for treating acne.
In a preferred embodiment, a patch is provided for topical application of an anti-acne formulation that includes a backing film, a release layer and a polymeric matrix located between the backing film and the release layer for containing the anti-acne formulation. The formulation includes an effective amount of at least two agents selected from the group consisting of an anti-microbial, an antiseptic, an anti-irritant and an acne therapeutic agent.
In a further embodiment, the acne therapeutic agent is selected from at least one of the group consisting of a keratolytic agent, a hormone, a hormone agonist, and a hormone antagonist.
In a further embodiment of the invention, a method for manufacturing a delivery device for treating acne is provided that includes mixing a single adhesive or a mixture of adhesives and at least one of a keratolytic agent, an antiseptic, an anti-irritant, and a solubilizer so as to form a blend; and laminating the blend on a first side with a release liner and on a second side with a backing film.
In a further embodiment of the invention, a device in the form of a patch for the topical application of an anti-acne formulation is provided that includes a synthetic pressure-sensitive adhesive used as a carrier or polymeric matrix or associated with a carrier or polymeric matrix, said carrier having the anti-acne formulation uniformly distributed therein, characterized in that said anti-acne formulation comprises effective amounts of at least two active ingredients from at least two different groups of active ingredients and in that said at least two different groups are selected from the group comprising keratolytic agents, anti-irritant agents, antiseptic agents,antimicrobial agents, hormones, hormone˜agonists, hormone-antagonists and other agents suitable for treating acne.
In another embodiment, a patch for the treatment of acne and acneiform skin diseases includes topically acceptable carriers for topical application, such as acrylics, paper, silicones, cellulosics, moisturizers; antioxidants; and stabilizers; wherein the patch is capable of delivering an effective amount of anti-acne agents to acneiform skin to be treated (i.e. comedones, pustules, papules).
In a further embodiment of the invention, the patch of the invention is capable of prolonged delivery of the formulation, the time range being greater than 4 hours, preferably at least 24 hours, more preferably 80 hours.
In a preferred embodiment of the invention, the patch has a thickness in the range of 0.5 to 2 cm 2 and a thickness in the range of 7 to 24 mils (about 178 to 610 μm)
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a side view of a three layered patch for delivering agents for the treatment of acneiform diseases.
FIG. 2 a is a side view of a four layered patch for delivering agents for the treatment of acneiform diseases.
FIG. 2 b is a top view of the same patch as in FIG. 2 a.
FIG. 3 shows the stability of the patch of the invention as for salicylic acid and triclosan.
FIG. 4 a shows the flux of salicylic acid through human stratum comeum as concerns two patches according to the invention and a gel.
FIG. 4 b is an enlargement of FIG. 4 a as concerns the two Patches of the invention
DESCRIPTION OF THE INVENTION
The term “automically acceptable carriers”, as used herein, means substances substantially lacking toxicity for human tissues.
The term “topical application”, as used herein, means directly laying on outer skin.
The term “stable”, as used in the specification is defined as possessing a shelf-life that extends for more than several weeks.
The term “effective amount”, as used herein, means an amount sufficient to provide an anti-acne effect.
The present invention provides methods and devices for treating patients affected by acne, where the device has been optimized for minimizing adverse effects and for maximizing efficacy and is simple and comfortable to use. The topical treatment of acne and acneiform diseases disclosed herein utilizes a patch to achieve local anti-acne effects that result from the suppression of the proliferation of horny cells and microbes involved in the pathogenicity of acne and reduction in associated inflammation. The patch has been designed so as to effectively deliver anti-acne agents to the stratum corneum (the outermost layer of epidermis, exposed to external environment) and subsequently to penetrate into the pilosebaceous unit (in the dermis) where the acneiform condition originates, while having very limited penetration into the systemic circulation. This is demonstrated by the skin flux permeation study (Example 12 hereafter), which indicates that the amount of salicylic acid that crosses stratum corneum is very small as compared to that of the gel formulation containing 2% of salicylic acid.
In order to ensure that the patch is simple and comfortable to use, a suitable size and thickness of a single patch has been identified. The patch proposed in this invention can be produced in a variety of sizes dependent on the area to be treated (i.e. comedones, papules, pustules). The size of the patch is classified as small being 0.5 to 2 cm 2 and large patch up to 40 cm 2 . Typically, the size of the patch is from 0.5 to 1.3 cm 2 and preferably 0.8 cm 2 .
The patch of the invention is stable and is capable of safe and effective delivery of the anti-acne formulation. For example, the stored patch containing anti-acne agent may remain effective up to two years such that any chemical changes that may occur during storage, but before the predetermined expiration date, are believed to be non-harmful.
An example of the patch suitable for treating acne is described in FIG. 1 . In this embodiment, the patch may include a backing film layer 1 , a single synthetic pressure-sensitive adhesive layer 2 and a release liner 3 with the anti-acne formulation contained within the synthetic pressure-sensitive adhesive layer.
In other embodiments, more than one matrix may be positioned between the release liner and the backing layer (see FIGS. 2 a and 2 b ). According to FIGS. 2 a and 2 b and Example 4, a patch is described that includes a backing film layer 1 , a synthetic pressure-sensitive peripheral adhesive layer 4 , a paper matrix 5 , and a release liner 3 . The patch may have a paper matrix diameter of ⅝″ (inches) (about 1.6 cm) and/or a peripheral adhesive layer diameter of ⅞″ (about 2.2 cm).
The backing film layer 1 may be made of plastic or fabric or woven or non-woven materials, porous or occlusive. Porous materials are sometimes used since some of the slain resident strains of the bacteria in the pilosebaceous unit are anaerobic.
The backing film layer can be made of any suitable material such as paper; cellophane; plastic films such as polyethylene, polyester, polyurethane, polyvinyl chloride and polyamide; fabrics and metallic foils, which are impermeable and non-reacting with the anti-acne formulation distributed in the adhesive polymeric matrix. The backing film can be composite or transparent or opaque or fleshtoned or aluminized or a combination thereof, with thickness ranging from 1 to 5 mils (about 25 to 110 μm), typically from 2 to 3.5 mile (about 50 to 90 μm) and preferably 3 mils (about 76 μm), and can be formed from any of CoTran™9720 (3M), Saranex®(Dow Chemicals), Multilam fleshtoned polyester film 1009 (3M), or any other material recognized in the art as having the desired properties.
The patch has an adhesive polymeric matrix 2 , which is adjacent to the backing layer and may be made of synthetic adhesives such as acrylics, rubber, silicone, cellulosics, paper or other suitable materials that may have pressure sensitive properties and adhere to the skin directly or through a peripheral adhesive. The adhesive polymeric matrix consists of at least one layer of the adhesive-containing substances and/or other additives. The adhesive polymeric matrix may be composed of more than one layer, but is preferably composed of one layer. The thickness of this adhesive polymeric matrix is in the range of 0.5-30 mils (about 13-760 μm), typically of 0.5-6 mils (13-152 μm), preferably 0.5-2.5 mils (about 13-64 μm) and more preferably 2.5 mils (about 64 μm). Contained within the adhesive polymeric matrix are a mixture of anti-acne agents including any of keratolytics, anti-irritants, antiseptics, antimicrobials, hormones, hormone-agonists, hormone-antagonists and other agents suitable for treating acne, preferably together with solubilizers.
The adhesive polymeric matrix can be made of inert materials which are further biologically and topically acceptable and compatible with the distributed active substances described above.
Preferably, topically acceptable polymers with adhesion properties may be acrylic-based polymers such as the GELVA® series sold by Monsanto and the DURO-TAK® series sold by National Starch; rubber-based polymers such as DURO-TAK® series sold by National Starch; and silicone-based polymers such as BIO-PSA X7-4302 SILICONE PSA sold by Dow Corning.
The said adhesive polymeric matrix can also be made of paper materials, preferably Whatman filter paper, which is adhered onto the skin through a peripheral adhesive layer. The thickness of such an adhesive polymeric matrix is usually 7 mils (about 178 μm).
A release liner 3 , is placed against the surface of the adhesive polymeric matrix on the surface opposite to the backing layer. The release liner can be made of materials impermeable to any substance dissolved in the said matrix, which is easily stripped off or released prior to the use. The release liner can be made of materials such as polyvinyl chloride, polyester, polyvinylidene chloride, polystyrene, polyethylene, paper etc. coated or not with an adhesive, but preferably with an easy release silicon formulation.
Preferably the release liner is made of a natural, high impact polystyrene film (grade code: 10106 or 15462) sold by REXAM Release or a siliconized polyester film sold by REXAM Release. The thickness of the release liner can range from 3 to 10 mils (about 76 to 250 μm), or preferably be 10 mils (about 250 μm).
Preferably, the patch has a size in the range of 0.5 to 2 cm 2 and a thickness in the range of 7 to 24 mils (about 178 to 610 μm).
In an embodiment of the invention, a combination of anti-acne agents has been selected to treat acne. These agents include a keratolytic agent, such as salicylic acid, in conjunction with an anti-irritant, an antiseptic, an antimicrobial agent and/or other acne fighting compounds such as for example urea, allantoin, hydroxyquinoline compounds, for delivery via a patch directly to the area to be treated. The presence of an anti-irritant counteracts the local irritation associated with the application of keratolytics to the skin. The antiseptic limits the growth of organisms which cause the acne. Furthermore, the antimicrobial may enhance the overall anti-acne properties of the compositions in moderate or severe stages of the disease. The use of a solubilizer ensures that the active agents in the patch are in form suited for diffusion from the patch to the skin.
Antimicrobials typically used for topical application can be penicillins, cephalosporins, other beta-lactam compounds, aminoglycosides, tetracyclines, erythromycin, antifungal agents, etc. and a combination thereof. Preferably, antimicrobial agents used for topical application onto acneiform skin are erythromycin, tetracycline, clindamycin, cephalosporin.
Antiseptics typically used for topical application onto acneiform skin are triclosan (Irgasan DP 300), phenoxy isopropanol, resorcinol, chlorhexidine, povidone and iodine.
Keratolytic agents typically used for topical application onto acneiform skin are salicylic acid, benzoyl peroxide, sulphur, retinoic acid and any of a number of fruit acids and alpha hydoxy acids.
Anti-irritants typically used for the topical application onto acneiform skin are α-bisabolol, farnesol, chamomile extract and glycyrrhetinic acid.
Solubilizers used in the anti-acne formulation of the present invention include any of glycerol, propylene glycol, polyalcohols, sorbitol and sorbitol derivatives, preferably sorbitan monooleate.
Compositions of the present invention can also comprise other topically acceptable agents such as solvents, antioxidants, moisturizers etc.
According to a preferred embodiment, the invention provides a device as described above, which comprises, related to the total weight of the carrier and the formulation:
one or more keratolytic agent(s), each in an amount of 0.1 to 10.0% w/w, preferably of 0.1 to 2.0% w/w and more preferably of 0.6% w/w;
one or more anti-irritant agent(s), each in an amount of 0.01 to 5.0% w/w, preferably of 0.01 to 3.0% w/w and more preferably of 1.0% w/w;
one or more antiseptic agent(s), each in an amount of 0.05 to 2.0% w/w, preferably of 0.1 to 1.0% w/w and more preferably of 0.3% w/w; and
one or more solubilizer(s), each in an amount of 0.1 to 5% w/w, preferably of 1 to 3.0% w/w and more preferably of 2% w/w.
This invention is further illustrated by the examples. Examples are not to be construed as being a limitation on the scope of invention, which scope is defined by the appended claims. The examples are conducted using salicylic acid, as keratolytic agent, in an amount of 0.1 to 2% w/w together with an anti-irritant such as α-bisabolol in 0.01 to 3% w/w, an antiseptic such as triclosan (Irgasan DP 300) in 0.1 to 1% w/w and a solubilizer such as sorbitan monooleate in 0.1 to 5% w/w, having all of them dispensed in a variety of adhesive polymeric matrices. Controlled delivery is achieved over a period of at least 4 hours, preferably over a period of at least 24 hours and more preferably over a period of at least 8 hours.
EXAMPLE No. 1
Preparation of Polymeric Matrix and Delivery Device in the Form of Patch
A composition of the adhesive polymeric matrix used in the preparation of a patch for the topical treatment of acne and acneiform skin diseases contains salicylic acid as keratolytic agent as described in Table 1.
TABLE 1
Composition of the single adhesive delivery system
QUANTITY
COMPONENT
% w/w (on a dry basis)
α-Bisabolol 1
1.0
Irgasan DP 300 2
0.3
Salicylic acid
0.6
Sorbitan
2.0
Monooleate
Gelva ® 737
96.1
1 α-Bisabolol is 6-methyl-2-(4-methyl-3-cyclohexen-1-yl)-5-hepten-2-ol
2 Irgasan DP 300 is 2,4,4′-trichloro-2′-hydroxy diphenyl ether
A method for producing the patch having the above composition is as follows:
Salicylic acid (0.6 g), Irgasan DP 300 (0.3 g), α-bisabolol (1.0 g), sorbitan monooleate (2.0 g) are added to 293.88 g of Gelva® 737 multi polymer resin solution (total solids content of about 32.7%), and the mixture is stirred at ambient temperature until all the ingredients have dissolved. The mixture is allowed to stand for several minutes so as to remove air bubbles.
The adhesive mixture was formulated into a patch system as follows:
Using an appropriate coating device (square tool steel Multi Clearance Applicator, sold by BYK Gardner) with a 5 or 10 mil (about 130-250 μm) casting gap, a layer of adhesive mixture was coated onto a siliconized polyester film and dried in an oven at 76-78° C. for 15-18 minutes. A breathable polyurethane film (Bertek Medfilm 390) was then laminated onto the adhesive film. The system was then delaminated and further laminated on an easy release silicon polystyrene film (REXAM Release). The final thickness of the dried polymeric matrix was, then, 3 to 5 mils (about 76-130 μm).
The multi-layer laminate was then cut to form a patch of circular shape with nominal size of 1 cm 2 (actual size of 0.8 cm 2 ) and thickness of 7 to 18 mils (about 178-457 μm).
EXAMPLE No. 2
Preparation of Adhesive Polymeric Matrix
The procedure of Example 1 is repeated to prepare the adhesive polymeric matrix. The adhesive used in this example is the acrylic-based polymer GELVA® 788. The patch, thus produced, finally has a circular shape of 1 cm 2 and thickness of 8 to 24 mils (about 203-610 μm).
EXAMPLE No. 3
Preparation of Adhesive Polymeric Matrix Containing a Mixture of Adhesives
The composition of the adhesive polymeric matrix described in this Example, in the specified amounts, is presented in Table 2:
TABLE 2
Composition of the mixed adhesive delivery system
QUANTITY
COMPONENT
% w/w (on a dry basis)
α- Bisabolol
1.0
Irgasan DP 300
0.3
Salicylic acid
0.6
Sorbitan Monooleate
2.0
Duro-Tak ® 87-2287:
96.1
Duro-Tak ® 87-2353
(1:9 ratio by weight
in dry coating)
A homogeneous mixture is obtained by mixing 18.95 g of Duro-Tak® 87-2287 acrylic solution (total solids content of about 50.7%) and 238.92 g of Duro-Tak® 87-2353 acrylic solution (total solids content of about 36.2%). To this mixture of adhesives, salicylic acid (0.6 g), α-bisabolol (1.0 g), Irgasan DP 300 (0.3 g), sorbitan monooleate (2.0 g) are added and the mixture is stirred at ambient temperature until all the ingredients are dissolved. The mixture is, then, kept aside for several minutes to have the air bubbles completely removed.
The adhesive mixture is formulated into a patch system as follows:
Using an appropriate coating device with a 5 mil (about 130 μm) applicator gap, a layer of adhesive mixture is coated onto a siliconized polyester film. The coating is left to dry in an oven at 80° C. for 17 minutes and then laminated using an occlusive polyethylene film.
The process ends with cutting the multi-layer laminate to a patch of circular shape, size of 1 cm 2 , and thickness of 7.5 to 20 mils (about 190-500 μm) which is finally pouched in a flexible, pouching laminate film composed of paper, low density polyethylene, aluminium and Surlyn®.
EXAMPLE No. 4
Preparation of a Delivery Device in the Form of Patch Containing a Plain Adhesive Layer and a Polymeric Matrix with and without Adhesive Properties
In this Example, substances such as antimicrobials, antiseptics, keratolytics, anti-irritants and solubilizers are distributed in a polymeric matrix in which the polymers may or may not have adhesive properties.
The procedure of preparing this patch is presented as follows:
To 10 g ethanol AR, salicylic acid (0.1 g), α-bisabolol (0.1 g), Irgasan DP 300 (0.03 g) and sorbitan monooleate (0.2 g) are added and the mixture is stirred until all the ingredients are dissolved.
Pieces of Whatman filter paper are impregnated with 3 ml of the above ethanolic solution and left to drain at ambient temperature. The impregnated paper pieces are, then, dried in an oven at 40° C. for 5 minutes and finally cut into a desirable size and shape (i.e. circular shape of ⅝″ diameter or area of 5 cm 2 ).
Siliconized polyester films are coated with a plain, acrylic-based adhesive such as Duro-Tak® 87-2287 or Duro-Tak® 87-2353. The bilayer system is dried in an oven at 78-80° C. for 15 minutes and, then, laminated with a polyethylene film such as CoTrant™ 9720. The whole system is cut into a desirable size and shape (i.e. circular shape of ⅞″ diameter or area of 7 cm 2 ).
The polyester film is removed and, onto exposed laminate, the impregnated paper is placed in a co-centric order. Finally the multi-layer system is coated on a polystyrene film, which can be scored on the backside (see FIGS. 2 a and 2 b ).
EXAMPLE No. 5
Preparation of a Delivery Device in the Form of Patch as in Example No. 4 Containing an Additional Adhesive Layer
The procedure of Example 4 is repeated to prepare a patch, in which the exposed laminate is coated on a polystyrene film coated completely or partially with a plain adhesive.
EXAMPLE No. 6
Stability of the Produced Patch
The patch proposed in the present invention will remain stable for two years. Methods such as composite assay for salicylic acid and physical tests (such as 90° dynamic adhesive strength peel test for matrix patch from stainless steel plate as in “Test Methods for Pressure Sensitive Adhesive Tape” developed by The Technical Committee of the Pressure Sensitive Tape Council, 11th Edition) are used to determine its stability over this time.
Furthermore the stability of the proposed patch was examined under ambient conditions. The results expressed as % amount of salicylic acid and triclosan detected in the patch over the time are presented in FIG. 3 .
EXAMPLE No. 7
Patch Depletion Analysis
The patch produced is designed to release its content at 4, 6, 10, and up to 24 hours after application. To determine the rate and extent of the release for salicylic acid from the patch, a patch depletion analysis is performed.
EXAMPLE No. 8
Primary Dermal Irritation Study
A Primary Dermal Irritation Study, in compliance with the FDA Requirements per 21 CFR 58, was performed using patches containing salicylic acid, as disclosed in preferred embodiments, in order to identify the potential irritation or corrosive effects that result from the exposure of rabbit skin to the test material.
The fur of six healthy New Zealand rabbits was clipped as close to the skin as possible at the test site twenty-four hours prior to the application of the test material.
The test material was applied to both intact and abraded skin, and each test area was covered with an 1 inch square gauze patch held in place with non-irritating tape. The skin exposed to the test material for a period of twenty-four hours and examinations of the animals for signs of erythema, edema, and any lesions or other toxic effects were made at thirty to sixty min after patch removal and, then, at seventy-two hours.
The study showed that the patches produced a very slight erythema with some flaking skin at some test sites but no edema. In addition, no other toxic effects were observed during the study.
The Primary Irritation Score as estimated was 0.54 which indicates that the test material is not considered to be a primary skin irritant as defined in 16 CFR 1500.3 (c) (4).
EXAMPLE No. 9
Delayed Contact Hypersensitivity Test—Modified Buehler Sensitization Test
A Delayed Contact Hypersensitivity test, in compliance with the FDA Requirements per 9 CFR 2.31, was performed using patches containing salicylic acid, as disclosed in the preferred embodiments, in order to determine the capacity of the test substance to induce a systemic hypersensitivity response.
The experimental procedure consisted of two phases:
1. Induction Phase
One group of 20 guinea pigs was exposed to the test material patch and one group of 10 guinea pigs was exposed to Dinitrochlorobenzene (DNCB), a known sensitizer. The day before dosing, the animals were clipped free of hair, as close to the skin as possible, using electric clippers.
The test material patch was applied to the clipped area of each of the 20 guinea pigs and held in place with a non-irritant tape. The patches were left in place for 6 hours and then removed. The test sites were scored for erythema at 24 and 48 hours post application. This procedure was repeated at the same site once a week for the next two weeks for a total of three 6-hour exposures. After the last patch application the animals remained untreated for approximately two weeks.
To the positive control group of 10 guinea pigs, a solution of 0.75% of DNCB in 50% ethanol was applied and scored as previously described.
In the following tables the individual scores for the test material patch and the positive control are presented.
TABLE 3
Individual animal scores for the test material.
Erythema
Week 1
Week 2
Week 3
Animal
24 h
48 h
24 h
48 h
24 h
48 h
1
0
0
0
0
0
0
2
0
0
0
0
0
0
3
0
0
0
0
0
0
4
0
0
0
0
0
0
5
0
0
0
0
0
0
6
0
0
0
0
0
0
7
0
0
0
0
0
0
8
0
0
0
0
0
0
9
0
0
0
0
0
0
10
0
0
0
0
0
0
11
0
0
0
0
0
0
12
0
0
0
0
0
0
13
0
0
0
0
0
0
14
0
0
0
0
0
0
15
0.5
0
0
0
0
0
16
0
0
0
0
0
0
17
0
0
0
0
0
0
18
0
0
0
0
0
0
19
0
0
0
0
0
0
20
0
0
0
0
0
0
There was no erythema noted for the test material during the three induction phases.
TABLE 4
Individual animal scores for the positive
control. Erythema
Week 1
Week 2
Week 3
Animal
24 h
48 h
24 h
48 h
24 h
48 h
1
0.5
0
0.5
0
2
1
2
1
0.5
1
1
2
1
3
1
0
1
0.5
1
1
4
0.5
0
1
0.5
2
2
5
1
0.5
0.5
0
1
1
6
1
0
1
0.5
2
1
7
0.5
0
1
1
2
1
8
1
0
1
1
2
1
9
1
0.5
1
1
1
1
10
1
0.5
1
0.5
2
1
During this test, animals showed from no to faint and faint confluent erythema.
2. Challenge Phase
After the two week rest, the test group and the positive control group were challenged on naive sites. The test material was applied to the test group and the DNCB to the positive control group. The procedure employed was as described above, except skin evaluations were made at 24, 48 and 72 hours post application. The results are presented in the following tables.
TABLE 5
Individual animal scores for the test
material. Erythema
Animal
24 h
48 h
72 h
1
0
0
0
2
0
0
0
3
0
0
0
4
0
0
0
5
0
0
0
6
0
0
0
7
0
0
0
8
0
0
0
9
0
0
0
10
0
0
0
11
0
0
0
12
0
0
0
13
0
0
0
14
0
0
0
15
0.5
0
0
16
0
0
0
17
0
0
0
18
0
0
0
19
0
0
0
20
0
0
0
During the challenge phase, no erythema was noted in the test material group at any point.
TABLE 6
Individual animal scores for the positive
control. Erythema
Animal
24 h
48 h
72 h
1
1
0.5
0.5
2
1
0.5
0.5
3
1
1
0.5
4
1
0.5
0.5
5
1
1
0.5
6
1
0.5
0
7
1
0.5
0.5
8
2
1
0.5
9
2
1
0.5
10
1
1
0.5
During this test, animals showed from no to faint and faint confluent erythema.
EXAMPLE No. 10
Repeated Insult Patch Test for Contact Sensitization and Photosensitization
The purpose of this study was to determine the cutaneous and contact sensitization and photosensitization in human volunteers of the patch containing salicylic acid as described in the preferred embodiments of the present invention, in order to claim the “hypoallergenicity” of the product.
Forty (40) healthy volunteers of both sexes, aged 20-55 years old, were included in the study.
1. Induction Phase
In this part, repeat insult patch tests in combination with maximization test were used. On intact skin of the upper back of the forty volunteers, a 1% solution of sodium lauryl sulfate was applied. The test product was, then, applied and held with a non-irritant tape. The test material was left on, for 48 hours and the site was read 30 minutes after the removal of the patch. A new patch was then reapplied to the same site. New patches were applied 3 times per week and assessments were carried out at 48 hour post removal. Repeated application of the patches using this method was continued for three weeks (total ten applications).
Additional patch tests were used to determine the contact photosensitization of the patch. During the induction phase and in parallel with the repeat patch tests, the patch tests sited were irradiated on five occasions with a solar stimulator or UVA (5 Joules) after removal of five repeated patches (serial). The phototoxic potential of the test patch was evaluated on hour, 6 and 24 hours after a single treatment.
2. Challenge Phase
After the end of the three week period a rest period of fifteen days followed. At the end of the rest period patch tests were performed as follows:
The sodium lauryl sulfate solution was first applied to the back followed by the test material patch. In the challenge test, the patch was removed at 48 hours post application and assessments were carried out at 24, 48 and 72 hours post application. During the challenge phase a second test patch was performed at another site and after its removal the site was irradiated with UVA (5 Joules). Readings were performed at 72 and 96 hours post application.
The assessments for both phases were carried out by the same investigator and under the same conditions. Scoring was based on the standard ICDRG scale. The results were negative for both phases and thus the test patch can be considered as “Hypoallergenic” and “Dermatological Tested”.
EXAMPLE No. 11
Repeated Irritation Test in Humans
The purpose of this study was to provide a quick and simple indication of the potential irritancy for the test patch. Because of the lower sensitivity of human skin to irritants, versus animal model, testing in man is generally performed by repetive application of the test patch.
The study involved 20 volunteers, male or female (15-50 years old), whose upper backs were free from any skin problems.
The test material patch was initially applied in the upper back of the volunteer for 24 hours, held with a non-irritant Scanpor tape, and then removed. One hour upon removal, the skin site was gently wiped with a moist wool ball and graded. The test material application was repeated at the same site, 24 hours later. The test material application continued for 20 days (total of 10 applications with a rest period over the weekends).
The results showed no sight of erythema, edema or exudation induced by the test patch and thus the product can be considerd as “Non irritant”.
EXAMPLE No. 12
Permeability of the Anti-acne Patches
To evaluate the local effect of the anti-acne patches according to the invention, the transdermal absorption (flux) of the salicylic acid from the adhesive matrix of the invention was determined in vitro by using human cadaver skin, according to the procedure described by Franz T., in Percutaneous absorption on the relevance of the in vitro data, J. Invest. Derm. 64, 190-195, 1975.
For in vitro flux studies, the stratum corneum of human cadaver skin was used. Using fresh, post-mortem skin samples, the stratum corneum was separated from the skin by the technique described by Kligman, A. M. Et al in Preparation of the isolated sheets of the human stratum corneum, Arch. Derm. 88, 702, 1963.
A comparative study of skin flux determination (expressed as cumulative amount of salicylic acid permeation per unit of area at any time) between the anti-acne patch of the invention (Patch 1 ), the same patch but having an adhesive matrix of double thickness (Patch 2 ) and a reference gel formulation containing 2% of salicylic acid (Gel) is presented in FIG. 4 [FIG. 4 a and FIG. 4 b].
The results showed a very limited penetration for the antiacne patch of both adhesive matrix thickness as compared to that of the reference gel formulation, assuring thus the local effect of the proposed anti-acne patch.
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A patch for topical application of an anti-acne formulation has in various embodiments a backing film, a release layer and at least one adhesive polymeric matrix layer located between the backing film and the release layer. The anti-acne formulation is uniformly distributed throughout one or more polymeric matrix layers and has an anti-acne effective amount of at least two agents selected from the group consisting of an anti-microbial, an antiseptic, an anti-irritant, a keratolytic agent, a hormone, a hormone agonist and a hormone antagonist.
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FIELD OF THE INVENTION
[0001] This invention relates to the preparation of sealing o-rings, especially very low moisture o-rings.
BACKGROUND OF THE INVENTION
[0002] A well-known method of semiconductor chip fabrication involves depositing epitaxially-grown silicon germanium (SiGe) on a silicon substrate in a chemical vapor deposition (CVD) reactor. This deposition of SiGe on the silicon substrate provides a layer of material to form transistors. SiGe deposition is commonly used to produce high-speed, low-power RF and photonic devices.
[0003] During SiGe deposition, oxygen present in the CVD reactor chamber is incorporated into the SiGe film. Although the mechanism for enhanced oxygen incorporation in SiGe films is not fully understood, it is a well-documented phenomenon. Elevated oxygen levels in the CVD reactor chamber used to deposit SiGe cause numerous problems in the SiGe films produced in the CVD reactor chamber. Among these problems are elevated sheet resistance of the SiGe p-type base and poor crystal quality. In addition, the reactor must be taken offline for weeks or even months before acceptable levels of oxygen in the chamber are achieved; while the reactor is offline, it is completely disassembled to remove moisture, reassembled, and then tested until acceptable oxygen levels in SiGe films are achieved. This is costly as the offline reactor clearly cannot be used for manufacturing semiconductor chips.
[0004] Reducing and stabilizing oxygen levels in the CVD reactor is desirable because it would reduce variation in resistance of the SiGe p-type base, improve crystal quality, and also increase the amount of time a single CVD reactor is online and used for manufacturing chips. In addition, minority carrier lifetime increases by 1.33 orders of magnitude for each decade of oxygen reduction. (T. Ghani et al., “Effect of Oxygen on Minority-Carrier Lifetime and Recombination Currents in Si 1-x -Ge x Heterostructure Devices,” Applied Physics Letters, 58(12), 1991) Increasing the minority carrier lifetime would improve the performance of the semiconductor chip by increasing the number of charge carriers.
[0005] Efforts to reduce the effects of elevated oxygen levels or SiGe base resistance in CVD reactors have focused on adding diborane (B 2 H 6 ) to the reaction chamber. While the addition of boron does reduce the sheet resistance of the SiGe p-type base, it may require other process adjustments which would ultimately have a negative effect on the process's stability. For instance, it has been demonstrated that variations to B 2 H 6 flow can modulate the SiGe base width and Ge concentration.
[0006] It is known that the elevated oxygen levels in a CVD reactor are due to outgassing and permeation of gas (moisture and solvents) from the sealing o-rings used on a CVD reactor. Outgassing is a result of gas, usually water vapor, desorbing from the CVD reactor chamber-side surface of the o-ring as well as gas in the bulk of the o-ring diffusing to the surface of the o-ring, where it is desorbed. Gas from the atmosphere can permeate across the bulk of the o-ring via diffusion transport and into the reactor chamber by desorbtion. (P. Danielson, “Gas Loads and O-Rings,” A Journal of Practical and Useful Vacuum Technology) Once moisture is in the reactor chamber, it will adsorb and desorb over and over.
[0007] Permeation is a function of material properties of the o-rings, how many linear inches of the o-rings are exposed to vacuum, and the pressure differential across the membrane or seal. While the gas load resulting from permeation is constant, the gas load resulting from outgassing and virtual leaks fluctuates; generally, permeation rates determine the lower boundary of oxygen concentration in the CVD reactor while outgassing rates set the upper boundary of oxygen concentration in the reactor. O-ring permeation can be described mathematically by the following equation: Q=K P 1 1lj −P 2 1lj /h, where h is the effective material thickness, K is the permeation constant, and j is the dissociation constant (generally, j=1 for gases in non-metals, j=2 for diatomic gas in metal).
[0008] As shown in FIG. 1 (taken from Phil Danielson, “Gas Loads and O-Rings,” A Journal of Practical and Useful Vacuum Technology, 2002), when a new unbaked o-ring is installed on a vacuum system, the outgassing via diffusion transport of the unbaked o-ring 10 is responsible for a gas load higher that that due to permeation 12 . As pumping time in the vacuum system increases, the gas load due to outgassing from the unbaked o-ring 10 decreases and permeation 12 becomes responsible for the primary gas load. The gas load due to permeation 12 remains constant. The gas load due to outgassing from a baked o-ring 14 over time becomes lower than that due to permeation 12 but, as will be noted in greater detail below, baked o-rings may be unsuitable as sealing rings in CVD reactors due to effects to elasticity and potentially the permeation properties.
[0009] In SiGe deposition, outgassing from the o-rings may affect the stability of the process and therefore frequently requires adjustments to the process. It would be desirable to reduce the oxygen concentration in the CVD reactor to levels due to permeation since, as noted above, oxygen levels due to permeation are constant over time and generally are lower than oxygen levels due to outgassing.
[0010] The gas load from the o-rings is due in large part to the manufacturing process. A new o-ring may contain unreacted monomer, solvents, volatile curing agents, and water vapor. The curing process may also increase the gas load since HF is formed during curing and acid acceptors such as MgO are added to react with HF. (Id.) It can take weeks or months for the water in a new ring to outgas; however, in an oxygen-sensitive process such as SiGe deposition in a CVD reactor, this can be extremely expensive since it removes the CVD reactor from the manufacturing process until acceptable oxygen levels are achieved. O-rings may be baked at atmosphere before installation but this only removes some of the water trapped in the o-ring bulk and may affect the elasticity of the o-ring, making it unsuitable for sealing the CVD reactor. The vacuum baking will remove a large portion of moisture but the effect on elasticity, mass loss, and permeation rates are a serious concern.
[0011] Although vacuum and/or heat-treated o-rings may be purchased from vendors, the gas load in these o-rings is still high. The lowest recorded level of oxygen in SiGe film using low-moisture o-rings per the vendor specifications for preparation (wiping the o-ring with isopropyl alcohol before installation) is 10 18 atoms/cc of oxygen; this oxygen level was achieved only after approximately 1500 wafers had been processed over the course of more than five weeks. Given the amount of time it takes for a new o-ring to outgas, the SiGe deposition process may be unstable for weeks following a preventive maintenance procedure where a new o-ring is installed before the oxygen concentration in a CVD reactor to reach an acceptable level and consistent performance is achieved. Therefore, it would be desirable to have moisture-depleted o-rings that could be installed on a CVD reactor without requiring the reactor to be offline for a long period of time until acceptable oxygen levels are reached.
[0012] It is an object of this invention to provide a preparation for sealing o-rings that removes excess moisture from the bulk of the o-ring without affecting the o-ring's elasticity, mass, and permeation rate.
[0013] It is an object of this invention to provide o-rings with a low gas load.
[0014] It is another object of the invention to provide o-rings for CVD reactors which will not create elevated oxygen levels in the reactor chamber due to outgassing.
[0015] It is yet another object of this invention to provide o-rings for use with CVD reactors so that oxygen levels in a CVD reactor are close to permeation levels which remain constant over time.
[0016] It is yet another object of this invention to provide moisture-depleted o-rings for use with a CVD reactor such that the oxygen concentration in SiGe films are reduced.
SUMMARY OF THE INVENTION
[0017] The objects are met by a method for preparing o-rings in which the o-rings are placed under vacuum in an inert atmosphere (N 2 , for instance) for a predetermined amount of time. Heat is not applied. While the o-rings are under vacuum, moisture is removed from the o-rings via diffusion transport.
[0018] When o-rings are prepared in the above fashion and then fastened to a CVD reactor, the oxygen levels in SiGe film are reduced to levels below typical secondary ion mass spectometry (SIMS) detection, i.e., below 2×10 17 atoms/cc (compared with 10 18 atoms/cc of oxygen when o-rings not placed under vacuum were used).
BRIEF DESCRIPTION OF THE DRAWINGS
[0019] [0019]FIG. 1 is a graph showing the gas load of an o-ring under vacuum over time.
[0020] [0020]FIG. 2 is a chart showing o-ring outgassing and permeation per linear inch of an o-ring following 1000 hours under vacuum.
[0021] [0021]FIG. 3 is a graph showing the outgassing rate for 100 linear inches of a viton o-ring as a function of vacuum time at room temperature.
[0022] [0022]FIG. 4 is a graph of in-film oxygen concentration versus the number of wafers cycled through a CVD reactor following a maintenance procedure in which either standard or moisture-depleted o-rings are installed on the CVD reactor.
[0023] [0023]FIG. 5 is a graph of normalized sheet resistance versus the number of wafers cycled through a CVD reactor following a maintenance procedure in which either standard or moisture-depleted o-rings are installed on the CVD reactor.
DETAILED DESCRIPTION
[0024] For best results, double clean-room gloves should be worn whenever o-rings are handled. The gloves should be changed frequently, every 30 or 60 minutes, and must be changed if they are contaminated. The o-rings should be kept in packaging in an N 2 environment until they are to be processed to avoid unnecessary exposure to the atmosphere. All work surfaces with which the o-rings may come in contact should be wiped with isopropyl alcohol (IPA).
[0025] Before placing the o-ring under vacuum, the vacuum's N 2 source should be checked to ensure that it is purified to <1 ppm H 2 O. The interior of the vacuum vessel should be wiped with IPA. For best results, the vacuum chamber should also be checked to verify that there are no external leaks and a rate-of-rise (ROR) should be performed to ensure it is less than 1 mtorr/minute. (An ROR procedure may be performed by: 1) turning off all gases and pump the vessel to base pressure; 2) isolating the vacuum vessel by closing the isolation valve; 3) recording the base pressure and allow the system to “leak-up” for a period of time ranging from 30 minutes to several hours; and 4) calculating the ROR by subtracting the initial pressure from the final pressure and dividing that number by the total leak-up time.) If the ROR exceeds 1 mtorr/minute, the system should be pumped and purged with N 2 until the ROR requirement is satisfied.
[0026] Prior to placing a new o-ring under vacuum, it should be dry-wiped with isopropyl alcohol (IPA) on a clean-room wipe. The o-ring should be placed in the vacuum chamber immediately after the IPA wipe. The N 2 flow should be 1 standard liter per minute (slpm) and the vacuum pressure should range from 1 mtorr-50 torr. In other embodiments, an N 2 flow greater than 1 slpm may be used as long as the vacuum pressure range noted above can be maintained. Low temperatures, ranging from 20° C. to 200° C. should be used. As noted above, heat facilitates the removal of moisture from an o-ring but excessive application of heat may result in loss of mass, shape, and flexibility and, therefore, difficult installation, premature failure, and increased permeation rates.
[0027] The o-rings should remain under vacuum with nitrogen purge for the minimum process time. The minimum process time takes the following into consideration: 1) outgassing rates as a function of pump time for baked and unbaked materials; 2) dimensions, principally length, of o-ring exposed to vacuum and the outgassing rate per linear inch of o-ring; and 3) if dopants are used, achieving outgassing rates that are 2 to 3 decades below the dopant injection (diborane injection levels for p-type SiGe are in the μ-sccm (standard centimeters cubed per minute) to m-sccm range).
[0028] The outgassing rate is expressed in terms of [(pressure×volume)/(time×length)], usually torr-litter/sec-inch, or throughput per linear inch. This is converted to sccm as follows: Q tot =Q inch (1 stdatm/760 torr)(1000 cc/liter)(60 sec/min)(x), where Q tot =total gas load from o-rings in sccm and x=linear inches of o-ring exposed to vacuum.
[0029] Outgassing rates may be obtained from vendors or by using the rate-of-rise (ROR) technique. In the ROR technique, the o-rings are placed under vacuum and the ROR is measured. The chamber ROR that was predetermined during the vacuum preconditioning procedures is substracted and the resulting ROR is converted to the equivalent outgassing rate.
[0030] In one embodiment of the invention, the outgassing rate may also be calculated as follows. Referring to FIG. 1, the total outgassing of an unbaked viton o-ring after a given number of hours may be obtained from experiments and calculations (in this instance performed by Phil Danielson and taken from “Gas Loads and O-Rings,” A Journal of Practical and Useful Vacuum Technology, 2002). Assuming a process time here of 1000 hours (depending on the size and type of o-ring, process times may vary), the total outgassing per linear inch is approximately 3×10 −7 torr-liters/sec/linear-inch. Using the equation above (Q tot =Q inch (1 stdatm/760 torr) (100 cc/liter) (60 sec/min) (x), where Q tot =total gas load from o-rings in sccm and x=linear inches of o-ring exposed to vacuum), the total outgassing rate of the o-ring surface exposed to vacuum may be calculated.
[0031] [0031]FIG. 2 shows o-ring outgassing and permeation 18 versus linear inches of o-ring following 1000 hours of pumping for a unbaked o-ring 16 and a baked o-ring 20 . Not surprisingly, as the number of linear inches in an o-ring increases, the gas load due to outgassing for both the baked 20 and unbaked 16 o-ring as well as permeation 18 increase.
[0032] [0032]FIG. 3 shows the outgassing rate 22 for 100 linear inches of a viton o-ring as a function of vacuum time at room temperature. As shown in FIG. 3, depletion of bulk moisture for a viton o-ring having 100 linear inches of material exposed to vacuum takes many hours. Using the equation discussed above in FIG. 1, Q tot =Q inch (1 stdatm/760 torr) (100 cc/liter) (60 sec/min) (x), where Qtot=total gas load from o-rings in sccm and x=linear inches of o-ring exposed to vacuum, for an o-ring having 100 linear inches exposed to vacuum, and assuming the total outgassing per linear inch (Q inch ) is approximately 3×10 −7 torr-liters/sec/linear-inch, the outgassing rate for this o-ring is 3×10 −5 torr-liters/sec (on the order of B 2 H 6 injection to SiGe films). Similar calculations may be performed for differently-sized o-rings made of different materials. Determining the required processing time to deplete moisture in an o-ring may require several iterations of the above calculations. For instance, if 1000 hours under vacuum is more than sufficient, the processing time should be recalculated by using 500 hours, etc. A few iterations may be required.
[0033] Two different techniques may be used to determine when the moisture removal process described above has reached its end point. Residual gas analyzer (RGA) techniques may be used, though this data may be difficult to interpret due to the extremely low partial pressure of oxygen and H 2 O within the system. Another technique is to measure in-film incorporation of oxygen by secondary mass spectometry (SIMS). FIG. 4 shows the in-film oxygen concentration (determined by SIMS) as a function of the number of wafers cycled through the CVD reactor after performing a preventive maintenance procedure (PM 1 ) where new standard o-rings are installed compared with a preventive maintenance procedure (PM 2 ) where moisture-depleted o-rings are installed. PM 1 24 shows in-film oxygen concentration when standard o-rings are used. After about 200 wafers are cycled, in-film oxygen concentration is 2×10 19 atoms/cc. The in-film oxygen concentration drops to 3.5×10 18 atoms/cc after about 500 wafers are recycled, and, after 1500 wafers have been cycled, the in-film oxygen concentration drops to 5.6×10 17 atoms/cc. When moisture-depleted o-rings are used in PM 2 26 , the initial in-film oxygen concentration is 10 18 atoms/cc. After about 450 wafers are processed, in-film oxygen concentration is 2.5×10 17 atoms/cc. The use of moisture-depleted o-rings on a CVD reactor clearly leads to lower in-film oxygen concentrations that are achieved much more quickly than in systems using standard, non-moisture-depleted o-rings.
[0034] [0034]FIG. 5 shows normalized sheet resistance versus the number of wafers cycled in a CVD reactor following preventive maintenance procedures PM 1 and PM 2 . PM 1 28 , which employs standard, non-moisture-depleted o-rings, results in a sheet resistance of approximately 1.25 after about 50 wafers are recycled; the sheet resistance does not drop to 1.0 until approximately 500 wafers have been recycled. In contrast, PM 2 30 , which employs moisture-depleted o-rings, results in a normalized sheet resistance of approximately 1.0 almost immediately; this sheet resistance remains more or less constant. Referring to both FIGS. 4 and 5, it appears that an in-film oxygen concentration of 10 18 atoms/cc, the initial in-film oxygen concentration achieved by using moisture-depleted o-rings in PM 2 26 as shown in FIG. 4, represents the point at which oxygen no longer affects sheet resistance since, as shown in FIG. 5, a normalized sheet resistance of 1.0 is achieved almost immediately when moisture-depleted o-rings are used in PM 2 30 , where, as shown in FIG. 4, the initial in-film oxygen concentration is 10 18 atoms/cc. This “sheet resistance versus oxygen threshold” will be process dependent; however, lowering oxygen is a must for any process threshold.
[0035] Referring to FIGS. 4 and 5, it is clear that maintenance procedures which use moisture-depleted o-rings achieve acceptable oxygen concentrations in a CVD reactor far more quickly than procedures which do not. In-film oxygen levels below SIMS detection, i.e., 2×10 17 atoms/cc have been demonstrated on a regular basis. In addition, using moisture-depleted o-rings leads to in-film oxygen concentrations of 10 18 atoms/cc (i.e., the level at which oxygen concentration does not affect sheet resistance) within 2-3 days; when non-moisture-depleted o-rings were used, it took more than five weeks to achieve this level, during which time approximately 1500 wafers were processed.
[0036] As noted above, o-rings should remain under vacuum with the nitrogen purge for the minimum calculated process time or until they are needed, whichever is greater. The vacuum chamber should therefore be considered an o-ring storage facility. Once the moisture depletion process starts for o-rings, i.e., when the o-rings are placed under vacuum, the vacuum should remain undisturbed. Adding additional o-rings to the vacuum chamber at a much later time will recontaminate those o-rings which were undergoing processing prior to the new o-rings being added. Cycling the chamber to atmosphere should also be avoided since that adds moisture, requiring additional process time to remove that moisture. If the vacuum chamber must be opened for maintenance issues, the o-rings must be stored in a nitrogen-purged cabinet. When the chamber is ready again, the o-ring conditioning can be resumed.
[0037] O-rings should not be removed from vacuum until they are to be installed on the CVD reactor. Once they are installed, an N2 purge box or something similar should be used to minimize exposure to atmosphere until the system is closed. As noted above, o-rings should be handled with gloves and all surfaces with which the o-rings will come into contact should be wiped with IPA, though the o-rings should not be wiped IPA once they are processed.
[0038] Once the o-rings are installed, cold chamber leakrates should be taken before heat is applied. The temperature should be slowly ramped over a period of 3-12 hours to no greater than 300° C. Following temperature ramping and chamber seasoning, SIMS and sheet resistance monitors should be taken periodically to determine overall effectiveness of the outgassing routine.
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Very low moisture o-rings are prepared by placing standard o-rings under vacuum in an inert atmosphere for a period of time sufficient to achieve a desired outgassing rate. Heat is not applied. While the o-rings are under vacuum, moisture is removed from the o-rings via diffusion transport.
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CLAIM OF PRIORITY
[0001] The present application claims priority from Japanese patent application JP2008-313876 filed on Dec. 10, 2009, the content of which is hereby incorporated by reference into this application.
BACKGROUND OF THE INVENTION
[0002] The present invention relates to a technique in which, by using a communication apparatus which is connected to a network, which receives packets transferred through the network to perform different processes in accordance with communication states between a client and a server that transmit and receive packets, and which changes data accumulated within the apparatus, and generates and transmits a new packet to the outside, plural servers are arrayed (coupled as one server), simultaneous transmission of large-volume data to plural users is realized by a system which requires less space and less electric power, and data reproduction in a high-speed response is realized by broadband transmission at the time of reproduction.
[0003] The progress of integration of broadcasting and communications increases the needs of large volume of video distribution services, improving a sensory speed, and reduction in server installation cost and power consumption in a data center. A VOD high-speed distribution apparatus and a VOD distribution system for satisfying these needs are required.
[0004] As shown in FIG. 28 , a conventional video distribution system is a system 2800 which includes a disk array 2801 , servers 2802 , and a load balancer 2803 .
[0005] The disk array 2801 is an apparatus obtained by logically integrating plural hard disks into one. Reading and writing are performed using disk access dedicated lines 2805 such as fiber channels or iSCSI.
[0006] The servers 2802 are connected to normal communication lines 2806 and the disk access dedicated lines 2805 . When receiving a video data distribution request from a client 2804 through the communication line 2806 , video data is read from the disk array 2801 through the disk access dedicated line 2805 , and the read data is transmitted to the client 2804 through the communication line 2806 .
[0007] The load balancer 2803 disperses, among plural servers 2802 - i (i=1 to n), the video data distribution request received from the client 2804 through a communication line 2807 .
[0008] As shown in FIG. 27 , each piece of video reproducing software 2705 of a client 2702 includes a reproducing unit which generates a video and a reception buffer which temporarily accumulates video data.
[0009] When the video reproducing software 2705 instructs to reproduce data, a video data distribution request is transmitted from the client 2702 to a server 2701 . When the server 2701 receives the video data distribution request from the client 2702 , distribution of video data 2703 is started. The video data 2703 is temporarily accumulated in the reception buffer of the video reproducing software 2705 of the client 2702 . If the amount of video data accumulated in the reception buffer exceeds a threshold value for starting reproduction, the reproducing unit of the video reproducing software 2705 reads the video data from the reception buffer, and reproducing of the video is started.
[0010] After the video reproducing software 2705 instructs to reproduce data, the server transmits the video data corresponding to the threshold value for starting reproduction in a broad band, and shortens time for the amount of video data accumulated in the reception buffer to exceed the threshold value for starting reproduction, so that the response speed (time from an instruction of reproduction to starting of reproduction) of video reproduction can be shortened. It is possible to realize video reproduction with a high sensory speed.
[0011] In the case where the server transmits the video data in a broad band after the instruction of reproduction, the server needs to be provided with a throughput performance 2603 for high-speed reproduction in addition to a throughput performance 2604 for normal distribution, as shown in FIG. 26 .
BRIEF SUMMARY OF THE INVENTION
[0012] Two problems involved in the data distribution system obtained by combining the disk array, the servers and the load balancer such as the above-described video data distribution system will be described below.
[0013] The first problem will be described first.
[0014] In the system using the disk array and the servers, an arithmetic circuit substrate for arraying the hard disks, and interfaces such as fiber channels or iSCSI are mounted in the disk array. Interfaces to be connected to the disk array are mounted in the servers as well. The elements mounted in the disk array cause a problem that power consumption and a system-occupied space are increased.
[0015] Next, the second problem will be described using FIG. 25 and FIG. 26 .
[0016] In the case where a server 2601 transmits the video data in a broad band after the instruction of reproduction, the server 2601 needs to be provided with the throughput performance 2603 for high-speed reproduction in addition to the throughput performance 2604 for normal distribution. The throughput performance 2603 for high-speed reproduction is used when data corresponding to the threshold value for starting reproduction is transmitted.
[0017] In a data distribution system used for conventional video distribution, a load balancer 2500 transmits a data distribution request received from a client to each server on the basis of only the load of each server which changes every second. Accordingly, it is impossible to preliminarily recognize what server distributes data, and as a result, each of servers 2504 , 2505 , and 2506 transmits data corresponding to the threshold value for starting reproduction in a broad band after the instruction of reproduction. Thus, the throughput performance for high-speed reproduction in addition to the throughput performance for normal distribution is needed in each server. If it is assumed that an average transmission band at the time of broadband transmission is bh (Mbps), a transmission band at the time of normal distribution is bl (Mbps), the number of server lines is m (lines), the number of clients is n (pieces), a frequency of changing an instruction of reproduction and a reproduced section per one client is r (the number of times/second), and a threshold value for starting reproduction (represented by multiplying a transmission band at the time of normal distribution by t seconds) of the reception buffer of the data reproducing software is bl/8·t (Mbyte), a total value Bh of the throughput performances for high-speed reproduction necessary for the lines of each server is obtained as follows.
[0018] In each line of the servers, bl/8·t (Mbyte) of data corresponding to the threshold value for starting reproduction is transmitted at a frequency of n/m·r (the number of times/second). Thus, an average throughput performance of bl/8·t·8·n/m·r (Mbps) for high-speed reproduction is required. Further, transmission of data corresponding to the threshold value for starting reproduction requires a broad band. Accordingly, a throughput performance for high-speed reproduction corresponding to the average transmission band bh (Mbps) at the time of broadband transmission is additionally required.
[0019] On the basis of the above, a throughput performance Bh′ for high-speed reproduction necessary for each line of the servers and the total value Bh (Mbps) of the throughput performances for high-speed reproduction necessary for the all lines are represented by formulae 2401 and 2402 of FIG. 24 , respectively.
[0020] Further, if it is assumed that the total value of the throughput performances of the all lines of the servers is B (Mbps), the total value Bh of the throughput performances for high-speed reproduction necessary for the all lines corresponds to a difference between the total value B of the throughput performances of the all lines and a total value n·bl of transmission bands at the time of normal distribution. (formula 2403 )
[0021] By using the formulae 2402 and 2403 , the average transmission band bh (Mbps) at the time of broadband transmission is represented by a formula 2404 .
[0022] Thus, the response time (transmission time when data corresponding to the threshold value for starting reproduction is transmitted in a broad band) T (seconds) of reproduction is represented by a formula 2405 . Accordingly, in the conventional data distribution system where each of the servers 2504 , 2505 , and 2506 transmits data corresponding to the threshold value for starting reproduction after the instruction of reproduction, the larger the number m of server lines becomes, the longer the response time T of reproduction becomes.
[0023] As described above, the data distribution system obtained by combining the disk array, the servers, and the load balancer involves two problems, namely, power consumption and a system-occupied space become large, and the larger the number of server lines becomes, the longer the response time of reproduction becomes.
[0024] Next, a problem involved in the load balancer used in data distribution such as the video distribution will be described below.
[0025] The load balancer 2500 used for the data distribution system such as the conventional video distribution transmits a data distribution request received from a client to each server on the basis of only the load of each server. Accordingly, in the data distribution system using the disk array and the servers, it is necessary to control an access to the requested file in the disk array, and an arithmetic circuit substrate for arraying the hard disks or interfaces such as fiber channels or iSCSI need to be mounted. Further, it is necessary for even the servers to be provided with interfaces to be connected to the disk array. That is, the data distribution request is transmitted by the load balancer 2500 to each server on the basis of only the load of the server, which leads to the necessity of the elements mounted in the disk array, resulting in increase of power consumption and a system-occupied space of the data distribution system.
[0026] Further, as described above, the load balancer 2500 used for the data distribution system such as the conventional video distribution system transmits the data distribution request received from the client to each server on the basis of only the load of each server which changes every second. Accordingly, it is impossible to preliminarily recognize what server distributes data, and as a result, each of the servers 2504 , 2505 , and 2506 transmits data corresponding to the threshold value for starting reproduction in a broad band after the instruction of reproduction as shown in FIG. 25 . Thus, if the conventional load balancer 2500 is used for the data distribution system, the throughput performance for high-speed reproduction in addition to the throughput performance for normal distribution is needed in each server.
[0027] If it is assumed that an average transmission band at the time of broadband transmission is bh (Mbps), a transmission band at the time of normal distribution is bl (Mbps), the number of server lines is m (lines), the number of clients is n (pieces), a frequency of changing an instruction of reproduction and a reproduced section per one client is r (the number of times/second), and a threshold value for starting reproduction (represented by multiplying a transmission band at the time of normal distribution by t seconds) of the reception buffer of the data reproducing software is bl/8·t (Mbyte), then a total value Bh of the throughput performances for high-speed reproduction necessary for each line of the servers is obtained as follows.
[0028] In each line of the servers, bl/8·t (Mbyte) of data corresponding to the threshold value for starting reproduction is transmitted at a frequency of n/m·r (the number of times/second). Thus, an average throughput performance of bl/8·t·8·n/m·r (Mbps) for high-speed reproduction is required. Further, transmission of data corresponding to the threshold value for starting reproduction requires a broad band. Accordingly, a throughput performance for high-speed reproduction corresponding to the average transmission band bh (Mbps) at the time of broadband transmission is additionally required.
[0029] On the basis of the above, a throughput performance Bh′ for high-speed reproduction necessary for each line of the servers and the total value Bh (Mbps) of the throughput performances for high-speed reproduction necessary for the all lines are represented by formulae 2401 and 2402 of FIG. 24 , respectively.
[0030] Further, if it is assumed that the total value of the throughput performances of the all lines of the servers is B (Mbps), the total value Bh of the throughput performances for high-speed reproduction necessary for the all lines corresponds to a difference between the total value B of the throughput performances of the all lines and a total value n·bl of transmission bands at the time of normal distribution. (formula 2403 )
[0031] By using the formulae 2402 and 2403 , the average transmission band bh (Mbps) at the time of broadband transmission is represented by a formula 2404 .
[0032] Thus, the response time (transmission time when data corresponding to the threshold value for starting reproduction is transmitted in a broad band) T (seconds) of reproduction is represented by a formula 2405 . Accordingly, if the conventional load balancer is used for the data distribution system such as the video distribution system, the throughput performance for high-speed reproduction in addition to the throughput performance for normal distribution is needed in each server, and the larger the number m of server lines becomes, the longer the response time T of reproduction becomes.
[0033] According to an aspect of the present invention, there is provided a network system including a first server and a second server which transmit data to a data destination apparatus, and a communication apparatus which is connected to the data destination apparatus, the first server and the second server through communication lines, wherein the communication apparatus includes: a first reception unit which receives a first file access request for requesting transmission of data in files contained in the first server and the second server from the data destination apparatus; a file access request processing unit which generates, on the basis of the first file access request, a second file access request for requesting the first server to transmit part of data in the files and a third file access request for requesting the second server to transmit data subsequent to the part of data in the files; and a first transmission unit which transmits the second file access request to the first server, and transmits the third file access request to the second server after the first server completes the transmission of the part of data on the basis of the second file access request, the first server includes: a second reception unit which receives the second file access request transmitted by the communication apparatus; and a second transmission unit which transmits the part of data in the files on the basis of the second file access request, and the second server includes: a third reception unit which receives the third file access request; and a third transmission unit which transmits the data subsequent to the part of data in the files on the basis of the third file access request.
[0034] Further, according to another aspect of the present invention, there is provided a network system including a first server and a second server which transmit data to a data destination apparatus, and a communication apparatus which is connected to the data destination apparatus, the first server and the second server through communication lines, wherein the communication apparatus includes: a first reception unit which receives a first file access request for requesting transmission of data in files contained in the first server and the second server from the data destination apparatus; a file access request processing unit which generates, on the basis of the first file access request, a second file access request for requesting the first server to transmit part of data in the files and a third file access request for requesting the second server to transmit data subsequent to the part of data in the files; and a first transmission unit which transmits the second file access request to the first server, and transmits the third file access request to the second server when a specified time passes after transmission of the second file access request, the first server includes: a second reception unit which receives the second file access request transmitted by the communication apparatus; and a second transmission unit which transmits the part of data in the files on the basis of the second file access request, and the second server includes: a third reception unit which receives the third file access request; and a third transmission unit which transmits the data subsequent to the part of data in the files on the basis of the third file access request.
[0035] On the other hand, according to still another aspect of the present invention, there is provided a communication apparatus connected, through communication lines, to a data destination apparatus, and a first server and a second server which transmit data to the data destination apparatus, the communication apparatus including: a first reception unit which receives a first file access request for requesting transmission of data in files contained in the first server and the second server from the data destination apparatus; a file access request processing unit which generates, on the basis of the first file access request, a second file access request for requesting the first server to transmit part of data in the files and a third file access request for requesting the second server to transmit data subsequent to the part of data in the files; and a first transmission unit which transmits the second file access request to the first server, and transmits the third file access request to the second server after the first server completes the transmission of the part of data on the basis of the second file access request.
[0036] Further, according to still another aspect of the present invention, there is provided a communication apparatus connected, through communication lines, to a data destination apparatus, and a first server and a second server which transmit data to the data destination apparatus, the communication apparatus including: a first reception unit which receives a first file access request for requesting transmission of data in files contained in the first server and the second server from the data destination apparatus; a file access request processing unit which generates, on the basis of the first file access request, a second file access request for requesting the first server to transmit part of data in the files and a third file access request for requesting the second server to transmit data subsequent to the part of data in the files; and a first transmission unit which transmits the second file access request to the first server, and transmits the third file access request to the second server when a specified time passes after transmission of the second file access request.
[0037] In the network system disclosed in this application of the present invention, effects obtained from representative aspects will be briefly described. Without using a disk array, plural servers are directly arrayed by a load balancing module (a module for dispersing a distribution request from a client among plural servers which accumulate the same file) and a file dispersion access module (a module for sorting a distribution request from a client into a server storing the file corresponding the distribution request). Accordingly, elements (an arithmetic circuit substrate for arraying the hard disks and interfaces such as fiber channels or iSCSI) to be mounted in the disk array used in the conventional method are not necessary. Thus, it is possible to provide a data distribution apparatus and a data distribution system in which power consumption and an occupied space used by unnecessary elements are reduced and a performance per 1 W·IU is improved.
[0038] Further, irrespective of the number m of server lines, the response speed of reproduction becomes constant, and thus, it is possible to provide a data distribution apparatus and a data distribution system in which the response time of reproduction becomes fast by m times as compared to the conventional ones.
[0039] It should be noted that if it is assumed that an average transmission band at the time of broadband transmission is bh (Mbps), a transmission band at the time of normal distribution is bl (Mbps), the number of server lines is m (lines), the number of clients is n (pieces), a frequency of changing an instruction of reproduction and a reproduced section per one client is r (the number of times/second), and a threshold value for starting reproduction (represented by multiplying a transmission band at the time of normal distribution by t seconds) of the reception buffer of the data reproducing software is bl/8·t (Mbyte), then a total value Bh of the throughput performances for high-speed reproduction necessary for the lines of the dedicated servers is obtained as follows.
[0040] In each line of the servers, bl/8·t (Mbyte) of data corresponding to the threshold value for starting reproduction is transmitted at a frequency of n·r (the number of times/second). Thus, an average throughput performance of bl/8·t·8·n·r (Mbps) for high-speed reproduction is required. Further, transmission of data corresponding to the threshold value for starting reproduction requires a broad band. Accordingly, a throughput performance for high-speed reproduction corresponding to the average transmission band bh (Mbps) at the time of broadband transmission is additionally required.
[0041] On the basis of the above, the total value Bh (Mbps) of the throughput performances for high-speed reproduction necessary for the lines of the dedicated servers is represented by a formula 2301 of FIG. 23 .
[0042] Further, if it is assumed that the total value of the throughput performances of the all lines of the servers is B (Mbps), the total value Bh of the throughput performances for high-speed reproduction necessary for the all lines corresponds to a difference between the total value B of the throughput performances of the all lines and a total value n·bl of transmission bands at the time of normal distribution. (formula 2302 )
[0043] By using the formulae 2301 and 2302 , the average transmission band bh (Mbps) at the time of broadband transmission is represented by a formula 2303 .
[0044] Thus, the response time (transmission time when data corresponding to the threshold value for starting reproduction is transmitted in a broad band) T (seconds) of reproduction is represented by a formula 2304 . The response time T of reproduction is constant irrespective of the number m of server lines.
[0045] In the communication apparatus disclosed in this application of the present invention, effects obtained from representative aspects will be briefly described.
[0046] In the communication apparatus disclosed in the application, plural servers can be directly arrayed by a load balancing module (a module for dispersing a distribution request from a client among plural servers which accumulate the same file) and a file dispersion access module (a module for sorting a distribution request from a client into a server storing the file corresponding the distribution request). Accordingly, elements (an arithmetic circuit substrate for arraying the hard disks and interfaces such as fiber channels or iSCSI) to be mounted in the disk array used in the conventional method are not necessary in the data distribution apparatus and the data distribution system. Thus, by using the communication apparatus disclosed in this application in the data distribution apparatus and the data distribution system, it is possible to reduce power consumption and an occupied space used by unnecessary elements of the data distribution apparatus and the data distribution system and to improve a performance per 1 W·IU.
[0047] Further, by using the communication apparatus disclosed in the application, the response speed of reproduction becomes constant irrespective of the number m of server lines, and thus, it is possible to provide a data distribution apparatus and a data distribution system in which the response time of reproduction becomes fast by m times as compared to the conventional ones.
BRIEF DESCRIPTION OF THE DRAWINGS
[0048] FIGS. 1A and 1B are explanation diagrams of a data distribution system according to an embodiment of the present invention;
[0049] FIG. 2 is a configuration block diagram of a communication apparatus according to the embodiment of the present invention;
[0050] FIG. 3 is a format diagram of a TCP/IP connection table mounted in the communication apparatus according to the embodiment of the present invention;
[0051] FIG. 4 is a flowchart for showing an address generating method of accessing the TCP/IP connection table mounted in the communication apparatus according to the embodiment of the present invention;
[0052] FIG. 5 is a flowchart for showing a method of accessing the TCP/IP connection table mounted in the communication apparatus according to the embodiment of the present invention;
[0053] FIG. 6 is an explanation diagram of the data distribution system including an initial data transmission server and a subsequent data transmission server according to the embodiment of the present invention;
[0054] FIG. 7 is an explanation diagram for showing a searching method of a conflict of a hash value in the TCP/IP connection table according to the embodiment of the present invention;
[0055] FIG. 8 is an explanation diagram for showing an aging method in the TCP/IP connection table according to the embodiment of the present invention;
[0056] FIG. 9 is an explanation diagram for showing a TCP state transition according to the embodiment of the present invention;
[0057] FIG. 10 is an explanation diagram of packets transmitted and received among the communication apparatus, clients, and servers according to the embodiment of the present invention;
[0058] FIG. 11 is an explanation diagram of packet headers transmitted and received among the communication apparatus, clients, and servers according to the embodiment of the present invention;
[0059] FIG. 12 is an explanation diagram of an example of a selecting method of an IP address of the server according to the embodiment of the present invention;
[0060] FIG. 13 is an explanation diagram of an example of a file accumulating method of the server according to the embodiment of the present invention;
[0061] FIG. 14 is an explanation diagram of an example of a selecting method of an IP address of the server according to the embodiment of the present invention;
[0062] FIG. 15 is an explanation diagram of an example of a file accumulating method of the server according to the embodiment of the present invention;
[0063] FIG. 16 is an explanation diagram of an example of a selecting method of an IP address of the server according to the embodiment of the present invention;
[0064] FIG. 17 is an explanation diagram of an example of a selecting method of an IP address of the server according to the embodiment of the present invention;
[0065] FIG. 18 is an explanation diagram of an example of a file accumulating method of the server according to the embodiment of the present invention;
[0066] FIG. 19 is an explanation diagram of an extended example of the data distribution system according to the embodiment of the present invention;
[0067] FIG. 20 is an explanation diagram of transmission bands of the server according to the embodiment of the present invention;
[0068] FIG. 21 is an explanation diagram of an extended example of the communication apparatus according to the embodiment of the present invention;
[0069] FIG. 22 is an explanation diagram of an extended example of the data distribution system according to the embodiment of the present invention;
[0070] FIG. 23 shows explanation formulae for a response time of reproduction in a conventional video data distribution system;
[0071] FIG. 24 shows explanation formulae for a response time of reproduction in the data distribution system according to the embodiment of the present invention;
[0072] FIG. 25 is an explanation diagram of an example of a conventional data distribution system;
[0073] FIG. 26 is an explanation diagram of data transmission bands of a data distribution server;
[0074] FIG. 27 is an explanation diagram of data transmission bands of a data distribution server and data reproducing software mounted in a client;
[0075] FIG. 28 is an explanation diagram of an example of the conventional data distribution system;
[0076] FIG. 29 is a format diagram of packet data according to the embodiment of the present invention; and
[0077] FIG. 30 is a sequence diagram for a case of using a UDP according to the embodiment of the present invention.
DETAILED DESCRIPTION OF THE INVENTION
[0078] In the following embodiment, an explanation will be made in plural divided sections or embodiments if needed as a matter of convenience. However, the sections or embodiments have a relation with each other unless otherwise specified, and one is for a modified example, a detailed explanation or a complementary explanation of a part or all of the other. In addition, if the number (including value, amount, range and the like) of constitutional elements is referred to in the following embodiment, the embodiment is not limited to a specified number and any number larger or smaller than the specified number may be used unless otherwise specified and unless the embodiment is apparently limited to the specified number in principle.
[0079] Further, it is obvious that the constituent elements (including element steps and the like) are not necessarily essential in the following embodiment unless otherwise specified and unless they are considered to be apparently essential in principle. Likewise, if the shapes and positional relations of constituent elements are referred to, constituent elements substantially approximate or similar to the shapes and the like are included unless otherwise specified and unless the shapes and positional relations are considered to be incorrect in principle. This is also applied to the value and the range.
[0080] Hereinafter, an embodiment of the present invention will be described in detail on the basis of the drawings. It should be noted that the same constituent elements are given the same reference numerals in principle throughout the all drawings for explaining the embodiment, and the explanations thereof will not be repeated.
Embodiment
[0081] Hereinafter, an embodiment of the present invention will be described using the drawings.
[0082] FIG. 1 is a configuration block diagram of an information processing system 101 according to the embodiment. It is assumed that the information processing system 101 is used as a VOD distribution system and a Web distribution system with advertisement.
[0083] In the case where the information processing system is used as the VOD distribution system, two types, i.e., an initial data transmission server 602 - 1 and a subsequent data transmission server 602 - 2 , are prepared, as shown in, for example, FIG. 6 . When data is distributed to clients A to C ( 603 - 1 to 603 - 3 ), data corresponding to a threshold value for starting reproduction of a reception buffer is transmitted from the initial data transmission server 602 - 1 in a broad band immediately after each piece of data reproducing software of the clients A to C ( 603 - 1 to 603 - 3 ) instructs to reproduce data. Thereafter, the subsequent data is transmitted from the subsequent data transmission server 602 - 2 in a normal distribution band.
[0084] The information processing system 101 includes a communication apparatus 100 and servers 102 - i (i=1 to 4). The communication apparatus 100 is connected to the servers 102 through communication lines 105 - i (i=1 to 4). Further, the communication apparatus 100 is connected to clients 103 - i (i=1 to 4) through lines 104 of a network 106 .
[0085] As shown in FIG. 1B , each server 102 is an apparatus configured in such a manner that a processor 108 , a memory 107 , a large-capacity storing unit 109 , and a network interface 110 including a transmission unit 111 and a reception unit 112 are connected to each other.
[0086] FIG. 2 shows a configuration of the communication apparatus 100 .
[0087] The communication apparatus 100 includes transmission/reception units 240 , a switching unit 201 , and a module implementation unit 200 in which a server arraying module and a broadband transmission module for reproduction are implemented.
[0088] The switching unit 201 receives packet data through the transmission/reception unit 240 - i from one of communication lines 202 - i (i=1 to 8), or from the module implementation unit 200 , and transmits the packet data to a different communication line 202 through the transmission/reception unit 240 - i , or transmits the packet data to the module implementation unit 200 .
[0089] FIG. 29 shows an example of a format of packet data transmitted and received within the communication apparatus 100 .
[0090] The packet data includes an InLine 2900 , an OutLine 2901 , a Type 2902 , a Vlan 2903 , an SMAC 2904 , a DMAC 2905 , a Proto 2906 , an SIP 2907 , a DIP 2908 , an SPort 2909 , a DPort 2910 , a TCP Flag 2911 , a PSEQ 2912 , a PACK 2913 , an OtherHeader 2914 , a various-commands 2915 , and a Payload 2916 . Further, the SIP 2907 , DIP 2908 , SPort 2909 , and DPort 2910 are collectively represented as a packet header (P.H.) 2917 in the embodiment. The P.H. 2917 shows the characteristics of the packet data.
[0091] Here, the InLine 2900 stores an input line number that is an identification number of a line through which the packet is input. The OutLine 2901 stores an output line number that is an identification number of a line through which the packet is output. The Type 2902 stores an identification number for identifying a protocol of a network layer. The Vlan 2903 stores a number for identifying a VLAN. The SMAC 2904 stores a source MAC address that is a source address of a data link layer. The DMAC 2905 stores a destination MAC address that is a destination address. The Proto 2906 stores an identification number for identifying a protocol of a transport layer such as a UDP (User Datagram Protocol). The SIP 2907 stores a source address, namely, a source IP address that is an address of a terminal on the transmission side. The DIP 2908 stores a destination address, namely, a destination IP address that is an address of a terminal on the reception side. The SPort 2909 stores a source port of a TCP. The DPort 2910 stores a destination port of a TCP. The TCP Flag 2911 stores a TCP flag number. The PSEQ 2912 stores a transmission sequence number (SEQ number). The PACK 2913 stores a reception sequence number (ACK number). The OtherHeader 2914 stores other IP/TCP header data. The various-commands 2915 stores a command of an application layer. The Payload 2916 stores data other than the packet header and the various-commands.
[0092] The module implementation unit 200 ( FIG. 2 ) includes an input/output controlling unit 205 , an ARP/IP/TCP processing unit 204 , a TCP/HTTP processing unit 203 , a TCP/IP connection table 207 , and a file access request temporarily-recording table 206 .
[0093] FIG. 3 shows an example of a format of the TCP/IP connection table.
[0094] Each of entries 320 - i (i=1 to n) includes a C-IP 301 , a D-IP 302 , a C-PORT 303 , a D-PORT 304 , a C-SEQ 305 , a DC-SEQ 306 , a C-ID 307 , a TIME 308 , a STATE 309 , an S-IP 310 , a C-IP 311 , an S-PORT 312 , a D-PORT 313 , an S-SEQ 314 , a DS-SEQ 315 , an S-ID 316 , a NEXT 317 , a POINTER 318 , and a packet header temporarily-storing area 319 .
[0095] The C-IP 301 records an IP address of a client. The D-IP 302 records a unique IP address released to the network 106 by the communication apparatus 100 . The C-PORT 303 records a TCP port number of a client. The D-PORT 304 records a TCP port number released to the network 106 by the communication apparatus 100 . The C-SEQ 305 records a TCP sequence number of a host on the client side. The DC-SEQ 306 records a TCP sequence number of the communication apparatus 100 for a host on the client side. The C-ID 307 records an ID number of an IP packet transmitted to a host on the client side by the communication apparatus 100 . The TIME 308 records the latest time when the packet is received. The STATE 309 records a state of TCP connection. The S-IP 310 records an IP address of a server. The C-IP 311 records an IP address of a client. The S-PORT 312 records a TCP port number of a server. The D-PORT 313 records a TCP port number released to the network 106 by the communication apparatus 100 . The S-SEQ 314 records a TCP sequence number of a host on the server side. The DS-SEQ 315 records a TCP sequence number of the communication apparatus 100 for a host on the server side. The S-ID 316 records an ID number of an IP packet transmitted to a host on the server side by the communication apparatus 100 . The NEXT 317 records presence or absence of a conflict of a hash value calculated when an address is generated. The POINTER 318 records a pointer to the file access request temporarily-recording table.
[0096] The input/output controlling unit 205 ( FIG. 2 ) receives a packet 231 from the switching unit 201 , and transmits a packet 230 to the ARP/IP/TCP processing unit 204 . Further, the input/output controlling unit 205 receives packets 227 to 229 transmitted from the ARP/IP/TCP processing unit 204 , and outputs a packet 232 to the switching unit 201 .
[0097] The ARP/IP/TCP processing unit 204 ( FIG. 2 ) includes a filter unit 215 , an ARP processing unit 214 , and a TCP/IP connection managing unit 213 . When receiving the packet 230 from the input/output controlling unit 205 , the filter unit 215 ( FIG. 2 ) determines whether or not the packet is the processing target. The communication apparatus 100 releases its unique IP address and MAC address to the network 106 on the client side. In the case where the packet 230 is an ARP REQUEST packet used for inquiring the unique MAC address, a packet 226 is transmitted to the ARP processing unit 214 . In addition, in the case where the packet 230 is to be transmitted to the unique IP address and has a specific number (for example, 80 or the like) that is preliminarily set by the destination port number DPort 2910 , a packet 225 is transmitted to the TCP/IP connection managing unit 213 .
[0098] Upon receiving the ARP REQUEST packet 226 , the ARP processing unit 214 ( FIG. 2 ) generates and outputs an ARP REPLY packet 228 in which the unique MAC address is described.
[0099] When receiving the TCP/IP packet 225 to be transmitted to the unique IP address and TCP port number, the TCP/IP connection managing unit ( FIG. 2 ) accesses the TCP/IP connection table 207 , and reads and initializes an entry 320 corresponding to the packet header P.H. 2917 ( 224 ). Further, the TCP/IP connection managing unit receives a new TCP state 218 and new packet data 219 from the TCP/HTTP processing unit, writes a new TCP state 224 into the TCP/IP connection table 207 ( 224 ), and outputs the new packet data 219 to the input/output controlling unit 205 ( 227 ).
[0100] FIG. 4 shows an example of an address generating method when accessing the TCP/IP connection table 207 .
[0101] In the first place, an XOR operation is performed using four field values (the source IP address SIP 2907 , destination IP address DIP 2908 , source TCP port number 2909 , and destination TCP port number 2910 ) described in the packet header P.H. 2917 shown in FIG. 29 (Step 401 ). Next, it is determined whether or not the packet is one from the server (Step 402 ). If the packet is one from the server, an XOR operation using the source IP address SIP 2907 descried in the packet header P.H. 2917 and the IP address released by the apparatus (Step 405 ).
[0102] Finally, a bit shift operation (Step 403 ) and addition of a table beginning address (Step 404 ) are performed so as to generate a table address value.
[0103] FIG. 5 shows an example of an algorithm accessible to the TCP/IP connection table 207 .
[0104] In the first place, an address is generated by the method shown in FIG. 4 (Step 502 ), and an entry is read from the TCP/IP connection table (Step 504 ) to determine whether or not the TCP Flag 2911 of the packet header is SYN (Step 505 ). If the TCP Flag 2911 is SYN in Step 505 (Step 517 ), it is determined whether or not any one of the followings is satisfied: the STATE 309 described in the entry is 0; the packet header P.H. 2917 corresponds to the C-IP 301 , D-IP 302 , C-PORT 303 , and D-PORT 304 described in the entry; and the packet header P.H. 2917 corresponds to the S-IP 310 , C-IP 311 , S-PORT 312 , and D-PORT 313 described in the entry (Step 506 ). If it is determined that one of them is satisfied in Step 506 (Step 519 ), the entry read in Step 504 is initialized (Step 511 ), the update time TIME 308 described in the entry is updated to the current time (Step 512 ), and various processes are performed for the packet (Step 515 ). If it is determined that none of them is satisfied in Step 506 (Step 520 ), 1 indicating a conflict of the hash value is written into the NEXT 317 of the entry read in Step 504 (Step 508 ). After the address value is incremented (Step 509 ), the flow returns to Step 504 to read the entry again using the address value incremented. If the TCP Flag 2911 is not SYN in Step 505 (Step 518 ), it is determined whether or not any one of the followings is satisfied: the packet header P.H. 2917 corresponds to the C-IP 301 , D-IP 302 , C-PORT 303 , and D-PORT 304 described in the entry; and the packet header P.H. 2917 corresponds to S-IP 310 , C-IP 311 , S-PORT 312 , and D-PORT 313 described in the entry (Step 507 ). If it is determined that any one of them is satisfied in Step 507 (Step 522 ), the update time TIME 308 of the entry read in Step 504 is updated to the current time (Step 512 ), and various processes are performed for the packet (Step 515 ). If it is determined that none of them is satisfied in Step 507 (Step 521 ), it is determined whether or not the NEXT of the entry read in Step 504 is 1 (Step 510 ). If it is determined that the NEXT is 1 in Step 510 (Step 523 ), the address value is incremented (Step 509 ), and then, the flow returns to Step 504 to read the entry again using the address value incremented. If it is determined that the NEXT is not 1 in Step 510 (Step 524 ), the packet is discarded and the flow is completed (Step 516 ).
[0105] By using the method for accessing the TCP/IP connection table 207 described using FIG. 4 and FIG. 5 , an access method shown in, for example, FIG. 7 can be realized.
[0106] In FIG. 7 , the address value generated using FIG. 4 is generated every four entries ( 701 - 1 to 701 - 6 ). When NEXT=0, the entry is initialized for use. When NEXT=1, entries are continuously read while shifting back to the previous entries one by one until the entry with NEXT=0 is found. The above method enables the use of all entries of the table, and it is possible to promptly search for the target entry even in a sate where the usage rate of entries of the table is high (about 90%).
[0107] As shown in FIG. 2 , the TCP/HTTP processing unit 203 includes a restructuring unit 212 , a state transition determination unit 211 , an HTTP processing unit 210 , a packet generating unit 209 , and a TCP state updating unit 208 .
[0108] FIG. 8 shows a method of deleting (aging) old entries. A table 800 - 1 shows a state before deleting (aging), and a table 800 - 2 shows a state after deleting (aging).
[0109] When the NEXT 317 described in the entry is 0, no conflict of the hash value is present, and the update time TIME 308 is much older than the current time, all the values of 0 described in the entry are cleared for deleting the entry. Further, when the NEXT 317 of the previous entry is 1, 1 is changed to 0.
[0110] The restructuring unit 212 ( FIG. 2 ) receives a TCP state 220 updated by the TCP/IP connection managing unit, and restructures a circuit configuration of the TCP/HTTP processing unit on the basis of the TCP state 220 . This is used for a case in which a dynamic restructuring processor or the like is used.
[0111] The state transition determination unit 211 ( FIG. 2 ) determines the state transition of the TCP on the basis of a TCP state 221 updated by the TCP/IP connection managing unit and packet data 222 transmitted from the TCP/IP connection managing unit. The determined state transition of the TCP is transmitted to the TCP state updating unit 208 , the packet generating unit 209 , and the HTTP processing unit 210 ( 216 ).
[0112] The TCP state updating unit 208 ( FIG. 2 ) generates a new TCP state on the basis of a determination result 216 of the state transition of the TCP, and outputs the same to the TCP/IP connection managing unit 213 ( 218 ).
[0113] FIG. 9 is a diagram for showing how the TCP state is transited by the state transition determination unit 211 and the TCP state updating unit 208 . FIG. 9 shows a transition in the case of being used as the VOD distribution system in FIG. 6 .
[0114] The initial state of the TCP state STATE 309 is a Close [value 0x00000000] 901 representing that the TCP connection has not been established. Upon receiving a packet in which the TCP Flag 2911 is SYN from the client in the state Close 901 ( 917 ), the state is transited to a state Half Open [value 0x00000001] 902 representing that the TCP connection is about to be established. Upon receiving a packet in which the TCP Flag 2911 is ACK and the PACK 2913 corresponds to the DC-SEQ 306 of the TCP/IP connection table 207 from the client in the state Half Open 902 ( 918 ), the state is transited to a state Open [value 0x00000100] 903 representing that the TCP connection has been established. Upon receiving a packet in which a GET or POST command of an HTTP protocol is described from the client in the state Open 903 ( 919 ), the state is transited to a state Burst Request [value 0x00000200] 904 representing that the TCP connection with the initial data transmission server has been started. Upon receiving a packet in which the TCP Flag 2911 is SYN-ACK and the PACK 2913 corresponds to the DS-SEQ 315 of the TCP/IP connection table 207 from the server in the state Burst Request 904 ( 920 ), the state is transited to a state Burst Half Open [value 0x00000800] 905 representing that the TCP connection with the initial data transmission server is about to be established. Upon receiving a packet in which the TCP Flag 2911 is ACK and the PACK 2913 does not correspond to the DS-SEQ 315 of the TCP/IP connection table 207 from the server in the state Burst Half Open 905 ( 926 ), the state is transited to the state Burst Half Open [value 0x00000800] 905 again. Upon receiving a packet in which the TCP Flag 2911 is ACK and the PACK 2913 corresponds to the DS-SEQ 315 of the TCP/IP connection table 207 from the server in the state Burst Half Open 905 ( 921 ), the state is transited to a state Burst Open [value 0x00010000] 906 representing that the TCP connection with the initial data transmission server has been established ( 921 ). Upon receiving a packet in which the TCP Flag 2911 is RST/PSH/URG/ACK from the server or the client in the state Burst Open 906 ( 927 ), the state is transited to the state Burst Open [value 0x00010000] 906 again ( 927 ). Upon receiving a packet in which the TCP Flag 2911 is FIN from the server in the state Burst Open 906 ( 922 ), the state becomes a state Burst Close Wait [value 0x00000002] 908 representing that the TCP connection with the initial data transmission server is about to end via a state Burst Open (FIN) [value 0x80010000] 907 representing that the FIN has been received. Upon receiving a packet in which the TCP Flag 2911 is ACK and the PACK 2913 corresponds to the DS-SEQ 315 of the TCP/IP connection table 207 from the server in the state Burst Close Wait 908 ( 923 ), the state is transited to a state Static Request [value 0x00000400] 909 representing that the TCP connection with the subsequent data transmission server has been started. Upon receiving a packet in which the TCP Flag 2911 is SYN-ACK and the PACK 2913 corresponds to the DS-SEQ 315 of the TCP/IP connection table 207 from the server in the state Static Request 909 ( 924 ), the state is transited to a state Static Half Open [value 0x00001000] 910 representing that the TCP connection with the subsequent data transmission server is about to be established. Upon receiving a packet in which the TCP Flag 2911 is ACK and the PACK 2913 does not correspond to the DS-SEQ 315 of the TCP/IP connection table 207 from the server in the state Static Half Open 910 ( 928 ), the state is transited to the state Static Half Open 910 again. Upon receiving a packet in which the TCP Flag 2911 is ACK and the PACK 2913 corresponds to the DS-SEQ 315 of the TCP/IP connection table 207 from the server in the state Static Half Open 910 ( 925 ), the state is transited to a state Static Open [value 0x00020000] 911 representing that the TCP connection with the subsequent data transmission server has been established ( 925 ). Upon receiving a packet in which the TCP Flag 2911 is RST/PSH/URG/ACK from the server or the client in the state Static Open 911 ( 929 ), the state is transited to the state Static Open 911 again ( 929 ). Upon receiving a packet in which the TCP Flag 2911 is FIN-ACK and the PACK 2913 corresponds to the DC-SEQ 306 of the TCP/IP connection table 207 from the client in a state after the state Half Open ( 931 ), the state becomes a state Close Wait [value 0x0000000C] 914 representing that the termination of the TCP connection has been started via a state FIN Recv. [value 0x8------- (- is an arbitrary value)] 913 representing that the FIN has been received. Upon receiving a packet in which the TCP Flag 2911 is FIN-ACK and the PACK 2913 corresponds to the DS-SEQ 315 of the TCP/IP connection table 207 in a state after the state Burst Request ( 930 ), the state becomes a state Close Wait [value 0x0000000C] 914 representing that the termination of the TCP connection has been started via a FIN Recv. [value 0x8------- (- is an arbitrary value)] 912 representing that the FIN has been received. Upon receiving a packet in which the TCP Flag 2911 is FIN-ACK/ACK and the PACK 2913 corresponds to the DS-SEQ 315 of the TCP/IP connection table 207 from the server in the state Close Wait 914 ( 933 ), the state is transited to a state Client Close Wait [value 0x00000004] 915 representing that the TCP connection is about to end. Upon receiving a packet in which the TCP Flag 2911 is FIN-ACK/ACK and the PACK 2913 corresponds to the DC-SEQ 306 of the TCP/IP connection table 207 from the client in the state Close Wait 914 ( 932 ), the state is transited to a state Server Close Wait [value 0x00000008] 916 representing that the TCP connection is about to end. Upon receiving a packet in which the TCP Flag 2911 is FIN-ACK/ACK and the PACK 2913 corresponds to the DC-SEQ 306 of the TCP/IP connection table 207 from the client in the state Client Close Wait 915 ( 935 ), the state is transited to the state Close 901 . Upon receiving a packet in which the TCP Flag 2911 is FIN-ACK/ACK and the PACK 2913 corresponds to the DS-SEQ 315 of the TCP/IP connection table 207 in the state Server Close Wait 916 ( 934 ), the state is transited to the Close 901 .
[0115] As described above, the TCP state is transited in the state transition determination unit 211 and the TCP state updating unit 208 . The TCP connection is established between the dedicated server and the apparatus 100 by the state transition after the instruction of reproduction from the client, and data corresponding to a threshold value for starting reproduction of the reception buffer is transmitted from the dedicated server in a broad band. Thereafter, the TCP connection is switched between the normal server and the apparatus 100 , and the subsequent data can be transmitted from the normal server in a normal distribution band. Accordingly, it is not necessary for each server to be provided with a throughput performance for high-speed reproduction.
[0116] On the basis of the packet data 222 received from the TCP/IP connection managing unit 213 and the determination result 216 of the state transition of the TCP, the HTTP processing unit 210 ( FIG. 2 ) analyzes an HTTP command described in the packet, or records an HTTP command into the file access request temporarily-recording table ( 223 ), or reads an HTTP command from the file access request temporarily-recording table ( 223 ). The analysis result and the read file access request are output to the packet generating unit 209 ( 217 ).
[0117] On the basis of the analysis result and the file access request output from the HTTP processing unit 210 and the determination result 216 of the state transition output from the state transition determination unit 211 , the packet generating unit 209 ( FIG. 2 ) generates a new packet to be output to the TCP/IP connection managing unit 213 ( 219 ). Further, the header portion of the generated packet is output to the TCP state updating unit 208 ( 233 ).
[0118] FIG. 10 is a diagram showing the types of packets transmitted and received among the communication apparatus 100 , a server 602 , and a client 603 by the HTTP processing unit 210 and the packet generating unit 209 . FIG. 10 shows a case in the VOD distribution system of FIG. 6 .
[0119] The client 603 transmits a packet 1004 in which the TCP Flag 2911 is SYN, the PSEQ 2912 is A, and the PACK 2913 is 0 to the communication apparatus 100 . Upon receiving the packet 1004 , the communication apparatus 100 changes the TCP state STATE, the C-SEQ 305 , and the DC-SEQ 306 of the TCP/IP connection table 207 into the Half Open, A+1, and B (random value)+1, respectively, and returns a packet 1005 in which the TCP Flag 2911 is SYN-ACK, the PSEQ 2912 is B, and the PACK 2913 is A+1 to the client 603 . Upon receiving the packet 1005 , the client 603 transmits a packet 1006 in which the TCP Flag 2911 is ACK, the PSEQ 2912 is A+1, and the PACK 2913 is B+1 to the communication apparatus 100 . Upon receiving the packet 1006 , the communication apparatus 100 changes the TCP state STATE of the TCP/IP connection table 207 into the Open. Accordingly, the TCP connection is established between the client 603 and the communication apparatus 100 .
[0120] After transmitting the packet 1006 , the client 603 transmits a packet 1007 in which the TCP Flag 2911 is PSH-ACK, the PSEQ 2912 is A+1, the PACK 2913 is B+1, and GET is described as a command of an HTTP protocol to the communication apparatus 100 . Upon receiving the packet 1007 , the communication apparatus 100 changes the TCP state STATE, the C-SEQ 305 , the S-SEQ 314 , and the DS-SEQ 315 of the TCP/IP connection table 207 into the Burst Request, A+1+G (the payload length of the packet 1007 ), 0, and C (random value)+1, respectively, and transmits a packet 1008 in which the TCP Flag 2911 is SYN, the PSEQ 2912 is C, and the PACK 2913 is 0 to the initial data transmission server 602 - 1 . Further, the payload data included in the packet 1007 is recorded into the file access request temporarily-recording table 206 , and the recorded beginning address is written into the POINTER 318 of the TCP/IP connection table 207 . Upon receiving the packet 1008 , the initial data transmission server 602 - 1 transmits a packet 1009 in which the TCP Flag 2911 is SYN-ACK, the PSEQ 2912 is D (random value), and the PACK 2913 is C+1. Upon receiving the packet 1009 , the communication apparatus 100 changes the TCP state STATE, the S-SEQ 314 , and the DS-SEQ 315 of the TCP/IP connection table 207 into the Burst Half Open, D+1, and C+1+G (the payload length of the packet 1007 ), respectively, and transmits a packet 1010 in which the TCP Flag 2911 is ACK, the PSEQ 2912 is C+1, and the PACK 2913 is D+1 to the initial data transmission server 602 - 1 . Accordingly, the TOP connection is established between the communication apparatus 100 and the initial data transmission server 602 .
[0121] After transmitting the packet 1010 , the communication apparatus 100 transmits, to the initial data transmission server 602 - 1 , a packet 1011 in which the TCP Flag 2911 is PSH-ACK, the PSEQ 2912 is C+1, and the PACK 2913 is D+1 while data (the payload data included in the packet 1007 ) read from the file access request temporarily-recording table 206 using the POINTER 318 of the TCP/IP connection table 207 as the beginning address is used as the payload. If the initial data transmission server 602 - 1 cannot correctly receive the packet 1011 , the initial data transmission server 602 - 1 transmits a packet 1012 in which the TCP Flag 2911 is ACK, the PSEQ 2912 is D+1, and the PACK 2913 is C+1. Upon receiving the packet 1012 , the communication apparatus 100 transmits a packet 1013 which is the same as the packet 1011 to the initial data transmission server 602 - 1 . If the initial data transmission server 602 - 1 correctly receives the packet 1011 or the packet 1013 , the initial data transmission server 602 - 1 transmits a packet 1014 in which the TCP Flag 2911 is ACK, the PSEQ 2912 is D+1, and the PACK 2913 is C+1+G (the payload lengths of the packets 1007 , 1011 and 1013 ). Upon receiving the packet 1014 , the communication apparatus 100 changes the TCP state STATE of the TCP/IP connection table 207 into the Burst Open, and transmits a packet 1015 in which the PSEQ 2912 and the PACK 2913 were changed into B+1 and A+1+G, respectively, to the client 603 . Accordingly, the initial data transmission server 602 is ready for broadband transmission of data towards the client 603 .
[0122] After transmitting the packet 1014 , the initial data transmission server 602 - 1 starts to transmit data corresponding to a threshold value for starting reproduction of the reception buffer. The initial data transmission server 602 - 1 transmits a packet 1016 in which data (length L) is included as the payload, the TCP Flag 2911 is ACK, the PSEQ 2912 is D+1, and the PACK 2913 is C+1+G. Upon receiving the packet 1016 , the communication apparatus 100 changes the S-SEQ 314 and the DC-SEQ 306 of the TCP/IP connection table 207 into D+1+L and B+1L, respectively, and transmits a packet 1017 in which the TCP Flag 2911 is ACK, the PSEQ 2912 is B+1, and the PACK 2913 is A+1+G to the client 603 . Upon receiving the packet 1017 , the client 603 transmits a packet 1019 in which the TCP Flag 2911 is ACK, the PSEQ 2912 is A+1+G, and the PACK 2913 is B+1+L to the communication apparatus 100 . Upon receiving the packet 1019 , the communication apparatus 100 transmits a packet 1018 in which the PSEQ 2912 and the PACK 2913 were changed into C+1+G and D+1+L, respectively, to the initial data transmission server 602 - 1 . Thereafter, the data corresponding to the threshold value for starting reproduction of the reception buffer is continuously transmitted from the initial data transmission server 602 - 1 to the client 603 . Finally, the initial data transmission server 602 - 1 transmits a packet 1020 in which the TCP Flag 2911 is ACK, the PSEQ 2912 is D+1+(n−1)L, and the PACK 2913 is C+1+G to the communication apparatus 100 . Upon receiving the packet 1020 , the communication apparatus 100 changes the S-SEQ 314 and the DC-SEQ 306 of the TCP/IP connection table 207 into D+1+nL and B+1+nL, respectively, and transmits a packet 1021 in which the PSEQ 2912 and the PACK 2913 were changed into B+1+(n−1)L and A+1+G, respectively, to the client 603 . Upon receiving the packet 1021 , the client 603 transmits a packet 1023 in which the TCP Flag 2911 is ACK, the PSEQ 2912 is A+1+G, and the PACK 2913 is B+1+nL to the communication apparatus 100 . Upon receiving the packet 1023 , the communication apparatus 100 transmits a packet 1022 in which the PSEQ 2912 and the PACK 2913 were changed into C+1+G and D+1+nL, respectively, to the initial data transmission server 602 - 1 . Accordingly, transmission of data corresponding to the threshold value for starting reproduction of the reception buffer is completed.
[0123] Upon receiving the packet 1022 , the initial data transmission server 602 - 1 transmits a packet 1024 in which the TCP Flag 2911 is FIN-ACK, the PSEQ 2912 is D+1+nL, and the PACK 2913 is C+1+G to the communication apparatus 100 for a request of disconnecting the TCP connection. Upon receiving the packet 1024 , the communication apparatus 100 changes the S-SEQ 314 and the DS-SEQ 315 into D+2+nL and C+2+G, respectively, while changing the TCP state STATE of the TCP/IP connection table 207 into the Burst Close Wait via the Burst FIN Receive, and transmits a packet 1025 in which the TCP Flag 2911 is FIN-ACK, the PSEQ 2912 is C+1+G, and the PACK 2913 is D+2+nL to the initial data transmission server 602 - 1 . Upon receiving the packet 1025 , the initial data transmission server 602 - 1 transmits a packet 1026 in which the TCP Flag 2911 is ACK, the PSEQ 2912 is D+2+nL, and the PACK 2913 is C+2+G to the communication apparatus 100 . Accordingly, the TCP connection between the communication apparatus 100 and the initial data transmission server 602 - 1 is disconnected.
[0124] Upon receiving the packet 1026 , the communication apparatus 100 changes the TCP state STATE, the S-SEQ 314 and the DS-SEQ 315 of the TCP/IP connection table 207 into the Static Request, 0 and E (random value)+1, respectively, and transmits a packet 1027 in which the TCP Flag 2911 is SYN, the PSEQ 2912 is E, and the PACK 2913 is 0 to the subsequent data transmission server 602 - 2 for establishment of the TCP connection with the subsequent data transmission server 602 - 2 . Upon receiving the packet 1027 , the subsequent data transmission server 602 - 2 transmits a packet 1028 in which the TCP Flag 2911 is SYN-ACK, the PSEQ 2912 is F (random value), and the PACK 2913 is E+1. Upon receiving the packet 1028 , the communication apparatus 100 changes the TCP state STATE, the S-SEQ 314 , and the DS-SEQ 315 of the TCP/IP connection table 207 into the Static Half Open, F+1, and E+1+G (the payload length of the packet 1007 ), respectively, and transmits a packet 1029 in which the TCP Flag 2911 is ACK, the PSEQ 2912 is E+1, and the PACK 2913 is F+1 to the subsequent data transmission server 602 - 2 . Accordingly, the TCP connection between the communication apparatus 100 and the subsequent data transmission server 602 - 2 is established.
[0125] After transmitting the packet 1029 , the communication apparatus 100 transmits, to the subsequent data transmission server 602 - 2 , a packet 1030 in which the TCP Flag 2911 is PSH-ACK, the PSEQ 2912 is E+1, the PACK 2913 is F+1 while data (the payload data included in the packet 1007 ) read from the file access request temporarily-recording table 206 using the POINTER 318 of the TCP/IP connection table 207 as the beginning address is used as the payload. If the subsequent data transmission server 602 - 2 cannot correctly receive the packet 1030 , the subsequent data transmission server 602 - 2 transmits a packet 1031 in which the TCP Flag 2911 is ACK, the PSEQ 2912 is F+1, and the PACK 2913 is E+1. Upon receiving the packet 1031 , the communication apparatus 100 transmits a packet 1032 which is the same as the packet 1030 to the subsequent data transmission server 602 - 2 . If the subsequent data transmission server 602 - 2 correctly receives the packet 1030 or the packet 1032 , the subsequent data transmission server 602 - 2 transmits a packet 1033 in which the TCP Flag 2911 is ACK, the PSEQ 2912 is F+1, and the PACK 2913 is E+1+G. Upon receiving the packet 1033 , the communication apparatus 100 changes the TCP state STATE of the TCP/IP connection table 207 into the Static Open, and transmits a packet 1034 in which the PSEQ 2912 and the PACK 2913 were changed into B+1+nL and A+1+G, respectively, to the client 603 . Accordingly, the subsequent data transmission server 602 - 2 is ready for data transmission in a normal distribution band towards the client 603 .
[0126] After transmitting the packet 1033 , the subsequent data transmission server 602 - 2 starts to transmit data subsequent to the data transmitted by the initial data transmission server 602 - 1 . The subsequent data transmission server 602 - 2 transmits a packet 1035 in which data (length L) is included as the payload, the TCP Flag 2911 is ACK, the PSEQ 2912 is F+1, and the PACK 2913 is E+1+G. Upon receiving the packet 1035 , the communication apparatus 100 changes the S-SEQ 314 and the DC-SEQ 306 of the TCP/IP connection table 207 into F+1+L and B+1+(n+1)L, respectively, and transmits a packet 1036 in which the TCP Flag 2911 is ACK, the PSEQ 2912 is B+1+nL, and the PACK 2913 is A+1+G to the client 603 . Upon receiving the packet 1036 , the client 603 transmits a packet 1038 in which the TCP Flag 2911 is ACK, the PSEQ 2912 is A+1+G, and the PACK 2913 is B+1+(n+1)L to the communication apparatus 100 . Upon receiving the packet 1038 , the communication apparatus 100 transmits a packet 1037 in which the PSEQ 2912 and the PACK 2913 were changed into E+1+G and F+1+L, respectively, to the subsequent data transmission server 602 - 2 . Thereafter, data is continuously transmitted from the subsequent data transmission server 602 - 2 to the client 603 . Finally, the subsequent data transmission server 602 - 2 transmits a packet 1039 in which the TCP Flag 2911 is ACK, the PSEQ 2912 is F+1+(m−1)L, and the PACK 2913 is E+1+G to the communication apparatus 100 . Upon receiving the packet 1039 , the communication apparatus 100 changes the S-SEQ 314 and the DC-SEQ 306 of the TCP/IP connection table 207 into F+1+mL and B+1+(m+n)L, respectively, and transmits a packet 1040 in which the PSEQ 2912 and the PACK 2913 were changed into B+1+(m+n−1)L and A+1+G, respectively, to the client 603 . Upon receiving the packet 1040 , the client 603 transmits a packet 1041 in which the TCP Flag 2911 is ACK, the PSEQ 2912 is A+1+G, and the PACK 2913 is B+1+(m+n)L to the communication apparatus 100 . Upon receiving the packet 1041 , the communication apparatus 100 transmits a packet 1042 in which the PSEQ 2912 and the PACK 2913 were changed into E+1+G and F+1+mL, respectively, to the subsequent data transmission server 602 - 2 . Accordingly, transmission of data is completed.
[0127] Finally, the client 603 transmits a packet 1043 in which the TCP Flag 2911 is FIN-ACK, the PSEQ 2912 is A+1+G, and the PACK 2913 is B+1+(m+n)L to the communication apparatus 100 . The communication apparatus 100 changes the DS-SEQ 315 , the DC-SEQ 306 , and the C-SEQ 305 of the TCP/IP connection table 207 into E+2+G, B+2+(m+n)L, A+2+G, respectively, transmits a packet 1044 in which the TCP Flag 2911 is FIN-ACK, the PSEQ 2912 is B+1+(m+n)L, and the PACK 2913 is A+2+G to the client 603 , and transmits a packet 1045 in which the TCP Flag 2911 is FIN-ACK, the PSEQ 2912 is E+1+G, and the PACK 2913 is F+1+mL to the subsequent data transmission server 602 - 2 . Upon receiving the packet 1044 , the client 603 transmits a packet 1046 in which the TCP Flag 2911 is ACK, the PSEQ 2912 is A+2+G, and the PACK 2913 is B+2+(m+n)L to the communication apparatus 100 . Upon receiving the packet 1045 , the subsequent data transmission server 602 - 2 transmits a packet 1047 in which the TCP Flag 2911 is FIN-ACK, the PSEQ 2912 is F+1+mL, and the PACK 2913 is E+2+G to the communication apparatus 100 . Upon receiving the packet 1047 , the communication apparatus 100 changes the S-SEQ 314 of the TCP/IP connection table 207 into F+2+mL, and transmits a packet 1048 in which the PSEQ 2912 and the PACK 2913 were changed into E+2+G and F+2+mL, respectively, to the subsequent data transmission server 602 - 2 . Accordingly, the TCP connection between the client 603 and the communication apparatus 100 and the TCP connection between the communication apparatus 100 and the subsequent data transmission server 602 - 2 are terminated.
[0128] As described above, the packets are transmitted and received among the communication apparatus 100 , the server 602 , and the client 603 by the HTTP processing unit 210 and the packet generating unit 209 .
[0129] There is realized a broadband transmission module for reproduction with a device by which through transmission and reception of the packets, data corresponding to a threshold value for starting reproduction of the reception buffer is transmitted from the dedicated server in a broad band immediately after the data reproducing software instructs to reproduce the data, and then, the subsequent data is transmitted from the normal server in a normal distribution band.
[0130] FIG. 11 shows a source MAC address, a source IP address, a destination MAC address, and a destination IP address of each packet transmitted and received among the communication apparatus 100 , the server 602 , and the client 603 .
[0131] Between the client 603 and the communication apparatus 100 , communications are performed using a MAC address c and an IP address C of the client 603 , and a MAC address p and an IP address P released by the communication apparatus 100 to the client side. The MAC address and the IP address of each packet transmitted and received between the client 603 and the communication apparatus 100 are shown as a packet 1101 and a packet 1104 .
[0132] Between the server 602 and the communication apparatus 100 , communications are performed using the MAC address c and the IP address C of the client 603 , and a MAC address s and an IP address S of the server 602 . The MAC address and the IP address of each packet transmitted and received between the server 602 and the communication apparatus 100 are shown as a packet 1102 and a packet 1103 .
[0133] It should be noted that since it is assumed that the communication apparatus 100 is used in a system where plural servers 602 are present as shown in FIG. 1 , the packet generating unit 209 is provided with a device for selecting one of the MAC addresses s and the IP addresses S of plural servers 602 .
[0134] FIG. 12 shows a first example of the device for selecting one of the IP addresses of plural servers 602 . The MAC address is selected by the similar device.
[0135] The packet generating unit 209 includes a memory 1203 in which an IP address of the initial data transmission server is recorded. When the communication apparatus 100 receives the packet (the packet 1007 of FIG. 10 ) including a command for requesting a file and transmits the SYN packet (the packet 1008 of FIG. 10 ) to the initial data transmission server, first letters (8 bits) 1201 of a requested file name are input to the memory 1203 as an input address, and output data is selected as an IP address 1204 of the initial data transmission server.
[0136] Further, the packet generating unit 209 includes a memory 1207 in which an IP address of the subsequent data transmission server is recorded. When the communication apparatus 100 receives the packet (for example, the packet 1026 of FIG. 10 ) for terminating the TCP connection with the initial data transmission server and transmits the SYN packet (the packet 1027 of FIG. 10 ) to the subsequent data transmission server, first letters (8 bits) 1205 of a requested file name recorded in the file access request temporarily-recording table 206 are input to the memory 1207 as an input address, and output data is selected as an IP address 1208 of the subsequent data transmission server.
[0137] FIG. 13 shows a method of accumulating files in the servers when the IP address and the MAC address of the server are selected using the device shown in FIG. 12 .
[0138] In an initial data transmission server 1300 , a file with file name first letters A to M is accumulated, and in an initial data transmission server 1301 , a file with file name first letters N to Z is accumulated.
[0139] In a subsequent data transmission server 1302 , a file with file name first letters A to D is accumulated. In a subsequent data transmission server 1303 , a file with file name first letters E to I is accumulated. In a subsequent data transmission server 1304 , a file with file name first letters J to N is accumulated. In a subsequent data transmission server 1305 , a file with file name first letters O to R is accumulated. In a subsequent data transmission server 1306 , a file with file name first letters S to V is accumulated. In a subsequent data transmission server 1307 , a file with file name first letters W to Z is accumulated.
[0140] Although the first letters (8 bits) 1201 of the requested file name are used as an input address in the explanation related to FIG. 12 and FIG. 13 , other letters of the requested file name or a letter string representing a directory path of the requested file can be used as an input address to the memory 1203 .
[0141] FIG. 14 shows a second example of the device for selecting one of the IP addresses of plural servers 602 . The MAC address is selected by the similar device.
[0142] The packet generating unit 209 includes a hash value generating circuit 1402 and a memory 1403 in which an IP address of the initial data transmission server is recorded. When the communication apparatus 100 receives the packet (the packet 1007 of FIG. 10 ) including a command for requesting a file and transmits the SYN packet (the packet 1008 of FIG. 10 ) to the initial data transmission server, information 1401 representing a requested file name, a directory path, or a letter string representing a part thereof is input to the hash value generating circuit 1402 . Further, a hash value output from the hash value generating circuit 1402 is input to the memory 1403 , and output data is selected as an IP address 1404 of the initial data transmission server.
[0143] Further, the packet generating unit 209 includes a hash value generating circuit 1406 and a memory 1407 in which an IP address of the subsequent data transmission server is recorded. When the communication apparatus 100 receives the packet (for example, the packet 1026 of FIG. 10 ) for terminating the TCP connection with the initial data transmission server and transmits the SYN packet (the packet 1027 of FIG. 10 ) to the subsequent data transmission server, information 1405 representing a requested file name, a directory path, or a letter string representing a part thereof is input to the hash value generating circuit 1406 . Further, a hash value output from the hash value generating circuit 1406 is input to the memory 1407 , and output data is selected as an IP address 1408 of the subsequent data transmission server.
[0144] FIG. 15 shows a method of accumulating files in the servers when the IP address and the MAC address of the server are selected using the device shown in FIG. 14 .
[0145] In an initial data transmission server 1500 , a file with a hash value 0 or 1 is accumulated using the device shown in FIG. 14 , and in an initial data transmission server 1501 , a file with a hash value 2 or 3 is accumulated using the device shown in FIG. 14 .
[0146] In a subsequent data transmission server 1502 , a file with a hash value 0 is accumulated using the device shown in FIG. 14 . In a subsequent data transmission server 1503 , a file with a hash value 1 is accumulated using the device shown in FIG. 14 . In a subsequent data transmission server 1504 , a file with a hash value 2 is accumulated using the device shown in FIG. 14 . In a subsequent data transmission server 1505 , a file with a hash value 3 is accumulated using the device shown in FIG. 14 .
[0147] FIG. 16 shows a third example of the device for selecting one of the IP addresses of plural servers 602 . The MAC address is selected by the similar device.
[0148] The packet generating unit 209 includes a memory 1603 in which an IP address of the initial data transmission server is recorded. When the communication apparatus 100 receives the packet (the packet 1007 of FIG. 10 ) including a command for requesting a file and transmits the SYN packet (the packet 1008 of FIG. 10 ) to the initial data transmission server, lower 8 bits 1601 of a client IP address are input to the memory 1603 as an input address, and output data is selected as an IP address 1604 of the initial data transmission server.
[0149] Further, the packet generating unit 209 includes a memory 1607 in which an IP address of the subsequent data transmission server is recorded. When the communication apparatus 100 receives the packet (for example, the packet 1026 of FIG. 10 ) for terminating the TCP connection with the initial data transmission server and transmits the SYN packet (the packet 1027 of FIG. 10 ) to the subsequent data transmission server, lower 8 bits 1605 of a client IP address are input to the memory 1607 as an input address, and output data is selected as an IP address 1608 of the subsequent data transmission server.
[0150] It should be noted that even if the client IP address is used, a selection device for IP addresses similar to that explained in relation to FIG. 14 and FIG. 15 can be realized. The client IP address or a part thereof is input into the hash value generating circuit 1402 , a hash value output from the hash value generating circuit is input into the memory 1403 in which an IP address of the initial data transmission server is recorded, and output data is selected as an IP address of the initial data transmission server. Further, the client IP address, or a part thereof is input into the hash value generating circuit 1402 , a hash value output from the hash value generating circuit is input into the memory 1407 in which an IP address of the subsequent data transmission server is recorded, and output data is selected as an IP address of the subsequent data transmission server.
[0151] FIG. 17 shows a fourth example of the device for selecting one of the IP addresses of plural servers 602 . The MAC address is selected by the similar device.
[0152] The packet generating unit 209 includes a server load table 1701 containing n entries each of which records an IP address of an initial data transmission server and the number of TCP connections with the server, and a heap circuit 1702 which repeatedly performs an operation in which the numbers of TCP connections of adjacent entries are compared to each other to extract the entry with the smaller number and extracts the entry with the smallest number of the TCP connections. When receiving the packet (the packet 1007 of FIG. 10 ) including a command for requesting a file and transmitting the SYN packet (the packet 1008 of FIG. 10 ) to the initial data transmission server, the entry with the smallest number of TCP connections is extracted from the heap circuit 1702 , and the IP address described in the entry is selected as an IP address of the initial data transmission server. After extraction, the number of TCP connections described in the entry is incremented and the heap circuit is updated ( 1703 ).
[0153] Further, the packet generating unit 209 includes a server load table 1704 containing n entries each of which records an IP address of a subsequent data transmission server and the number of TCP connections with the server, and a heap circuit 1705 which repeatedly performs an operation in which the numbers of TCP connections of adjacent entries are compared to each other to extract the entry with the smaller number and extracts the entry with the smallest number of the TCP connections. When receiving the packet (the packet 1026 of FIG. 10 ) including a command for requesting a file and transmitting the SYN packet (the packet 1027 of FIG. 10 ) to the initial data transmission server, the entry with the smallest number of TCP connections is extracted from the heap circuit 1705 , and the IP address described in the entry is selected as an IP address of the subsequent data transmission server. After extraction, the number of TCP connections described in the entry is incremented and the heap circuit is updated ( 1706 ).
[0154] FIG. 18 shows a method of accumulating files in the servers when the IP address and the MAC address of the server are selected using the device shown in FIG. 16 or FIG. 17 .
[0155] All servers of initial data transmission servers 1800 - 1 and 1800 - 2 and subsequent data transmission server 1800 - 3 and 1800 - 4 accumulate the same file.
[0156] As a fifth example of the device for selecting one of the IP addresses of plural servers 602 , a server to be accessed may be selected in accordance with the content of a command. This method is used together with a system including an initial data transmission server 1902 and a fast-forward data transmission server 1903 as shown in, for example, FIG. 19 .
[0157] When the communication apparatus 100 receives the packet (the packet 1007 of FIG. 10 ) including a command for requesting a file and transmits the SYN packet (the packet 1008 of FIG. 10 ) to the initial data transmission server, the IP address of the initial data transmission server 1902 is selected when the content of the command is a normal file access request, and the IP address of the fast-forward data transmission server 1903 is selected when the content of the command is a digest data request.
[0158] By using the server selecting methods shown in FIG. 12 and FIG. 14 and the file accumulating methods shown in FIG. 13 and FIG. 15 , a file dispersion access module (a module for sorting a distribution request from a client into a server storing the file corresponding to the distribution request) can be realized. Further, by using the server selecting methods shown in FIG. 16 and FIG. 17 and the file accumulating method shown in FIG. 18 , a load balancing module (a module for dispersing a distribution request from a client among plural servers accumulating the same file) can be realized.
[0159] Accordingly, it is possible to provide a communication apparatus which is provided with a server arraying module including the load balancing module (a module for dispersing a distribution request from a client among plural servers accumulating the same file) and the file dispersion access module (a module for sorting a distribution request from a client into a server storing the file corresponding to the distribution request) and which includes a device for integrating resources (CPUs, I/Os, and storages) of servers into one, and a VOD distribution system including the communication apparatus and plural servers.
[0160] FIG. 20 shows an example of an extended system in which a transmission band for one connection is set for each server. Transmission bands for each one connection of servers 2000 , 2001 , 2002 , and 2003 are set to Bn (n=1 to 4). Usage of the system enables changing of the transmission band in accordance with file types.
[0161] FIG. 21 shows an example of an extended system in which a buffer amount assigned is changed or preferential transfer is controlled on the transmission apparatus side in accordance with the type of a server connected to communication apparatus. A communication apparatus 2101 includes a buffer amount preferentially-assigning module for preferentially accumulating a packet transmitted by the initial data transmission server into a buffer and a preferential transfer module for preferentially transferring a packet transmitted by the initial data transmission server. Usage of the system improves the quality of communications immediately after a file access request.
[0162] FIG. 22 shows an extended system in which a UDP is used instead of a TCP. When receiving a file access request from a client, a communication apparatus 2201 transmits the file access request to an initial data transmission server 2202 , and transmits the file access request to a subsequent data transmission server 2203 after waiting for a specified time (time specified using a value obtained by dividing the data size corresponding a threshold value for starting reproduction of the reception buffer by the normal communication band of the subsequent data transmission server). Upon receiving a request 2218 , an initial data transmission server 2202 distributes data corresponding to the reception buffer. When receiving a request 2219 , a subsequent data transmission server 2203 distributes subsequent data. Usage of the system enables data distribution using a UDP.
[0163] FIG. 30 shows a sequence diagram using a UDP.
[0164] Until data transmission is started, the communication connection is established using a TCP (the packets 1004 to 1015 ). When the communication connection with the initial data transmission server is established, initial data is transmitted from the initial data transmission server using a UDP (the packets 3016 to 3023 ). When the transmission of the initial data is completed, the communication connection with the initial data transmission server is disconnected using a TOP, and the communication connection with the subsequent data transmission server is newly established (the packets 1024 to 1034 ). When the communication connection with the subsequent data transmission server is established, subsequent data is transmitted from the subsequent data transmission server using a UDP (the packets 3035 to 3042 ). When the transmission of the subsequent data is completed, the communication connection with the subsequent data transmission server is disconnected using a TCP (the packets 1043 to 1048 ).
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An object of the present invention is to provide a communication apparatus and a data distribution system which are fast in the response speed of data distribution and require less space and less electric power. The present invention provides a communication apparatus which is provided with a broadband transmission module for reproduction by which a constant amount of data is transmitted from an initial data transmission server in a broad band immediately after a client instructs to distribute the data and then, subsequent data is transmitted from a subsequent data transmission server in a normal band, a load balancing module (a module for dispersing a distribution request from a client among plural servers accumulating the same file) and a file dispersion access module (a module for sorting a distribution request from a client into a server storing the file corresponding to the distribution request), and which includes a server arraying module for directly arraying plural servers without using a disk array to integrate resources of the servers into one. Further, the present invention provides a VOD distribution system including the communication apparatus and the plural servers.
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TECHNICAL FIELD
[0001] The present invention relates generally to methods of making nonwoven fabrics, and more particularly, to a method of manufacturing a nonwoven fabric exhibiting a durable three-dimensional image, permitting use of the fabric in floor underlayment of laminate floor systems so as to reduce acoustic feedback under normal use (walking) due to sound absorption and leveling of the floating laminate floor system applications.
BACKGROUND OF THE INVENTION
[0002] The production of conventional textile fabrics is known to be a complex, multi-step process. The production of fabrics from staple fibers begins with the carding process whereby the fibers are opened and aligned into a feedstock referred to in the art as “sliver”. Several strands of sliver are then drawn multiple times on a drawing frames to; further align the fibers, blend, improve uniformity and reduce the sliver's diameter. The drawn sliver is then fed into a roving frame to produce roving by further reducing its diameter as well as imparting a slight false twist. The roving is then fed into the spinning frame where it is spun into yarn. The yarns are next placed onto a winder where they are transferred into larger packages. The yarn is then ready to be used to create a fabric.
[0003] For a woven fabric, the yarns are designated for specific use as warp or fill yarns. The fill yarns (which run on the y-axis and are known as picks) are taken straight to the loom for weaving. The warp yarns (which run on the x-axis and are known as ends) must be further processed. The large packages of yarns are placed onto a warper frame and are wound onto a section beam were they are aligned parallel to each other. The section beam is then fed into a slasher where a size is applied to the yarns to make them stiffer and more abrasion resistant, which is required to withstand the weaving process. The yarns are wound onto a loom beam as they exit the slasher, which is then mounted onto the back of the loom. The warp yarns are threaded through the needles of the loom, which raises and lowers the individual yarns as the filling yarns are interested perpendicular in an interlacing pattern thus weaving the yarns into a fabric. Once the fabric has been woven, it is necessary for it to go through a scouring process to remove the size from the warp yarns before it can be dyed or finished. Currently, commercial high-speed looms operate at a speed of 1000 to 1500 picks per minute, where a pick is the insertion of the filling yarn across the entire width of the fabric. Sheeting and bedding fabrics are typically counts of 80×80 to 200×200, being the ends per inch and picks per inch, respectively. The speed of weaving is determined by how quickly the filling yarns are interlaced into the warp yarns, therefore looms creating bedding fabrics are generally capable of production speeds of 5 inches to 18.75 inches per minute.
[0004] In contrast, the production of nonwoven fabrics from staple fibers is known to be more efficient than traditional textile processes, as the fabrics are produced directly from the carding process.
[0005] Nonwoven fabrics are suitable for use in a wide variety of applications where the efficiency with which the fabrics can be manufactured provides a significant economic advantage for these fabrics versus traditional textiles. However, nonwoven fabrics have commonly been disadvantaged when fabric properties are compared to conventional textiles, particularly in terms of resistance to elongation, in applications where both transverse and co-linear stresses are encountered. Hydroentangled fabrics have been developed with improved properties, by the formation of complex composite structures in order to provide a necessary level of fabric integrity. Subsequent to entanglement, fabric durability has been further enhanced by the application of binder compositions and/or by thermal stabilization of the entangled fibrous matrix.
[0006] Nonwoven composite structures typically improve physical properties, such as elongation, by way of incorporation of a support layer or scrim. The support layer material can comprise an array of polymers, such as polyolefins, polyesters, polyurethanes, polyarnides, and combinations thereof, and take the form of a film, fibrous sheeting, or grid-like meshes. Metal screens, fiberglass, and vegetable fibers are also utilized as support layers. The support layer is commonly incorporated either by mechanical or chemical means to provide reinforcement to the composite fabric. Reinforcement layers, also referred to as a “scrim” material, are described in detail in U.S. Pat. No. 4,636,419, which is hereby incorporated by reference. The use of scrim material, more particularly, a spunbond scrim material is known to those skilled in the art.
[0007] Spunbond material comprises continuous filaments typically formed by extrusion of thermoplastic resins through a spinneret assembly, creating a plurality of continuous thermoplastic filaments. The filaments are then quenched and drawn, and collected to form a nonwoven web. Spunbond materials have relatively high resistance to elongation and perform well as a reinforcing layer or scrim. U.S. Pat. No. 3,485,706 to Evans, et al., which is hereby incorporated by reference, discloses a continuous filament web with an initial random staple fiber batt mechanically attached via hydroentanglement, with a second random staple fiber batt then attached to the continuous filament web, again, by hydroentanglement. A continuous filament web is also utilized in U.S. Pat. Nos. 5,144,729; No. 5,187,005; and No. 4,190,695. These patents include a continuous filament web for reinforcement purposes or to reduce elongation properties of the composite.
[0008] More recently, hydroentanglement techniques have been developed which impart images or patterns to the entangled fabric by effecting hydroentanglement on three-dimensional image transfer devices. Such three-dimensional image transfer devices are disclosed in U.S. Pat. No. 5,098,764, which is hereby incorporated by reference, with the use of such image transfer devices being desirable for providing a fabric with enhanced physical properties as well as functional dimension.
[0009] A three-dimensionally imaged nonwoven fabric must exhibit a combination of specific physical characteristics so as to be beneficial in application as a floor underlayment. For example, when such fabrics are used in flooring underlayment, the fabric must exhibit sufficient durability to withstand application upon abrasive surfaces and yet exhibit a pronounced and resilient three-dimensional pattern so as to provide proper leveling of the floating laminate floor system. Further, three-dimensionally imaged nonwoven fabrics used in industrial applications require sufficient resistance to elongation so as to resist deformation of the image when the fabric is converted into a final end-use article and when used in the final application.
[0010] Notwithstanding various attempts in the prior art to develop an acoustic underlayment for pre-finished laminate floor systems, a need continues to exist for a nonwoven fabric, which provides a pronounced image for leveling purposes, as well as sound absorption to reduce acoustic feedback.
SUMMARY OF THE INVENTION
[0011] The present invention is directed to a method of forming a nonwoven fabric, which exhibits a pronounced durable three-dimensional image, permitting use of the fabric in floor underlayment of laminate floor systems so as to reduce acoustic feedback under normal use (walking) due to sound absorption and leveling of the floating laminate floor system applications. In particular, the present invention contemplates that a fabric is formed from a precursor web comprising at least one support layer or scrim, whereby when subjected to hydroentanglement on a moveable imaging surface of a three-dimensional image transfer device, an enhanced product is achieved. By formation in this fashion, hydroentanglement of the precursor web results in a more pronounced three-dimensional image, an image that is durable to abrasion and distortion.
[0012] In accordance with the present invention, a method of making a nonwoven fabric embodying the present invention includes the steps of providing a precursor web comprising a fibrous matrix. While use of staple length fibers is typical, the fibrous matrix may comprise substantially continuous filaments. In a particularly preferred form, the fibrous matrix comprises staple length fibers, which are carded and cross-lapped to form a precursor web. In one embodiment of the present invention, the precursor web is subjected to pre-entangling on a foraminous-forming surface prior to juxtaposition of a support layer or scrim and subsequent three-dimensional imaging. Alternately, one or more layers of fibrous matrix are juxtaposed with one or more support layers or scrims, then the layered construct is pre-entangled to form a precursor web which is imaged directly, or subjected to further fiber, filament, support layers, or scrim layers prior to imaging.
[0013] The present method further contemplates the provision of a three-dimensional image transfer device having a movable imaging surface. In a typical configuration, the image transfer device may comprise a drum-like apparatus, which is rotatable with respect to one or more hydroentangling manifolds.
[0014] The precursor web is advanced onto the imaging surface of the image transfer device. Hydroentanglement of the precursor web is effected to form a three-dimensionally imaged fabric. Significantly, the incorporation of at least one support layer or scrim acts to focus the fabric tension therein, allowing for improved imaging of the staple fiber layer or layers, and resulting in a more pronounced three-dimensional image.
[0015] Subsequent to hydroentanglement, the three-dimensionally imaged fabric may be subjected to one or more variety of post-entanglement treatments. Such treatments may include application of a polymeric binder composition, mechanical compacting, application of additives or electrostatic compositions, and like processes.
[0016] A further aspect of the present invention is directed to a method of forming a durable nonwoven fabric, which exhibits a pronounced and resilient three-dimensionality, while providing the necessary resistance to abrasion and distortion, to facilitate use in a wide variety of industrial applications. The fabric exhibits a high degree of fiber retention, thus permitting its use in those applications in which the fabric is used as an underlayment for various floating floor systems. Further, the support layer or scrim aids in preventing the distortion of the imprinted image upon the application of tension to the composite fabric during routine processing and use.
[0017] A method of making the present durable nonwoven fabric comprises the steps of providing a precursor web, which is subjected to hydroentangling. The precursor web is formed into a three-dimensionally imaged nonwoven fabric by hydroentanglement on a three-dimensional image transfer device. The image transfer device defines three-dimensional elements against which the precursor web is forced during hydroentanglement, whereby the fibrous constituents of the web are imaged by movement into regions between the three-dimensional elements and surface asperities of the image transfer device. In the preferred form, the precursor web is hydroentangled on a foraminous surface prior to hydroentangling on the image transfer device. This pre-entangling of the precursor web acts to integrate the fibrous components of the web, but does not impart a three-dimensional image as can be achieved through the use of the three-dimensional image transfer device.
[0018] Optionally, subsequent to three-dimensional imaging, the imaged nonwoven fabric can be treated with a performance or aesthetic modifying composition to further alter the fabric structure or to meet end-use article requirements. A polymeric binder composition can be selected to enhance durability characteristics of the fabric or an antimicrobial additive may be used utilized to deter the growth of fungus and mold.
[0019] Other features and advantages of the present invention will become readily apparent from the following detailed description, the accompanying drawings, and the appended claims.
BRIEF DESCRIPTION OF THE DRAWINGS
[0020] [0020]FIG. 1 is a diagrammatic view of an apparatus for manufacturing a durable nonwoven fabric, embodying the principles of the present invention;
[0021] [0021]FIG. 2 is a plan view of a three-dimensional image transfer device of the type, referred to as “node”, used for practicing the present invention, with approximate dimension as shown;
[0022] [0022]FIG. 3 is a top plan photomicrograph of an nonwoven fabric having been imaged using the “node” image transfer device of FIG. 2, produced from a fibrous matrix alone utilizing a backlit light source, the magnification is approximately 10×;
[0023] [0023]FIG. 4 is a top plan photomicrograph of a nonwoven fabric having been imaged using the “node” image transfer device of FIG. 2, produced in accordance with the present invention, the magnification is approximately 10×;
[0024] [0024]FIG. 5 is top plan photomicrograph of the same fabric as in FIG. 3, wherein a top-lit light source at an incident angle of 45 degrees was used, the magnification is approximately 10×;
[0025] [0025]FIG. 6 is a top plan photomicrograph of the same fabric as in FIG. 4, wherein a top-lit light source at an incident angle of 45 degrees was used, the magnification is approximately 10×;
[0026] [0026]FIG. 7 is a side photomicrograph of the same fabric as in FIG. 3, wherein a top-lit light source at an incident angle of about 90 degrees was used, the magnification is approximately 10×; and
[0027] [0027]FIG. 8 is a side photomicrograph of the same fabric as in FIG. 4, wherein a top-lit light source at an incident angle of about 90 degrees was used, the magnification is approximately 10×;
DETAILED DESCRIPTION
[0028] While the present invention is susceptible of embodiment in various forms, there is shown in the drawings, and will hereinafter be described, a presently preferred embodiment of the invention, with the understanding that the present disclosure is to be considered as an exemplification of the invention, and is not intended to limit the invention to the specific embodiment illustrated. The present invention is directed to a method of forming a durable three-dimensionally imaged nonwoven suitable for use as acoustic underlayment for pre-finished laminate floor systems wherein the three-dimensional imaging of the fabrics is enhanced by the incorporation of at least one support layer or scrim. Enhanced imaging can be achieved utilizing various techniques. One such technique involves minimizing and eliminating tension in the overall precursor web as the web is advanced onto a moveable imaging surface of the image transfer device, as represented by co-pending U.S. patent application, Ser. No. 60/344,259 to Putnam et al, entitled Nonwoven Fabrics Having a Durable Three - Dimensional Image, and filed on Dec. 28, 2002, which is hereby incorporated by reference. By use of a support layer or scrim, enhanced fiber entanglement is achieved, with the physical properties, both aesthetic and mechanical, of the resultant fabric being desirably enhanced. It is reasonably believed that the internal support of the precursor web provided by the support layer or scrim, as the precursor web is advanced onto the image transfer device, desirably acts to focus tension to the support layer or scrim. Without tension, the fibers or filaments of the fibrous matrix, from which the precursor web is formed, can more easily move and shift during hydroentanglement, thus resulting in improved three-dimensional imaging on the image transfer device. A more clearly defined and durable image is achieved.
[0029] With reference to FIG. 1, therein is illustrated an apparatus for practicing the present method for forming a nonwoven fabric. The fabric is formed from a fibrous matrix, which typically comprises staple length fibers, but may comprise substantially continuous filaments. The fibrous matrix is preferably carded and cross-lapped to form a fibrous batt, designated F. In a current embodiment, the fibrous batt comprises 100% cross-lap fibers, that is, all of the fibers of the web have been formed by cross-lapping a carded web so that the fibers are oriented at an angle relative to the machine direction of the resultant web. U.S. Pat. No. 5,475,903, hereby incorporated by reference, illustrates a web drafting apparatus.
[0030] A support layer or scrim is then placed in face to face juxtaposition with the fibrous web and hydroentangled to form precursor web P. Alternately, the fibrous web can be hydroentangled first to form precursor web P, and subsequently, at least one support layer or scrim is applied to the precursor web, and the composite construct optionally further entangled with non-imaging hydraulic manifolds, then imparted with a three-dimensional image on an image transfer device.
[0031] [0031]FIG. 1 illustrates a hydroentangling apparatus for forming nonwoven fabrics in accordance with the present invention. The apparatus includes a foraminous-forming surface in the form of belt 10 upon which the precursor web P is positioned for pre-entangling by entangling manifold 12 . Pre-entangling of the precursor web, prior to three-dimensional imaging, is subsequently effected-by movement of the web P sequentially over a drum 14 having a foraminous-forming surface, with entangling manifold 16 effecting entanglement of the web. Further entanglement of the web is effected on the foraminous forming surface of a drum 18 by entanglement manifold 20 , with the web subsequently passed over successive foraminous drums 20 , for successive entangling treatment by entangling manifolds 24 , 24 ′.
[0032] The entangling apparatus of FIG. 1 further includes a three-dimensional imaging drum 24 comprising a three-dimensional image transfer device for effecting imaging of the now-entangled precursor web. The image transfer device includes a moveable imaging surface which moves relative to a plurality of entangling manifolds 26 which act in cooperation with three-dimensional elements defined by the imaging surface of the image transfer device to effect imaging and patterning of the fabric being formed.
[0033] The present invention contemplates that the support layer or scrim be any such suitable material, including, but not limited to, wovens, knits, open mesh scrims, and/or nonwoven fabrics, which exhibit low elongation performance. Two particular nonwoven fabrics of particular benefit are spunbond fabrics, as represented by U.S. Pat. Nos. 3,338,992; No. 3,341,394; No. 3,276,944; No. 3,502,538; No. 3,502,763; No. 3,509,009; No. 3,542,615; and Canadian Patent No. 803,714, these patents are incorporated by reference, and nanofiber fabrics as represented by U.S. Pat. Nos. 5,678,379 and No. 6,114,017, both incorporated herein by reference. A particularly preferred embodiment of support layer or scrim is a thermoplastic spunbond nonwoven fabric. The support layer may be maintained in a wound roll form, which is then continuously fed into the formation of the precursor web, and/or supplied by a direct spinning beam located in advance of the three-dimensional imaging drum 24 .
[0034] Manufacture of a durable nonwoven fabric embodying the principles of the present invention is initiated by providing the fibrous matrix, which can include the use of staple length fibers, continuous filaments, and the blends of fibers and/or filaments having the same or different composition. Fibers and/or filaments are selected from natural or synthetic composition, of homogeneous or mixed fiber length. Suitable natural fibers include, but are not limited to, cotton, wood pulp and viscose rayon. Synthetic fibers, which may be blended in whole or part, include thermoplastic and thermoset polymers. Thermoplastic polymers suitable for blending with dispersant thermoplastic resins include polyolefins, polyarnides and polyesters. The thermoplastic polymers may be further selected from homopolymers; copolymers, conjugates and other derivatives including those thermoplastic polymers having incorporated melt additives or surface-active agents. Staple lengths are selected in the range of 0.25 inch to 10 inches, the range of 1 to 3 inches being preferred and the fiber denier selected in the range of 1 to 22, the range of 1.2 to 6 denier being preferred for general applications. The profile of the fiber and/or filament is not a limitation to the applicability of the present invention.
EXAMPLES
Comparative Example 1
[0035] Using a forming apparatus as illustrated in FIG. 1, a nonwoven fabric was made by providing a precursor web comprising 100 weight percent polyester fibers. The web had a basis weight of 3 ounces per square yard (plus or minus 7%). The precursor web was 100% carded and cross-lapped, with a draft ratio of 2.5 to 1.
[0036] Prior to three-dimensional imaging of the precursor web, the web was entangled by a series of entangling manifolds such as diagrammatically illustrated in FIG. 1. FIG. 1 illustrates disposition of precursor web P on a foraminous forming surface in the form of belt 10 , with the web acted upon by an entangling manifold 12 . The web then passes sequentially over a drum 14 having a foraminous forming surface, for entangling by entangling manifold 16 , with the web thereafter directed about the foraminous forming surface of a drum 18 for entangling by entanglement manifold 20 . The web is thereafter passed over successive foraminous drums 22 , with successive entangling treatment by entangling manifolds 24 ′, 24 ′. In the present examples, each of the entangling manifolds included 120 micron orifices spaced at 42.3 per inch, with the manifolds successively operated at 100, 300, 700, and 1300 pounds per square inch, with a line speed of 45 yards per minute. A web having a width of 72 inches was employed.
[0037] The entangling apparatus of FIG. 1 further includes a three-dimensional imaging drum 24 comprising a three-dimensional image transfer device for effecting imaging and patterning of the now-entangled precursor web. The entangling apparatus includes a plurality of entangling manifolds 26 , which act in cooperation with the three-dimensional image transfer device of drum 24 to effect patterning of the fabric. In the present example, the imaging manifolds 26 were successively operated at 2800, 2800, and 2800 pounds per square inch, at a line speed which was the same as that used during pre-entanglement. A performance or aesthetic modifying composition can optionally be applied to the imaged fabric at 30 , with the fabric then dried on drying cans 32 .
[0038] The three-dimensional image transfer device of drum 24 was configured as a so-called “node” image, as illustrated in FIG. 2.
[0039] Images of the comparative material are presented in FIGS. 3, 5, and 7 .
Example 1
[0040] A three-dimensionally imaged nonwoven fabric was manufactured by a process as described in Comparative Example 1, wherein in the alternative, and in accordance with the present invention, a lighter 1.5 ounce per square yard polyester staple fiber web was juxtaposed with a 1.5 ounce polyester spunbond web of approximately 2.0 denier. The staple fiber web/spunbond web layered matrix was then subjected to equivalent hydraulic pressures as described in Comparative Example 1.
[0041] Images of the improved material of the present invention are presented in FIGS. 4, 6 and 8 .
[0042] With reference to FIGS. 3 through 8, it is apparent that the imaged nonwoven fabrics made in accordance with the present invention exhibit greater three-dimensional image clarity and are more pronounced than the image imparted to equivalent basis weight materials without the support layer or scrim. The more pronounced three-dimensional images further result in increased bulk, as is depicted in the comparison of FIG. 7 and FIG. 8. Imaged nonwoven fabrics, such as Example 1, further exhibit a significantly reduced performance, resulting in improved image retention during mechanical processing and use.
[0043] The material of the present invention may be utilized as a sound absorbent underlayment as well as provide for leveling of various floor systems, including floating laminate floor systems, and other end use products where a three-dimensionally imaged nonwoven fabric can be employed. Other end uses include; fabrication into acoustic wall systems, automotive applications, wet or dry hard surface wipes, which can be readily hand-held for cleaning and the like, protective wear for industrial uses, such as gowns or smocks, shirts, bottom weights, lab coats, face masks, and the like, and protective covers, including covers for vehicles such as cars, trucks, boats, airplanes, motorcycles, bicycles, golf carts, as well as covers for equipment often left outdoors like grills, yard and garden equipment, such as mowers and roto-tillers, lawn furniture, floor coverings, table cloths and picnic area covers.
[0044] From the foregoing, it will be observed that numerous modifications and variations can be affected without departing from the true spirit and scope of the novel concept of the present invention. It is to be understood that no limitation with respect to the specific embodiments illustrated herein is intended or should be inferred. The disclosure is intended to cover, by the appended claims, all such modifications as fall within the scope of the claims.
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The present invention is directed to a method of forming a nonwoven fabric, which exhibits a pronounced durable three-dimensional image, permitting use of the fabric in floor underlayment of laminate floor systems so as to reduce acoustic feedback under normal use (walking) due to sound absorption and leveling of the floating laminate floor system applications. In particular, the present invention contemplates that a fabric is formed from a precursor web comprising at least one support layer or scrim, whereby when subjected to hydroentanglement on a moveable imaging surface of a three-dimensional image transfer device, an enhanced product is achieved. By formation in this fashion, hydroentanglement of the precursor web results in a more pronounced three-dimensional image, an image that is durable to abrasion and distortion.
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CROSS REFERENCE TO RELATED APPLICATIONS
The present application is a continuation-in-part of copending application Ser. No. 08/819,557, filed Mar. 14, 1997 now allowed and hereby incorporated by reference herein, which is a continuation of application Ser. No. 08/449,831 filed May 24, 1995, now U.S. Pat. No. 5,674,620.
FIELD OF THE INVENTION
The invention relates to composite articles which are coated with diamond and more specifically to cutting tools made of cemented carbide which are coated with diamond by chemical vapor deposition (CVD).
BACKGROUND OF THE INVENTION
Several properties of diamond, such as its hardness and thermal conductivity, make it highly desirable for use as a coating or thin-film applied to articles whose life is limited by excessive wear, such as cutting tools. However, because diamond is a brittle material, in the form of a monolith it does not have the toughness of other traditional cutting tool materials, such as tungsten carbide or PDC (polycrystalline diamond compact). Toughness is especially important to the performance of cutting tool materials in environments where impulsive or high impact forces may be involved, for example in interrupted cutting. The use of diamond as a thin-film, or coating, takes advantage of the wear resistant properties of the thin-film while also taking advantage of the bulk properties (toughness) of an underlying substrate base material. However, in order to reduce this goal to practice, the adhesion strength of the diamond film to the underlying substrate must allow the thin-film and substrate to operate as a "composite" system. This may be particularly challenging for some base materials due to thermal expansion mismatch between the film and substrate which gives rise to very large residual stresses. In addition, the chemical composition of some base materials can impair or prevent the formation of strong bonds between the film and substrate. Ignoring these effects can lead to very weak bonding and may result in delamination of the film or coating from the base material of the substrate during use.
One of the most important base materials for various kinds of flat and rotary cutting tools is cemented carbide, such as tungsten carbide (WC) ceramic particles sintered in a matrix of cobalt (Co) binder. The utility of this class of materials is based upon the combination of a hard, abrasive phase (WC grains) which is cemented or bonded by a metal, ductile phase (Co binder). While the metal binder phase gives the cemented carbide toughness, it is this constituent which is primarily responsible for the difficulties encountered in establishing adhesion to CVD diamond films. Under typical conditions of CVD diamond synthesis, the binder phase of cemented carbides, which is commonly cobalt, but may also be iron or nickel, may interact with the gaseous CVD diamond growth species and catalyze the formation of graphitic material instead of or in addition to diamond. The formation of a graphitic layer on the substrate results in poor adhesion between the film and substrate. In addition, during the chemical vapor deposition of diamond films, the binder phase may dissolve the diamond substrate interface, thereby reducing the interfacial contact area between the film and substrate to degrade mechanical bonding. Finally, the mismatch in thermal expansion between the diamond film and substrate typically results in large residual stresses in the diamond film following deposition which further challenges the interface integrity.
Early efforts to improve the adhesion of diamond films to WC-Co materials led researchers to remove cobalt from the surface of WC-Co materials using several techniques. In U.S. Pat. No. 4,731,296, Kikuchi et al. discuss the formation of an "etch layer" with reduced cobalt concentration extending to between 0.1 to 1.0 micrometers (micrometers) into a WC-Co based substrate with 1-4 wt % (weight percent) Co. This method encourages the nucleation and growth of diamond films without the preferential deposition of graphite. However, methods based on the chemical removal of the binder phase have several drawbacks which can influence the utility of the diamond coated article. Removal of the binder phase to a depth which is greater than the general size dimension of the free surface grains results in the formation of an embrittled layer at the surface of the WC-Co article. In the presence of an applied stress, such as the residual stresses imposed on the diamond film following deposition or those encountered during use of the article, failure of the interface by loss of WC grain cohesion or by crack extension in this embrittled area results in delamination. On the other hand, removal of the binder phase to a depth which is less than the general size dimension of the free surface WC grains usually results in interaction between the diamond and binder phase unless a physical barrier to diffusion across the interface is created. Furthermore, these approaches do not have a means of producing a mechanically tough, interfacial crack deflection mechanism which is necessary to provide the interfacial fracture toughness required for the abrasive applications of metal cutting.
Other researchers have recognized that a physical barrier or so-called "diffusion barrier" to diamond/binder interaction may improve adhesion by preventing interaction between the binder phase and the diamond film. Proper selection of such a layer may also reduce residual stresses between the diamond film and the underlying substrate by selection of an interlayer material having a coefficient of thermal expansion with a value between those of the film and underlying substrate. However, the interlayer approach is not preferred because it is complicated, expensive, and does not result in the increase in interfacial toughness which other techniques achieve.
The U.S. Pat. No. 5,415, 674 issued to Feistritzer et al. discloses a technique to vaporize and re-crystallize surface WC grains. This process is a significant improvement over methods which produce a sub-surface binder-depleted region. However, this process is carried out at a temperature too low for rapid grain growth of the free surface WC grains. There is no discussion of the important details of free surface chemical composition or structural features of the free surface of the WC-Co which are necessary for adhesion of the diamond film under abrasive conditions as described above.
The U.S. Pat. No. 5,100,703 issued to Saijo discloses a process for treating WC-Co having a binder phase of 4 wt % (weight percent) or less by using a decarburizing gas comprised of oxygen and hydrogen between a temperature of 500 and 1200 C. (centigrade). While decarburization of the free surface WC grains promotes re-carburization during CVD diamond deposition and thus promotes chemical bonding between the diamond film and substrate, the method disclosed in this patent results in a free surface in which the WC grains are smaller than the WC grains in the bulk. This process therefore does not contain the crack deflection or interfacial toughening mechanism essential for highly abrasive applications.
The U.S. Pat. No. 5,648,119 issued to Grab et al. discloses the formation of a roughened substrate to improve the "mechanical component of adhesion". However, the excessive roughness of the surface described limits the utility of the diamond-coated article by resulting also in a rough surface for the diamond coating.
There is a need for a process for coating a cemented carbide article with a strongly adherent diamond film by which both the mechanical and chemical components of bonding are optimized, while at the same time the structural characteristics of the interface are designed to maximize crack deflection phenomena.
SUMMARY OF THE INVENTION
In accordance with the novel process of the present invention, a cemented carbide article has its surface treated at an elevated temperature and in an acitivated gas environment to remove some binder from the surface region, while at the same time carburizing a surface depth region of the binder remaining between exposed surface particulates. Simultaneously with the removal of binder, the particulates grow in size and undergo a change in the stoichiometry of their free surface region, which becomes somewhat depleted of carbon. When exposed to diamond growth conditions, these carbon-depleted free surface regions of the particulates are initially recarburized, and in the process of doing so form a stronger chemical bond with the deposited diamond. With the process of the invention it becomes feasible to adhere CVD diamond to WC with relatively small particulate dimensions and a low surface roughness, thus resulting in a smoother surface finish. Moreover, the resulting coated article also possesses the essential structural characteristics of the diamond/substrate interface which maximize crack deflection in order to prevent delamination of the diamond.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a schematic cross-sectional view of a fragment of a substrate of base material which has been coated with CVD diamond in accordance with one embodiment of the present invention.
DETAILED DESCRIPTION
By means of the process of the present invention, the chemical composition of the substrate/diamond interface is controlled to minimize deleterious binder phase-diamond reactions which can reduce the chemical bonding of the diamond film to the substrate and which can also induce a deleterious phase transformation of the diamond film to graphite. However, unlike techniques which remove the binder phase to some depth below the exposed WC-Co substrate surface, binder phase removal is done in a way which limits removal to only an area directly exposed to the CVD growth species, herein referred to as the "free surface."
The phase composition of the WC phase is controlled to maximize the density of direct chemical bonding between the diamond film and substrate. Unlike chemical etching methods, which de-carburize the WC grains by chemically attacking them, this decarburization is achieved without sacrificing the mechanical properties of the substrate or interface.
The process in accordance with the present invention permits control of the microstructural composition of the interface to minimize crack nucleation sites due to interfacial voids and to provide a toughening crack deflection mechanism which resists interfacial crack propagation. This feature essentially arrests or deflects cracks which may nucleate at the interface and impedes the propagation of these cracks to thereby suppress delamination of the diamond. The crack deflection mechanism is evolved without gross damage to the surface, such as results from abrading or blasting. Furthermore, the process of the present invention makes it feasible to use base material for the substrate which has a relatively small WC grain size, thereby resulting in a much smoother diamond coating surface, since the diamond coating surface profile tends to mirror that of the underlying substrate surface.
GENERAL FEATURES OF THE PROCESS
In accordance with the invention, an article 10, a fragment of which is shown in cross-seciton in FIG. 1 composed of commercially available WC-Co in its bulk region 12 with up to 10 wt % Co and having an average particle size in the range of from about 0.25 mm (millimeters) to 1.0 mm is sintered to form a cemented carbide article. The article may then be ground to a final desired geometry, which may include chip-forming or other complex surface features. The article is then treated at an elevated temperature in the presence of activated hydrogen, hydrocarbon, or inert gas in order to simultaneously a) vaporize the free surface binder phase, b) induce growth of the WC grains at the free surface, and c) shift the stoichiometery of the free surface WC grains to a carbon-deficient ratio without formation of the of the brittle eta phase of WC (M 6 C, M 12 C). The free surface thus produced is microstructurally roughened and cobalt-free, and the WC phase is de-carburized (with respect to bulk WC grains). An important feature of the process is that the WC grains within the bulk 12 are left essentially un-altered by the process. The substrate is then coated with a diamond film 16 of between 5 and 50 micrometers thick under temperature and time conditions which limit diffusion of the binder phase from a surface depth region 14 to the interface.
The novel process leaves the free surface of the substrate essentially free of the cobalt binder phase, as confirmed by analytical techniques such as energy dispersive spectroscopy (EDS). The removal of the binder phase from the free surface occurs through two mechanisms: a) some diffusion of cobalt atoms into the WC grains and b) vaporization and entrainment of the binder phase by process gases. Raising the temperature of the WC-Co material shifts the gas-liquid-solid equilibrium and produces a partial pressure of the metallic binder phase above the tool. Entraining this vapor by using an inert gas such as nitrogen or argon enables more surface cobalt to be vaporized. If the rate of vaporization is greater than the bulk-to-surface diffusion rate, the free surface will be essentially free of the binder phase. The temperature at which this process is carried out is a function of gas composition and gas velocity rate. For instance, if a dissociated hydrogen gas is used, vaporization occurs at a temperature below the standard melting point temperature of pure Co, which is 1495 degrees C. However, if nitrogen is used, the rapid grain growth and vaporization occurs at a temperature at or above the melting point temperature. At temperatures above the melting point of the binder phase, the growth process occurs rapidly. However, temperatures below the melting point temperature may be preferred to minimize any gravity-induced deformation of the article in its relatively soft state during processing.
During the early stages of the process, the WC grains at the free surface undergo common Ostwald ripening and re-crystallization. Following this, continued mass transport of W and C atoms result in grain-growth of the WC phase. However, while the conditions at the free surface support rapid grain growth of the surface WC grains, the grains within the bulk material grow at a much slower rate. For this reason, the important mechanical advantages of a fine-grained WC-Co material are retained within the bulk material. Under continued processing, the stoichiometery of the individual WC grains at the free surface is shifted in such a way that a stoichiometeric gradient exists on individual grains. Continued treatment or annealing under these conditions would eventually lead to the formation of the brittle eta-phase, which is a carbon-deficient W-C-Co phase, by essentially reducing the carbon concentration of WC grains at the free surface. The vaporization grain growth thermal de-carburization process of the present invention may be achieved under a range of processing conditions by varying time and temperature appropriately.
Following the evolution of the surface microstructure and chemical composition as described above, the surface is coated with a diamond film. During the initial stage of the CVD diamond nucleation or incubation period, carbon source gas re-carburizes the free surface WC grains and thus promotes direct chemical bonding between the diamond film and the WC grains at the interface. Diamond growth is thereby achieved under conditions which suppress bulk-to-interface diffusion of the binder phase.
EXAMPLE 1
A commercially available WC-Co cutting tool insert with 6 wt % Co binder, an average grain size of 0.5-1.0 mm, and a ground free surface was placed in a commercially-available vacuum-sintering graphite furnace. The sample was placed on a bed of graphite and SiC particles. The graphite was in the form of a graphite paint which covers a layer of SiC particulates. The graphite is present to suppress the formation of eta phase material. The SiC particles form a barrier between the insert and any supporting kiln furniture to prevent fusion of the insert to such furniture. The sample was heated to a temperature of 1560 deg. C. (Centigrade) in the presence of flowing nitrogen under a pressure of 0.30 torr for approximately 45 minutes and cooled to room temperature. The exact time, temperature and carbon concentration of the binder phase were controlled to promote the vaporization of the binder phase and the growth and de-carburization of the WC phase. These parameters are a function of batch size and geometry of the item being processed and can be readily ascertained by those skilled in the art. Following treatment, the free surface of the WC-Co article was characterized by EDS (energy dispersive spectrometery), XRD (x-ray diffraction), and SEM (scanning electron microscopy). EDS revealed the presence of W and the absence of Co at the surface. XRD revealed Co and WC with no formation of eta phase material. SEM showed free surface grain growth in the WC phase by extension of prismatic planes. The part was then coated with a 30 mm thick diamond film and tested by machining Reynold's A390 aluminum stock at 2500 surface feet per minute, 0.005 inches per revolution, and 0.025 inches depth of cut. The tool life was approximately 50% that of a PDC-tipped cutting tool insert subjected to a similar test. The tool failed by excessive wear, but not by delamination of the diamond film.
EXAMPLE 2
A commercially-available WC-Co cutting tool insert having 6 wt % Co, an average grain size of 0.5 mm-1.0 mm, and a ground free surface was placed in a dc arc-jet CVD diamond deposition system. The sample was placed in a holder which allows for accurate control of temperature and processing conditions during deposition as described in copending patent application Ser. No. 08/473,198 of J. Olson filed Jun. 7, 1995, entitled SPINNING SUBSTRATE HOLDER FOR CUTTING TOOL INSERTS FOR IMPROVED ARC-JET DIAMOND DEPOSITION and assigned to the same assignee as is the present invention. In the presence of dissociated hydrogen, the sample was heated to a temperature of between 1200° C. and 1350° C. in a pressure of about 5 torr. The surface of the WC-Co cutting tool insert was maintained in these conditions for a period of about 0.5 hours, during which a low concentration (approximately 0.10%) of methane was cycled on and off at 5 minute intervals. Diffusion transport (gettering) of the vaporized binder phase was controlled by the presence of a low temperature sink in close proximity to the processing inserts. The free surface was characterized by EDS, XRD and SEM as described above. EDS revealed the presence of W and absence of Co at the surface. XRD revealed Co and WC with no formation of the eta-phase. SEM showed free surface grain growth in the WC phase by extension of prismatic planes. The gas phase carbon, which is necessary to suppress the formation of eta-phase material, may also be supplied as a solid source by placing graphite in the pockets of the holder, for instance.
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A process for coating a tungsten carbide base material substrate with CVD diamond film includes carburization and gas-assisted vaporization of cobalt from the surface with simultaneous recrystallization of surface grains of tungsten carbide to change their stoichiometry for improved adherence.
Also disclosed is a WC-Co cutting tool having a relatively fine WC grain size and coated with adherent CVD diamond.
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This is a continuation, of application Ser. No. 930,612 filed Aug. 3, 1978, now abandoned.
BACKGROUND OF THE INVENTION
Because of the increasing shortage of raw material resources and the raw material price increases resulting therefrom, processes for working up plastic consumer articles which are no longer useful, in the sense of recovery either of starting substances or the original plastic directly, are becoming more and more important.
Thus, in German Democratic Republic Patent Specification Nos. 45,575, 46,282, 45,599, 45,600 and 46,353, E. Bullack describes a process for the working up of polycarbonates, in particular with regard to the isolation of 4,4'-dihydroxy-diaryl-alkanes as starting substances for polycarbonate syntheses.
According to German Democratic Republic Patent Specification Nos. 45,575, 46,282 and 45,599, the 4,4'-dihydroxy-diaryl-alkanes are obtained, after purification processes which in some cases are expensive, via cleavage by means of alcohols, acid anhydrides or small amounts of basic catalysts. According to Patent Specification Nos. 45,600 and 46,353, the cleavage is achieved by adding phenols or diaryl carbonates in the presence of metal oxide catalysts at temperatures above 180° C. There is the danger of side reactions at these temperatures, especially if metal oxide catalysts are present, and extensive purification operations are necessary in order to isolate clean starting substances.
SUMMARY OF THE INVENTION
The present invention relates to a process for the recovery of aromatic, high-molecular weight, thermoplastic polycarbonates from polycarbonate scrap, which is characterized in that the polycarbonate strap is saponified in bulk or in solution at temperatures between about 25° C. and 220° C., the non-saponified constituents are then separated off and the saponification mixture is then phosgenated and subjected to polycondensation by the two-phase boundary polycondensation methods, without further purification steps and treatment steps.
DETAILED DESCRIPTION OF THE INVENTION
It has now been found, surprisingly, that it is possible to gently saponify polycarbonates, either in the pure or colored form or in the form of polymer blends, in a one-pot reaction which proceeds smoothly, and, if appropriate after filtering off additives, dyestuffs and the like constituents of the blend, then to phosgenate the products again in a smooth one-pot reaction in the same reaction media to give high-molecular weight, thermoplastic and soluble polycarbonates. Polycarbonates have thus been cleaved without adding catalysts which are troublesome later and under mild conditions with respect to heat, and the reaction mixture which remains after the cleavage can be directly reacted again, without intermediate purification, by the phase boundary process, in order to synthesize polycarbonates.
After adding a water-immiscible solvent which is customary in the phase boundary condensation of polycarbonates, such as, for example, methylene chloride or chlorobenzene, the condensation reaction can be carried out directly, by passing in phosgene, without any intermediate purification. The pH value of the alkaline phase should be kept between about 9 and 14 during this procedure, depending on the nature of the diphenol. Tertiary amines, such as, for example, triethylamine, tributylamine or N-alkylpiperidine, or ammonium, sulphonium, phosphonium or arsonium compounds or also nitrogen-hetaryls, such as, for example, pyridine, are usually added before, and especially after, the phosgenation.
After the saponification step, the monohydric phenols present in scrap polycarbonates at the chain ends are found as cleavage products in the alkaline reaction medium and are again incorporated completely as chain stoppers during or after the phosgenation, so that the resynthesized polycarbonates attain the same solution viscosity as the polycarbonate scrap reacted as the starting material. If other soluble viscosities are to be established, an additional amount of free bisphenol can be metered in for a higher desired solution viscosity, and an additional amount of monohydric phenol can be metered in for a lower solution viscosity.
Cocondensed compounds with more than two functional groups capable of undergoing condensation, such as, for example, trisphenols or tetraphenols, which are incorporated as branching agents into polycarbonates, are also incorporated again completely during the resynthesis of the polycarbonates. A change in the branching agent concentration in the recovered polycarbonate is again made possible by adding an additional amount of branching agent or of free bisphenol to the reaction medium before the phosgenation.
Polycarbonate strap is to be understood as all polycarbonate plastic articles which can no longer be used, and also the residues, scrap, trimmings and the like obtained during the preparation and shaping of the polycarbonate plastic.
The polycarbonate scrap suitable for reuse results from aromatic homopolycarbonates and copolycarbonates, which are based, for example, on one or more of the following diphenols: hydroquinone, resorcinol, dihydroxydiphenyls, bis-(hydroxyphenyl)-alkanes, bis-(hydroxyphenyl)-cycloalkanes, bis-(hydroxyphenyl)sulphides, bis-(hydroxyphenyl)ethers, bis-(hydroxyphenyl) ketones, bis-(hydroxyphenyl) sulphoxides, bis-(hydroxyphenyl) sulphones, α,α'-bis-(hydroxyphenyl)diisopropylbenzenes and, for example, their nuclear-halogenated compounds. These and further suitable diphenols are described, for example, in U.S. Pat. No. 3,028,365, incorporated herein by reference, and in the monograph "H. Schnell, Chemistry and Physics of Polycarbonates, Interscience Publishers, New York, 1964".
Examples of preferred diphenols are: 4,4'-dihydroxydiphenyl, 2,2-bis-(4-hydroxyphenyl)-propane (bisphenol A), 2,4-bis-(4-hydroxyphenyl)-2-methylbutane, 1,1-bis-(4-hydroxyphenyl)-cyclohexane, α,α'-bis-(4-hydroxyphenyl)-p-diisopropylbenzene, 2,2-bis-(3-chloro-4-hydroxyphenyl)-propane, 2,2-bis-(3,5-dichloro-4-hydroxyphenyl)-propane and 2,2-bis-(3,5-dibromo-4-hydroxyphenyl)-propane.
The aromatic polycarbonates which can be reused as polycarbonate scrap can also be branched by incorporating small amounts, preferably amounts between about 0.05 and 2.0 mol % (relative to diphenols employed), of compounds which are trifunctional or more than trifunctional, in particular those with three or more than three phenolic hydroxyl groups, for example by incorporating phloroglucinol, 1,3,5-tri-(4-hydroxy-phenyl)-benzene, 1,1,1-tri-(4-hydroxyphenyl)-ethane or 1,4-bis-(4,4'-dihydroxytriphenyl-methyl)benzene.
As a rule, the aromatic polycarbonates which can be reused as polycarbonate scrap have average weight average molecular weights Mw of about 10,000 to over 200,000, preferably of about 20,000 to 80,000, determined by measurements of the relative viscosity in CH 2 Cl 2 at 25° C. and at a concentration of 0.5% by weight.
The molecular weights of the polycarbonates can be regulated in the customary manner, for example by incorporating phenol, tribromophenol or p-tert.-butylphenol.
The polycarbonates which can be reused from polycarbonate scrap can also be in the form of mixtures of different polycarbonates, for example mixed with proportions of low-molecular polycarbonates, or can also be in the form of polymer blends, for example with polymers or copolymers based on styrene, styrene/acrylonitrile, acrylonitrile/butadiene/styrene or butadiene rubber.
The polycarbonate scrap is saponified in bulk or in solution, the solvents used being the customary solvents which are suitable for the preparation of polycarbonates by the two-phase boundary process, such as methylene chloride or chlorobenzene.
The saponification is carried out in a neutral, but preferably alkaline, aqueous reaction medium, the saponification in bulk being effected heterogeneously and the saponification in solution being effected at the boundary of the two-phase system, the latter proceeding more favourably and rapidly. With respect to the aqueous reaction medium there are preferably used between 25 and 100 moles of water per mol of structural polycarbonate unit to be saponified.
Examples of basic saponification agents which can be used are sodium hydroxide, potassium hydroxide and calcium oxide, preferably sodium hydroxide.
The saponification is carried out at temperatures between about 25° and 220° C., optionally applying excess pressure, preferably up to about 100 atmospheres.
The amount of basic saponification agents is between about 0.01 and 15 times the molar amount, relative to the mols of aromatic hihydroxy compound formed; the pH value of the saponification medium is between about 9 and 14; and the saponification time is between about 0.5 and a maximum of 20 hours, depending on the steric shielding of the carbonate structure.
Phosphites or phosphines can additionally be added as catalysts.
If the polycarbonate scrap contains unsaponifiable constituents, such as lubricants, stabilizers, pigments, dyestuffs and fillers, such as glass powder, quartz products, graphite, molybdenum sulphide, metal powders, powders of higher-melting plastics, such as p-lytetraethylene powder, natural fibers, such as asbestos, and furthermore glass fibers of the most diverse nature, metal filaments and the like, after the saponification has been carried out, these are separated off in a known manner, for example by filtration.
The single-phase or two-phase solutions resulting after the saponification of the polycarbonate scrap can be employed directly for the preparation of polycarbonates by the phase boundary process, the customary polycarbonate solvents, such as methylene chloride or chlorobenzene, being appropriately added and the pH value of the aqueous solution being adjusted to between about 9 and 14, depending on the requirement.
The subsequent phosgenation is usually carried out at room temperature, an amount of phosgene of about 1 to 3 mols, relative to 1 mol of diphenol, preferably being employed.
The phosgenation time is a maximum of about 1 hour.
Tertiary amines or other polycondensation catalysts are added in amounts between about 0.01 to 10 mol %, relative to the mols of diphenols, before, or especially after, the phosgenation.
The polycondensation reaction is then carried out in the customary manner at temperatures between about 20° and 40° C. for a period of about 1-5 hours, depending on the diphenol employed.
The polycarbonate solutions obtained are worked up in the customary manner and the polycarbonate is isolated in the customary manner.
EXAMPLES
EXAMPLE 1
25.4 g of a polycarbonate obtained from 2,2-bis-(4-hydroxyphenyl)-propane and having a solution viscosity η rel =1.288 (measured on a solution of 0.5 g of polycarbonate in 100 ml of methylene chloride) are added, in the form of granules, to 80 ml of 15 N sodium hydroxide solution. The reaction mixture is heated to 100° C. for 4 hours. In this time, complete cleavage of the polycarbonate down to the monomer unit bisphenol A is achieved. If 500 ml of distilled water are added to the resulting suspension, a clear alkaline solution of bisphenol A is obtained which, after adding 500 ml of methylene chloride, can be phosgenated by the customary phase boundary condensation methods.
For this, 15 g of phosgene are passed in at 25° C. in the course of 1 hour, the pH value being adjusted to 13-14, and, after adding 1.5 mol of a 4% strength aqueous triethylamine solution, the condensation reaction is then carried out for a further 1 hour. The organic phase is separated off and washed twice with 2% strength phosphoric acid and then with distilled water until free from electrolytes. After evaporating off the solvent, 24 g of polycarbonate are obtained with a θ rel =1.295. The recyclized polycarbonate exhibits mechanical and rheological properties which are equally as good as those of the starting material.
EXAMPLE 2
25.4 g of the polycarbonate of Example 1, obtained from 2,2-bis-(4-hydroxyphenyl)-propane are added, in the form of granules, to 30 ml of 15 N sodium hydroxide solution. 2.5 g (10% by weight) of triphenyl phosphite are also additionally added, and saponification is then carried out at 100° C. according to Example 1. By adding the phosphite, the time until saponification is complete is shortened to 2 hours 45 minutes. Thereafter, phosgenation is carried out at the phase boundary analogously to Example 1. The polycarbonate recovered has a solution viscosity η rel =1.297 and, after precipitation from the methylene chloride solution by means of methanol, exhibits no difference from the starting material with respect to the mechanical and rheological properties.
EXAMPLE 3
25.4 g of the polycarbonate according to Example 1, obtained from 2,2-bis-(4-hydroxyphenyl)-propane are dissolved in 300 ml of chlorobenzene, and 80 ml of 15 N sodium hydroxide solution are added as the alkaline phase. The mixture was brought to 100° C. and the content of polycarbonate still not saponified in the organic phase was examined at short intervals of time. The cleavage had completely ended after 60 minutes, and the phase boundary mixture could be phosgenated directly analogously to Example 1, after adding 350 ml of water, and the phosgenation mixture then subsequently worked up. 23.5 g of a polycarbonate are obtained with a η rel of 1.315 and a similar pattern of properties to the starting material.
By adding 450 mg of p-tert.-butylphenol to the saponification mixture as an additional chain stopper, the solution viscosity η rel =1.282 can be obtained after the phosgenation and condensation reaction.
EXAMPLE 4
The saponification time and amount of the base employed are directly related. As this example shows, the amount of sodium hydroxide employed can be reduced at the expense of extended saponification times. The saponification was carried out at the phase boundary: 25.4 g of the polycarbonate of Example 1 were dissolved in 300 ml of chlorobenzene and varying amounts of 15 N sodium hydroxide solution were added. In each case the time until the saponification of the polycarbonate was complete was measured:
25.4 g of the polycarbonate from Example 1 in 300 ml of chlorobenzene and 80 ml of 15 N NaOh results in a saponification time of 55 minutes; in 300 ml of chlorobenzene and 63 ml of 15 N NaOH in a saponification time of 70 minutes; in 300 ml of chlorobenzene and 46 ml of 15 N NaOH in a saponification time of 120 minutes and in 300 ml of chlorobenzene and 33 ml of 15 N NaOH in a saponification time of 260 minutes.
EXAMPLE 5
The saponification can also be carried out under pressure. 101.6 g of the polycarbonate of Example 1, 400 ml of distilled water and 2.26 g of 45% strength sodium hydroxide solution are heated to 210° C. under pressure of 50 bars in an autoclave in the course of 1 hour and kept under these conditions for 2 hours. 840 g of 6.2% strength sodium hydroxide solution and 1,500 ml of methylene chloride are added to the resulting mixture. 60 g of phosgene are passed in during the course of 1 hour while maintaining a pH value of 13-14, and, after adding 6 ml of 4% strength aqueous triethylamine, the condensation reaction is then carried out for 1 hour. The reaction mixture is worked up according to Example 1. Since it is probable that small amounts of monofunctional monomers are split off during the saponification under pressure, the solution viscosity of the resulting polycarbonate is η rel =1.212. A polycarbonate having the desired η rel =1.287 can be obtained by additionally adding 17 g of bisphenol A to the saponification mixture and correspondingly increasing the proportions of phosgene and triethylamine.
EXAMPLE 6
80 ml of 15 N sodium hydroxide solution are added to 27.9 g of a polycarbonate based on bisphenol A (η rel =1.305) containing 10% by weight of glass fibers and the mixture is warmed to 100° C. The saponification has ended after 3 hours. 500 ml of distilled water are added to the saponification mixture and the glass fibers which remain are filtered off. 500 ml of methylene chloride are added to the filtrate, and 15 g of phosgene are then added to the mixture analogously to Example 1 and after adding 1.5 ml of a 4% strength aqueous triethylamine solution the mixture is subjected to a condensation reaction. After working up according to Example 1, 10 g of a glass fiber-free polycarbonate are obtained, η rel =1.317.
The polycarbonate exhibits the same pattern of properties as a polycarbonate of corresponding chain length which has been obtained by customary condensation of bisphenol A and phosgenation by the phase boundary process.
EXAMPLE 7
80 ml of 15 N sodium hydroxide solution are added to 25.4 g of a polycarbonate which is based on bisphenol A, has a solution viscosity η rel =1.367 and contains 0.2 mol %, relative to the proportions of diphenols of the tetrafunctional branching agent 1,4-bis-(4,4'-dihydroxytriphenyl-methyl)benzene incorporated therein, and the mixture is kept at 100° C. for 3 hours. Thereafter, 500 ml of distilled H 2 O are added until a clear solution is formed and 500 ml of methylene chloride are then added. 15 g of phosgene are added to the saponification mixture analogously to Example 1 and the mixture is subjected to a condensation reaction with 1.5 ml of a 4% strength aqueous triethylamine solution. A polycarbonate is obtained by the customary working up methods, which has a solution viscosity η rel =1.375 and, after cleavage and investigation of the monomer constituents by chromatography, contains 0.2 mol % of the tetrafunctional branching agent.
EXAMPLE 8
36.3 g of a polymer blend which is composed of 30% by weight of an ABS polymer and 70% of a polycarbonate based on bisphenol A (η rel =1.292) are treated with 120 ml of 15 N sodium hydroxide solution at 100° C. for 10 hours. Thereafter, the mixture is mixed with 500 ml of distilled H 2 O and the undissolved ABS polymer is filtered off. 500 ml of methylene chloride are then also added to the filtrate and 11 g of phosgene are passed in at room temperature in the course of 1 hour and, after adding 1.5 ml of a 4% strength aqueous triethylamine solution, the condensation reaction is carried out for a further 1 hour. 17 g of the high-molecular, thermoplastic polycarbonate with a solution viscosity η rel =1.305 are obtained by the customary working up methods.
EXAMPLE 9
80 ml of sodium hydroxide solution are added to 25.4 g of a polycarbonate based on bisphenol A (η rel % 1.285), dyed red with 0.35% by weight of cadmium selenide, and the mixture is warmed to 100° C. for 3 hours. Thereafter, the mixture s mixed with 500 ml of distilled H 2 O and the undissolved colored pigment is filtered off. 500 ml of methylene chloride are added to the clear filtrate and the phase boundary mixture is phosgenated and worked up, as in Example 1. 22 g of a non-dyed, thermoplastic polycarbonate remain with a solution viscosity η rel =1.297.
EXAMPLE 10
27 g of a copolycarbonate based on bisphenol A and tetrabromo-bisphenol A (5.3% by weight of bromine) (η rel =1.297) are dissolved in 150 ml of chlorobenzene, and 80 ml of 15 N sodium hydroxide solution are metered in. After 4 hours, the saponification has ended and, after adding 350 ml of methylene chloride and 400 ml of water, a clear phase mixture is obtained. In order to recover the polycarbonate, 15 g of phosgene are passed in at room temperature in the course of 1 hour. At the end of the phosgenation, the solution should have a pH value of abot 11-12. After adding 0.43 ml of triethylamine, the condensation reaction is carried out for a further 1 hour and the mixture is worked up according to Example 1. A bromine-containing polycarbonate results (5.4% of bromine) with a solution viscosity η rel =1.285 and similar properties to the starting material.
Although the invention has been described in detail for the purpose of illustration, it is to be understood that such detail is solely for that purpose and that variations can be made therein by those skilled in the art without departing from the spirit and scope of the invention except as it may be limited by the claims.
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The present invention relates to a process for the recovery of aromatic, high-molecular weight, thermoplastic polycarbonates from polycarbonate scrap, it being possible for the polycarbonate scrap to be either in the pure form as transparent naturally-occurring material, or mixed together with organic and, especially, inorganic dyestuffs and/or other additives, or in the form of a blend with other thermoplastic materials.
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FIELD OF THE INVENTION
[0001] The invention disclosed broadly relates to the field of information handling systems and more particularly relates to the field of querying data documents such as Extensible Markup Language (XML) documents.
BACKGROUND OF THE INVENTION
[0002] “Extensible Markup Language” (XML) is a textual notation for a class of data objects called “XML Documents” and partially describes a class of computer programs processing them. A characteristic of XML documents is that they use a hierarchical structure to organize information within the documents. This hierarchical structure may be represented using a rooted-tree data structure with node representing the “elements” of the XML document. Element nodes have a tag name, may be associated with named attributes, and may have relationships to other nodes in the tree, where such relationships may refer to “parent” and “child” nodes. In addition, element nodes may contain data in various forms (specifically text, comments, and special “processing instructions”).
[0000] XML Document Trees.
[0003] An XML document can be represented as a labeled tree whose nodes represent the structural components of the document—elements, text, attributes, comments, and processing instructions. Element and attribute nodes have labels derived from the corresponding tags in the document and there may be more than one node in the document with the same label. Parent-child edges in the tree represent the inclusion of the child component in its parent element, where the scope of an element is bounded by its start and end tags. The tree corresponding to an XML document is rooted at a virtual element, called the root, which represents the document itself. Hereinafter, XML documents will be discussed in terms of their tree representations. One can define an arbitrary order on the nodes of a tree. One such order might be based on a left-to-right depth-first traversal of the tree, which, for a tree representation of an XML document, corresponds to the document order. The memory footprint of an XML document can be large. XML processors may not be able to handle large documents due to the memory requirement of storing the entire document. As a result, in processing XML, reducing the memory overhead of an XML document is of great importance.
[0000] XPath.
[0004] “XML Path Language” (XPath) is a query language for creating an expression that selects nodes of data from an XML document. XPath is used to address XML data using path notation to navigate through the hierarchical structure of an XML document. XPath queries allow applications to determine if a given node matches a pattern, including patterns involving its location in the XML document hierarchy.
[0005] XPath has been widely accepted in many environments, especially in database environments. Given the importance of XPath as a mechanism for querying and navigating data, it is important that the evaluation of XPath expressions on XML documents be as efficient as possible.
[0000] XPath Axes.
[0006] Given an order on a tree, we can define a notion of a forward and backward relation on a tree. A relation R is a forward relation if whenever two nodes x and y are related by R, x precedes y in the order on the tree. Similarly, a relation is a backward relation whenever x is related to y, x follows y in the order on the tree. For example, assuming the document order for a tree representation of an XML document, the child and descendant relations are both forward relations, whereas the parent and ancestor relations are both backward relations.
[0007] An XPath expression over the tree representation of an XML document is evaluated in terms of a context node. The context node is a node in the tree representation of the document, and is well known to those of skill in the art of XML. If the context node is the root node of the document, the XPath expression is said to be an absolute XPath expression, otherwise, it is known as a relative XPath expression. Starting at a context node, an XPath expression specifies the axis to search and conditions that the results should satisfy. For example, assume that the context node is an element node c in the tree representation of an XML document. The XPath expression “descendant::x” specifies a descendant axis, where searching begins at the context node, and produces a sequence of all element nodes that are descendants of the node c and are labeled “x”. One can combine XPath expressions to form larger XPath expressions. For example, the XPath expression “descendant::x/ancestor::y” specifies that starting from the context node c, find all element nodes that are descendants of c with label x, and for each such node, find all ancestor nodes with label y.
[0000] XML Processing.
[0008] In traditional XML processing, a tree representation of an XML document that is to be processed is built in memory. When the document is large, this construction of the tree representation, for example, as an instance of the familiar Document Object Model (DOM), may be prohibitively expensive in both time and memory. For large documents, XML processing may fail due to the large memory requirements of the document. In main-memory XML processors, one of the primary sources of overhead is the cost of constructing and manipulating main-memory representations of XML documents.
[0009] The cost of construction of an in-memory data model instance of an XML document can be reduced significantly if only those portions that are relevant to the processing are instantiated. This insight is the basis for projection, an optimization introduced by Marian and Simeon. See Marian and Simeon, Projecting XML Documents, Proceedings of the 29 th VLDB Conference, Berlin, Germany (2003). Given a set of XPath expressions and an XML document, a projected document is constructed such that the result of the execution of the set of XPath expressions on the projected document is the same as that of the execution of the set on the original document. For example, FIG. 1 depicts the tree representation of an XML document; the boxes in the figure with thick borders denote its projection with respect to the XPath expression “//Title”, which selects for the projection all elements with the tag “title” in the document, in this case, elements 140 and 180 . The projected document is usually substantially smaller than the original document. As a result, the in-memory construction time is lower than it might be otherwise. Moreover, as a side-effect, the smaller size of the projected document results in lower query evaluation times on the projected document than a similar evaluation on the original document. The root node of the tree is root 100 . A “catalog” 110 is the next node. One branch begins at node 120 and another at node 160 . The “book” nodes 130 and 170 begin another pair of sub-branches: a branch under “book” 130 includes “title” 140 and “compilers” 150 and the branch under “title” 180 includes the “algorithms” node 190 .
[0010] The drawback to current techniques of projection is that they cannot handle complex XPath expressions. Current techniques are only defined for queries using child and descendant axes—other XPath axes such as parent and ancestor are not supported by the current schemes. Therefore, a need exists to overcome the problems with the prior art as discussed above, and particularly, for a way to project XML documents efficiently when XPath expressions contain axes other than child and descendant.
SUMMARY OF THE INVENTION
[0011] Briefly, according to embodiments of the invention, a method, computer readable medium, and apparatus (system) for constructing a projected representation of a document in the Extensible Markup Language (XML) format with respect to a set of expressions in XPath or other query language through approximate matching. The method of the present system supports all XPath axes, including backward axes and predicates.
[0012] The subject matter, which is regarded as the invention, is particularly pointed out and distinctly claimed in the claims at the conclusion of the specification. The foregoing and other features, and also the advantages of the invention, will be apparent from the following detailed description taken in conjunction with the accompanying drawings. Additionally, the left-most digit of a reference number identifies the drawing in which the reference number first appears.
BRIEF DESCRIPTION OF THE DRAWINGS
[0013] FIG. 1 illustrates a tree representation of an XML document.
[0014] FIG. 2 illustrates one possible system architecture for a system according to an embodiment of the invention.
[0015] FIG. 3 illustrates a tree representation of an XPath expression in an embodiment of the present invention.
[0016] FIGS. 4-8 illustrate various rules for rewriting edges, in an embodiment of the present invention.
[0017] FIG. 9 illustrates an information processing system implementing an embodiment of the present invention.
DETAILED DESCRIPTION
[0018] We describe a method, computer readable medium, and information processing system for projecting a representation of a document in the XML format based on a set of XPath expressions, where the XPath expressions may involve use of both forward and backward axes.
[0000] Tree Model of XML Documents.
[0019] An XML document may be represented as a tree whose nodes represent the structural components of the document—elements, text, attributes, and the like. Parent-child edges in the tree represent the inclusion of the child component in its parent element, where the scope of an element is bounded by its start and end tags. The tree corresponding to an XML document is rooted at a virtual element, root, which contains the document element. A system according to an embodiment uses XML documents in terms of their tree representation; we will use “D” to denote an XML document, and N D and E D denote its nodes and edges respectively. For simplicity, the description focuses on XML elements, though one of ordinary skill in the art will be aware that the implementation can also handle the other XML nodes, such as attribute nodes. We assume that the following functions are available for the elements in an XML document:
[0020] id D : N D →Integer: Returns a unique identifier for each element in a document We assume that id D is a total order on the elements in D, such that the assignment of identifiers to elements corresponds to a depth-first preorder traversal of the tree (corresponds to document order in XML).
[0021] tag D : N D →String: Returns the tag name of the element.
[0022] level D : N D →Integer: Returns the distance of the element from the root, where level D (root)=0.
[0023] We also define functions, child D , desc D , self D , fs D , and following D , each with the signature N D ×N D →{true, false}. The semantics of these functions is straightforward, child D (v1, v2) returns true if v2 is a child of v1 in D, and fs D (v1, v2) returns true if v1 and v2 share a common parent, and moreover, id D (v1)<id D (v2). Following D (v1, v2) returns true if id D (v2)>id D (v1) and v2 is not an ancestor of v1. Finally, self D (v1, v2) returns true if v1=v2.
[0000] System Architecture
[0024] The architecture of our system is depicted in FIG. 2 . A client provides a query (or set of queries) 200 that must be evaluated against document 250 (or set of documents) to Query Processor 210 . The query processor derives a set of XPath expressions 230 from this set and passes it to the Projector 220 . The Projector 220 constructs a representation of the input document based on the set of XPath expressions 230 . A reference to the root of document 240 is returned to the query processor. The query processor then evaluates the query over projected document 240 and serializes results 260 back to the client. The result 260 of the execution of the query set 200 on the projected document 240 is guaranteed to be the same as if the query set 200 were executed on the original document 250 .
[0025] In query evaluation, our system constructs a representation of the input document based on the XPath set 230 which is derived from the query set 200 . In the current embodiment, this set is derived by hand from the query set 200 , but other techniques such as static analysis and profiling may be used as well. The set of XPath expressions 230 passed to projector 220 is an approximation of the XPath expressions that may be executed during query evaluation of the query set 200 —projector 220 must construct document projection 240 of the input document 250 based on this set efficiently. A novel feature of the projection algorithm discussed herein is the ability to handle complex XPath axes, as well as, predicates in an efficient manner.
[0000] Projection XPath Subset
[0026] The grammar of the set of XPath expressions 230 accepted by this projection algorithm is provided below. In the grammar, the non-terminal axis includes all axes defined in the XPath specification. Note that current art of projection algorithms cannot handle all XPath expressions as defined in the grammar; this grammar is used herein to explain at least one embodiment of the invention.
[0000] AbsLocPath :=‘/’ RelLocPath
[0000] RelLocPath :=Step‘/’ RelLocPath|Step :=Axis:: NodeTest|
[0000] Step‘[’PredExpr‘]’ PredExpr :=RelLocPath and PredExpr|
[0000] AbsLocPath and PredExpr|
[0000] RelLocPath|AbsLocPath
[0000] NodeTest :=String|*
[0027] An absolute path expression corresponds to one that satisfies AbsLocPath and is evaluated with respect to the root node of the tree. A relative XPath expression corresponds to RelLocPath, and is evaluated with respect to a provided set of elements in the tree.
[0000] XPath Expression Trees
[0028] An XPath expression can be represented as a rooted tree T=(V T , E T ), with labeled vertices and edges. The root of the tree is labeled root. For every NodeTest in the expression, there is a vertex labeled with the NodeTest. Each vertex other than root has a unique incoming edge labeled with the Axis specified before the NodeTest. The vertex corresponding to the rightmost NodeTest which is not contained in a PredExpr is designated to be the output vertex. There are functions, label T : V T →String, and axis T : E T →Axis that return the labels associated with the vertices and edges respectively. FIG. 3 provides an example of the tree representation of the XPath expression “//Book[Title and Author]/ancestor::Publisher”. In XPath, “//,” called the descendant operator, selects any Book element in the document. In FIG. 3 , element Book 310 corresponds to this part of the expression. “[Title and Author]” requires element Book 310 to also have particular children, here Title 330 and Author 320 correspond to these requirements. The next part of the expression, “/ancestor::Publisher” is met by element Publisher 340 , whose ancestor is element Book 310 .
[0029] The semantics of an XPath expression is defined in terms of embeddings. The following definitions should be helpful in understanding embeddings.
[0030] Definition 1: A pair of elements (n1, n2) in a document, D, where n1, n2 are elements of N D satisfies an edge constraint (v1, v2) in the tree representation T of an XPath expression if the relation between n1 and n2 in the document matches axis T (v1, v2). For example, if axis T (v1, v2)=child, child d (n1, n2)=true, and if axis T (v1, v2)=ancestor, desc D (n2, n1)=true.
[0031] Definition 2: An embedding of an XPath expression T into a document D is a function E: V T →N D such that:
Labels are matched, that is, for each v in V T , label T (v)=* or label T (v)=tag D (E(v)). Edges are satisfied, that is, if (v1, v2) in E T , then (E(v1), E(v2)) satisfies (v1, v2).
[0034] Let O be the output vertex of the tree representation of an XPath expression. The output of an XPath expression is defined as all n in N D such that there exists an embedding E such that E(O)=n.
[0000] Redefining Projection.
[0035] A projected document is defined in the prior art by Marian and Simeon in terms of an input document D and a set of XPath expressions P, where some of the expressions may be marked with the special output flag #. In that system, each XPath expression in P is an absolute XPath expression (that is, it is evaluated with respect to the root of the document). Marian and Simeon only allow the use of the child and descendant axes, predicates and backward axes are not supported. Given P and D, the projected document D is defined in the prior art by Marian and Simeon as follows:
[0036] Definition 3: Given a document D and a set of projection paths P. D′ is the projected document of D for the paths P if and only if D′ is composed of the subset of the nodes n in D such that either: (i) the node n is in the result of the evaluation of a path p in P over D,(ii) the node n is an ancestor of a node n, where n is in the result of the evaluation of a path p in P over D, or (iii) the node n is a descendant of a node n′, where n is in the result of the evaluation of a path p in P over D and p has the flag #.
[0037] The projected document contains all elements that are in the result set of an XPath expression in P, as well as, their ancestors. All subtrees rooted at some result of an XPath expression marked # are materialized as well. The definition guarantees that the projected document D′ satisfies the key property that the evaluation of any XPath expression in P on D′ returns the same result as the evaluation of that XPath expression on D. As a result, one can substitute D′ for D without changing the behavior of query evaluation with respect to P.
[0038] When XPath expressions with axes other than child and descendant are allowed in P, Definition 3 can no longer be applied; the evaluation of an XPath expression on the projected document D′ may differ from that on D. Consider the XPath expression, “//Author/ancestor::Publisher//Title” executed on the document in FIG. 1 . By Definition 3, only the elements outlined in bold in the FIG. 1 belong to the projected document D′. The result of this XPath expression on D′ will be the empty set since D′ does not contain any “Author” elements.
[0039] The embeddings of XPath expressions into a document D can be used as the basis for a general definition of projection when complex axes such as ancestor are allowed. We provide a definition that subsumes Definition 3 and serves as the basis for the algorithm presented below.
[0040] Definition 4: Let D be a document and P be a set of absolute XPath expressions, where some XPath expressions in P are marked with a special flag #. The projected document D′ is composed of the set of all elements n in D if:
(1) For some XPath expression p in P, there is an embedding E of p into D such that E(v)=n, where v is some vertex in p; or (2) For some XPath expression p in P, there is an embedding E of p into D such that E(v)=n, where v is some vertex in p, and n is a descendant of n in D; or (3) For some XPath expression p in P marked with the symbol #, n is the descendant of an element in the results of the evaluation of p on D.
[0044] In other words, the projected document consists of all elements that participate in an embedding and their ancestors. Moreover, for each element in the result set of the evaluation of a specially marked XPath expression, that element and all its descendants belong to the projected document.
[0000] Projection Construction
[0045] The system encompasses an algorithm for constructing projections from a given set of XPath expressions. The challenge is in being able to handle complex XPath axes such as ancestor efficiently in a single pass over the input document. This embodiment takes advantage of a key property of projection; since the query processor eventually evaluates the input query over the projected tree to determine the exact solution to the query, the projection construction algorithm can be approximate. This embodiment creates nodes in the tree for some elements that do not satisfy any of the conditions of Definition 4. The algorithm is, however, careful in limiting the construction of these inessential nodes. This embodiment ensures that the result of executing the input query on the projected document is the same as that of executing on the original document.
[0046] The embodiment works in two stages. First, the set of input XPath expressions P is normalized into a canonical form. In the second stage, a document (or a subtree of the document) is traversed to build a projection.
[0000] Normalizing XPath Expressions
[0047] The XPath axes following, preceding, following-sibling and preceding-sibling are order-based axes (the result set for these axes depends on the order between sibling tree nodes). The first step in our normalization is to rewrite instances of these axes in XPath expressions into order-blind axes (such as parent and ancestor). The rules for rewriting XPath expression trees are shown in FIGS. 4-8 . For example, in the FIG. 4 , vertex 400 and vertex 410 are vertices in a given XPath expression tree, connected by an edge labeled with one of the order-based axes. The rewriting rules introduces new vertices 420 and 430 . The rules are ordered so that the rules of FIG. 4 and FIG. 5 are applied until there are no instances of following and preceding in the XPath expression tree. The rules of FIG. 6 and FIG. 7 are then applied to the XPath expression tree.
[0048] For example, for the following-sibling axes, the present embodiment replaces instances of the pattern v1/following-sibling::v2 ( 600 - 610 ) with instances of v1/parent::*/v2 ( 600 , 620 , 610 ). The rewritten XPath expression is an approximation of the original one—it chooses “v2” elements that both precede and follow “v1” elements. The rewritings guarantee that for any document, if an element n participates in an embedding of the original XPath expression tree into the document, n also participates in an embedding of the rewritten tree into the document.
[0049] Once the XPath expression trees have been rewritten, the present embodiment performs further rewritings to remove redundancies. For example, if a vertex in an XPath expression tree has an incoming edge labeled child, and an outgoing edge labeled parent, the present embodiment merges the two vertices from which these edges are incident. The two vertices may be merged if they have the same label, or if the label of one of the vertices is the wildcard *. If the vertices cannot be merged because their labels differ, the present embodiment concludes that the XPath expression is unsatisfiable—there can be no document for which the XPath expression will return a result. For example, the XPath expression “//a/b/parent::c” is unsatisfiable. Unsatisfiable XPath expressions may be removed from the set of projection XPath expressions—there can be no embedding of these expressions into any document. FIG. 8 shows a rewritten XPath expression tree, where the vertices with edges incident on the vertex labeled “c” are merged.
[0000] Constructing a Projection
[0050] The present embodiment of the projection construction algorithm traverses the document in a depth-first manner and generates events, similar to SAX. A start element event is generated when the traversal first visits an element, and an end element event once the traversal of the subtree rooted at that element is finished. The present invention assumes that an event contains all information about the relevant element, such as its tag and unique identifier. At each of these events, an event handler is invoked to perform actions related to the construction of the tree. A start element event handler may direct the traverser to skip a subtree by issuing a skipSubtree call. In response to this call, the document traverser does not generate any events for the elements in the subtree of the element currently being processed. The next event generated will be an end element event for the corresponding element.
[0000] Definitions and Data Structures
[0051] The description of the present embodiment will use the following definitions and data structures.
[0052] Definition 5: Given a vertex vεV T in the input XPath expression tree, the backward vertex set of v, B(v) is defined as {v′|(v,v)εE T , axis(v,v)ε{parent, ancestor, ancestor-or-self, self}∪{v|(v,v)εE T , axis(v,v)ε{child, descendant, descendant-or-self, self}. A backward constraint is an edge between v and a vertex in its backward vertex set.
[0053] In other words, the backward vertex set with respect to a vertex v consists of those vertices to which an outgoing edge from v is labeled with a backward axis and those from which an incoming vertex into v is labeled with a forward axis. The present embodiment has a dual definition for a forward vertex set with respect to a vertex v.
[0054] Definition 6: Given a vertex vεV T in the input XPath expression tree, the forward vertex set of v, F(v) is defined as {v′|(v,v)εE T , axis (v,v)ε{(child, descendant, descendant-or-self, self}∪{v″|(v,v)εE T , axis(v″,v)ε{parent, ancestor, ancestor-or-self, self}. A forward constraint is an edge from between v and a vertex in its forward vertex set.
[0055] The following data structures are used in the algorithm of the present embodiment:
[0000] An active stack which maintains, at any time, the list of elements for which a start event has been received, but no end event has been received yet. For each element e in the stack the present embodiment maintains the following information:
[0000]
tag(e), level(e), and id(e).
[0057] An ordered set children(e) of the byte array corresponding to the children of the element in the document.
A relation, match-found(e): V T ×V T . A boolean variable, locked(e).
[0060] For each vertex in the XPath expression tree, a set of elements, matches(v).
[0000] Algorithm Overview
[0061] As events are generated during the traversal of the tree, the algorithm attempts to determine whether the element currently being processed may participate in an embedding. At the end element event, the algorithm makes a decision on whether the element node should be created or not, based on current information—it is conservative, if it cannot determine conclusively that the element can be discarded, the element node is created. The following two properties are used to determine whether an element belongs to an embedding:
[0062] A. Let an element e belong to an embedding E of T into D such that for some vertex v, E(v)=e. For each vertex v′ in B(v), there must be some ancestor of e, say e′, such that E(v′)=e′, and the relation between e and e′ satisfies the edge constraint between v and v′. This is a straightforward consequence of the definition of embeddings. At a start element event for an event, the present embodiment verifies that if the label of e matches some vertex v, then such a candidate e′ exists for all vertices v′εB(v). The matches list is used for this purpose. For a vertex v, it contains all ancestors of the current element e that have been identified as a possible candidate in an embedding with respect to v′. If matches(v) for some v′εB(v) does not contain an appropriate e′, e cannot participate in an embedding with respect to v.
[0063] B. A similar statement can be made for forward vertex sets. Let an element e belong to an embedding E of T into D such that for some vertex v, E(v)=e. For each vertex v′ in F(v), there must be some descendant of e, e′, such that E(v′)=e′, and the relation between e and e′ satisfies the edge constraint between v and v′. At the end element event, the algorithm can verify that if the label of e matches some vertex v, that such a candidate e′ exists for all vertices v′εF(v). The match-found relation is used for this purpose. For some vertex v, if match-found(e) contains (v, v′) for all vertices in F(v), the algorithm can conclude that e is a possible candidate in an embedding. If, on other hand, this property does not hold for any v that matches the tag of e, the algorithm can conclude that the element does not participate in any embedding. The match-found (e) relation is set during end element events of descendants of e. When an element e is identified as a possible candidate in an embedding with respect to a vertex v″, then for all elements e in matches (v), where v εB(v″), the tuple (v, v′) is added to match-found(e).
[0064] The algorithm constructs nodes for all elements that may participate in an embedding. All ancestors of these elements are added as nodes as well. The locked(e) variable is used to propagate the information that a possible embedding candidate exists in the subtree of e so that the algorithm can create a node for that element as well.
[0065] The algorithm can improve efficiency by skipping subtrees when possible. A skipSubtree call can be issued in the start element event handler if it can be determined that no element in the subtree will participate in an embedding. During the processing of an element e, one can skip the subtree if for all vertices v:
[0066] For all (v, v′), axis T (v, v′)=descendant or descendant-or-self, matches(v) is empty, or
[0067] For all (v, v′), axis T (v, v′)=ancestor or ancestor-or-self, matches (v′) is empty, or
[0068] For all (v, v′), axis T (v, v′)=child, level(e)>level(e′)+2, where e′ is the element in matches(v) with the highest level, or
[0069] For all (v, v′), axis T (v, v′)=parent, level(e)>level(e′)+2, where e′ is the element in matches(v) with the highest level.
[0070] The handling of multiple XPath expressions is a straightforward extension to the handling of a single XPath expression—the algorithm evaluates each of them in parallel. A node is created in the tree for an element if it is required by any of the XPath expressions.
[0000] Algorithm Details
[0071] The projector algorithm processes a given XPath expression T=(V T ,E T ) and a document D=(N D ,E D ) to construct the tree representation in a bottom-up manner—at each end element event for an element, the projector decides whether to build a node or discard the element based on decisions taken for its children. Initially, the active stack and matches(v) for all vεV T are empty.
[0072] At a start element event for an element e, push e on to the active stack. children(e), match-found(e) are empty. locked(e) is set to be false.
[0073] For each vertex v in the XPath expression tree such that tag(e) matches label(v), matches(v)=matches(v)∪e.
[0074] For each vertex v in the XPath expression tree such that tag(e) matches label(v), prune matches(v). For each v′ in B(v), we check that there exists some element in matches(v′) such that the edge constraint between v and v′ is met. For example, if the edge between v and v′ is an edge labeled ancestor, matches(v′) should contain an ancestor of e. If not, remove e from matches(v).
[0075] At an end element event for an element e:
[0076] If locked(e) is true, materialize the element by creating a new materialized node. Add children(e) as children of that node.
[0077] Otherwise, if e does not belong to matches(v) for any v that is in V T , examine children(e). If children(e) contains any materialized nodes, construct a node for e, and add children(e) as children of that node. Otherwise, discard e and the contents of children(e).
[0078] Otherwise, if for all vεV T , where matches(v) contains e, there exists some v′ in F(v) such that (v, v′)∉ match-found(e), construct a node corresponding to e. The contents of children(e) are discarded.
[0079] Otherwise, create a node for the element and add children(e) as children of that node. Let S be the set of all elements e′ in the active stack such that there exists an edge (v, v′), where eε matches(v), e′ε matches(v′) and the edge constraint specified by (v, v′) is matched by (e, e′). For each such e′, the present embodiment adds the tuple (v′, v) to match-found(e′). If the cardinality of S is greater than 1, the present embodiment marks e as locked.
[0080] In all cases, once the node for e is constructed, e is popped of the active stack, and e is appended to children(e′) where e′ is the parent of e in D (the new head of the active stack). e is also removed from matches(v) for all v. Finally, if e is marked locked, e′ is marked locked as well.
[0081] The present embodiment can handle complex axes such as ancestor and following-sibling. Our experiments demonstrate that the projections generated by the present embodiment are small compared to the full data instance, even when these complex queries are used. In addition to reducing the memory overhead of the in-memory representation of XML, the present embodiment is efficient and can reduce the cost of constructing the instance significantly.
[0000] Computer Implementation
[0082] The present embodiment may be realized in hardware, software, or a combination of hardware and software. A system according to a preferred embodiment of the present embodiment may be realized in a centralized fashion in one computer system, or in a distributed fashion where different elements are spread across several interconnected computer systems. Any kind of computer system—or other apparatus adapted for carrying out the methods described herein—is suited. A typical combination of hardware and software could be a general-purpose computer system with a computer program that, when being loaded and executed, controls the computer system such that it carries out the methods described herein.
[0083] An embodiment of the present embodiment may also be embedded in a computer program product, which comprises all the features enabling the implementation of the methods described herein, and which—when loaded in a computer system—is able to carry out these methods. Computer program means or computer program in the present context mean any expression, in any language, code or notation, of a set of instructions intended to cause a system having an information processing capability to perform a particular function either directly or after either or both of the following: a) conversion to another language, code or, notation; and b) reproduction in a different material form.
[0084] A computer system may include, inter alia, one or more computers and at least a computer readable medium, allowing a computer system, to read data, instructions, messages or message packets, and other computer readable information from the computer readable medium. The computer readable medium may include non-volatile memory, such as ROM, Flash memory, Disk drive memory, CD-ROM, and other permanent storage. Additionally, a computer readable medium may include, for example, volatile storage such as RAM, buffers, cache memory, and network circuits. Furthermore, the computer readable medium may comprise computer readable information in a transitory state medium such as a network link and/or a network interface, including a wired network or a wireless network, that allow a computer system to read such computer readable information.
[0085] FIG. 9 is a high level block diagram showing an information processing system 900 useful for implementing one embodiment of the present embodiment. The computer system 900 includes one or more processors, such as processor 902 , a memory 904 , an input/output subsystem 906 , and a mass storage device 908 . The system 900 is connected to a network 910 such as the Internet. Various software embodiments are described in terms of this exemplary computer system.
[0086] The I/O subsystem 906 can include a removable storage drive reads from and/or writes to a removable storage unit in a manner well known to those having ordinary skill in the art. The removable storage unit, represents a floppy disk, a compact disc, magnetic tape, optical disk, etc. which is read by and written to by removable storage drive. As will be appreciated, the removable storage unit 1018 includes a computer readable medium having stored therein computer software and/or data.
[0087] Therefore, while there has been described what is presently considered to be the preferred embodiment, it will be understood by those skilled in the art that other modifications can be made within the spirit of the invention.
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A method, computer readable medium and information processing system for projecting a representation of a document in the Extensible Markup Language (XML) format. The method dynamically creates a tree representation of an XML document based on a provided set of XPath expressions through approximate matching techniques. The projection created by the method supports all XPath axes including backward axes such as ?parent? and ?ancestor.? The execution of the set of XPath queries on the projected document is guaranteed to be the same as that of executing the XPath queries on the original document. The projected document typically occupies much less space than the original document.
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This application is a Divisional of co-pending U.S. patent application Ser. No. 09/482,371 filed Jan. 13, 2000 now U.S. Pat. No. 6,261,326, herein incorporated by reference in its entirety.
TECHNICAL FIELD
The present invention relates to generally to textile dyeing and more particularly to the introduction of dyes and other chemicals into a process for dyeing a textile material in a supercritical fluid.
BACKGROUND ART
It will be appreciated by those having ordinary skill in the art that conventional aqueous dyeing processes for textile materials, particularly hydrophobic textile materials, generally provide for effective dyeing, but possess many economic and environmental drawbacks. Particularly, aqueous dyebaths that include organic dyes and co-solvents must be disposed of according to arduous environmental standards. Additionally, heat must be applied to the process to dry the textile material after dyeing in an aqueous bath. Compliance with environmental regulations and process heating requirements thus drive up the costs of aqueous textile dyeing to both industry and the consuming public alike. Accordingly, there is a substantial need in the art for an alternative dyeing process wherein such problems are avoided.
One alternative to aqueous dyeing that has been proposed in the art is the dyeing of textile materials, including hydrophobic textile materials like polyester, in a supercritical fluid. Particularly, textile dyeing methods using supercritical fluid carbon dioxide (SCF—CO 2 ) have been explored.
However, those in the art who have attempted to dye textile materials, including hydrophobic textile materials, in SCF—CO 2 have encountered a variety of problems. These problems include, but are not limited to, “crocking” (i.e. tendency of the dye to smudge when the dyed article is touched) of the dye on the dyed textile article; unwanted deposition of the dye onto the article and/or onto the dyeing apparatus during process termination; difficulty in characterizing solubility of the dyes in SCF—CO 2 ; difficulty introducing the dyes into the SCF—CO 2 flow; and difficulty in preparing the dyes for introduction into the dyeing process. These problems are exacerbated when attempts to extrapolate from a laboratory process to a plant-suitable process are made.
PCT Publication No. WO 97/13915, published Apr. 17, 1997, designating Eggers et al. as inventors (assigned to Amman and Söhne GmbH and Co.) discloses a system for introducing dye into a CO 2 dyeing process which comprises a bypass flow system associated with the main circulation system that includes a color preparing vessel. The bypass is opened, after a certain temperature and pressure are reached, so that SCF—CO 2 flows through the color preparing vessel and dissolves the previously loaded dye(s). The SCF—CO 2 -containing dissolved dye flows from the bypass back into the main circulation system where it joins the bulk of the SCF—CO 2 flow that is used to accomplish dyeing.
PCT Publication No. WO 97/14843, published Apr. 24, 1997, designating Eggers et al. as inventors (assigned to Amman and Söhne GmbH and Co.) discloses a method for dyeing a textile substrate in at least one supercritical fluid, wherein the textile substrate is preferably a bobbin and the fluid is preferably SCF—CO 2 . The disclosed invention attempts to prevent color spots from forming on the textile substrate during dyeing and is directed to ways of incorporating the dye material into the supercritical fluid using the basic bypass system as described above in PCT WO 97/13915.
The method involves the use of at least one dye which is contacted with the supercritical fluid as a dye bed, dye melt, dye solution, and/or dye dispersion before and/or during actual dyeing in an attempt to form a stable solution of dye in the supercritical fluid. A stated goal is avoiding the formation of dye agglomerates having a particle size of more than 30 microns, preferably more than 15 microns, in the solution.
This invention attempts to accomplish these aims through a variety of embodiments. In one embodiment, the dye bed is provided with inert particles, in particularly glass and/or steel balls, to prevent agglomeration. Alternatively, the dye bed itself can consist of inert particles coated with the dye. SCF—CO 2 is then passed through the dye bed to incorporate the dye within the SCF—CO 2 .
However, there are a number of significant drawbacks to this embodiment of the dye introduction method disclosed by Eggers et al. PCT Publication No. WO 97/14843. For example, use of a fixed or fluidized bed to introduce dye into the dyeing system can be hindered if appropriate flow conditions are not present. The dye particles must be at all times in intimate and vigorous contact with the supercritical fluid for effective dissolution. If this is not the case, the dissolution rate will be low and will likely not be complete by the end of the dyeing cycle.
Moreover, promotion of a high convective mass transfer coefficient (i.e., intimate and vigorous mixing) can result in substantial pressure losses through the dye-add vessel. Because of their relatively low viscosity values, supercritical fluids are easily diverted to areas of lower resistance, which can lead to mechanical problems such as channeling and stagnation. Channeling refers to the development of a fluid path, or channel, through a particulate bed that circumvents uniform flow throughout the bed; i.e., a stream of fluid develops through the bed such that the flow in the region where the stream exists is greater than the flow of fluid in the rest of the bed. In this case, the particles not in the channel are not properly contacted by the fluid. These conditions, in turn, result in dye particles not being contacted in a manner that will allow substantially complete dissolution.
Insuring the proper flow conditions when using fluidized dye beds, fixed dye beds, or dye bed holding devices requires very careful and complex design of the internals of the dye-add vessel in order to assure good mixing and to avoid mechanical flow problems without excessive pressure drop. Indeed, it is likely that dye bed holding devices that are chambered to force uniform flow of fluid through the bed, such as those proposed for use in dye introduction by Eggers et al., PCT Publication No. WO 97/14843, also suffer very high pressure losses.
Another drawback arises when the fluidized and fixed dye bed is installed in the system in a bypass loop. Since the dye dissolution process is rate limiting, this arrangement couples the dyeing process to the dye dissolution process, which is generally undesirable. In contrast, the dye should be introduced at a rate consistent with dyeing the textile material as rapidly as possible but also in a level manner.
An alternative embodiment of the dye injection method disclosed by Eggers et al. PCT Publication No. WO 97/14843 involves injection of the dye as a melt incorporated in an inert gas, preferably nitrogen or carbon dioxide (with property of being inert for these two gases being a function of the process conditions). It has been observed by the present applicants that melting of disperse dyes can lead to decreased solubility in SCF—CO 2 . This circumstance indicates that the applicability of this embodiment of the disclosed dye injection method is limited.
Yet another embodiment of the dye introduction method disclosed by Eggers et al. PCT Publication NO. WO 97/14843 involves delivery of the dye into the supercritical fluid flow as a solution or suspension. When a solution is being injected and water-soluble dyes are being used, the recommended injection solvent is water. For water-insoluble dyes, a variety of common nontoxic injection solvents are suggested, with acetone, which readily dissolves disperse dyes, being foremost. The water-insoluble dyes are injected as a solution or suspension in the chosen solvent. In the case that a suitable nontoxic solvent cannot be found or the required amount of solvent is so great that it adversely affects the dyeing process, injection of a dispersion, preferably an aqueous dispersion, is recommended.
This embodiment of the method disclosed by Eggers et al. PCT Publication No. WO 97/14843 also suffers from several drawbacks. Firstly, water is an anti-solvent in SCF—CO 2 when used with disperse dyes. Thus, for SCF—CO 2 , the presence of water results in a significantly impaired dyeing process to the extent that it is questionable whether dyeing could be accomplished at all. At best, the action of water in the SCF—CO 2 would cause the dye to reside in the dyeing process as dispersion. In the worst case, the dye would exist as an unstable suspension with unsuitable properties for dyeing. Secondly, in the case that a suitable SCF—CO 2 /water/dye dispersion was obtained, the SCF—CO 2 dyeing process would be similar to the conventional aqueous process, the replacement of which is a desired goal in the art.
Poulakis et al., Chemiefasern/Textilindustrie, Vol. 43-93, February 1991, pages 142-147 discuss the phase dynamics of supercritical carbon dioxide. An experimental section describing an apparatus and method for dyeing polyester in supercritical carbon dioxide in a laboratory setting is also presented. Thus, this reference only generally describes the dyeing of polyester with supercritical carbon dioxide in the laboratory setting and is therefore believed to be limited in practical application.
U.S. Pat. No. 5,199,956 issued to Schlenker et al. on Apr. 6, 1993 describes a process for dyeing hydrophobic textile material with disperse dyes by heating the disperse dyes and textile material in SCF—CO 2 with an azo dye having a variety of chemical structures. The patent thus attempts to provide an improved SCF—CO 2 dyeing process by providing a variety of dyes for use in such a process.
U.S. Pat. No. 5,250,078 issued to Saus et al. on Oct. 5, 1993 describes a process for dyeing hydrophobic textile material with disperse dyes by heating the disperse dyes and textile material in SCF—CO 2 under a pressure of 73 to 400 bar at a temperature in the range from 80° C. to 300° C. Then the pressure and temperature are lowered to below the critical pressure and the critical temperature, wherein the pressure reduction is carried out in a plurality of steps.
U.S. Pat. No. 5,578,088 issued to Schrell et al. on Nov. 26, 1996 describes a process for dyeing cellulose fibers or a mixture of cellulose and polyester fibers, wherein the fiber material is first modified by reacting the fibers with one or more compounds containing amino groups, with a fiber-reactive disperse dyestuff in SCF—CO 2 at a temperature of 70-210° C. and a CO 2 pressure of 30-400 bar. Specific examples of the compounds containing amino groups are also disclosed. Thus, this patent attempts to provide level and deep dyeings by chemically altering the fibers prior to dyeing in SCF—CO 2 .
U.S. Pat. No. 5,298,032 issued to Schlenker et al. on Mar. 29, 1994 describes a process for dyeing cellulosic textile material, wherein the textile material is pretreated with an auxiliary that promotes dye uptake subsequent to dyeing, under pressure and at a temperature of at least 90° C. with a disperse dye from SCF—CO 2 . The auxiliary is described as being preferably polyethylene glycol. Thus, this patent attempts to provide improved SCF—CO 2 dyeing by pretreating the material to be dyed.
Despite extensive research into SCF—CO 2 textile dyeing processes, there has been no disclosure of a suitable method for introducing dyes or other textile treatment materials into such processes. An environmentally and economically sound method for introducing dyes or other textile treatment materials would be particularly desirable in the plant-scale application of a SCF—CO 2 textile dyeing process. Therefore, the development of such a method meets a long-felt and significant need in the art.
DISCLOSURE OF THE INVENTION
A process for introducing a textile treatment material into a textile treatment system is disclosed. The process comprises: (a) providing a preparation vessel in fluid communication with a textile treatment system; (b) loading a textile treatment material into the preparation vessel; (c) dissolving or suspending the textile treatment material in near-critical liquid carbon dioxide or supercritical fluid carbon dioxide in the preparation vessel; and (d) introducing the dissolved or suspended textile treatment material into a textile treatment system. A system suitable for use in carrying out the process is also disclosed.
The process and system of the present invention are preferred for use with a textile treatment system that utilizes SCF—CO 2 as a treatment medium. Optionally, the textile treatment material can be selected from a group including, but not limited to, a brightening agent, a whitening agent, a dye and combinations thereof.
Accordingly, it is an object of the present invention to provide an improved process and system for introducing dyes or other textile treatment materials into a textile treatment system, preferably a SCF—CO 2 textile treatment system.
It is another object of the present invention to provide an environmentally benign process and system for introducing dyes or other textile treatment materials into a textile treatment system, preferably a SCF—CO 2 textile treatment system.
It is another object of the present invention to provide a process and system for introducing dyes or other textile treatment materials into a textile treatment system, preferably a SCF—CO 2 textile treatment system, that reduces the loss of such textile treatment materials in a textile processing operation.
It is yet another object of the present invention to provide a process and system for introducing dyes or other textile treatment materials into a textile treatment system, preferably a SCF—CO 2 textile treatment system, that can be isolated from the textile treatment system to thereby facilitate addition of dyes and other textile treatment materials thereto.
It is a further object of the present invention to provide an improved process and system for introducing dyes or other textile treatment materials into a textile treatment system, preferably a SCF—CO 2 textile treatment system, in accordance with an introduction profile that facilitates correspondence between the introduction rate and an appropriate dyeing rate.
It is a further object of the present invention to provide an improved process and system for introducing dyes or other textile treatment materials into a textile treatment system, preferably a SCF—CO 2 textile treatment system, at an introduction point where there is high fluid shear to ensure proper mixing of the introduced treatment material into the textile treatment system.
It is yet a further object of the present invention to provide an improved process and system for introducing dyes or other textile treatment materials into a textile treatment system, preferably a SCF—CO 2 textile treatment system, that utilizes supercritical fluid and/or near-critical liquid carbon dioxide as a solvent for the dye or other textile treatment material.
Some of the objects of the invention having been stated herein above, other objects will become evident as the description proceeds, when taken in connection with the accompanying drawings as best described herein below.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a schematic of a prior art system for introducing textile treatment materials into a SCF—CO 2 textile dyeing process;
FIG. 2 is a schematic of a system for introducing textile treatment materials into a textile treatment system wherein the system utilizes a stirred dye-add vessel in accordance with a process of the present invention;
FIG. 3 is a schematic of a system for introducing textile treatment materials into a textile treatment system wherein the system utilizes a circulated dye-add loop in accordance with a process of the present invention;
FIG. 4 is a schematic of a syringe pump with mechanical piston and circulation pump for use in a system for introducing textile treatment materials into a textile treatment system in accordance with the present invention;
FIG. 5 is a schematic of a syringe pump with mechanical piston and magnetically coupled stirrer for use in a system for introducing textile treatment materials into a textile treatment system in accordance with the present invention;
FIG. 6 is a schematic of a syringe pump with mechanical piston and no agitation for use in a system for introducing textile treatment materials into a textile treatment system in accordance with the present invention;
FIG. 7 is a schematic of a syringe pump with an inert fluid piston and magnetically coupled stirrer for use in a system for introducing textile treatment materials into a textile treatment system in accordance with the present invention; and
FIG. 8 is a schematic of a syringe pump with an inert fluid piston and no agitation for use in a system for introducing textile treatment materials into a textile treatment system in accordance with the present invention.
DETAILED DESCRIPTION OF THE INVENTION
While the following terms are believed to be well-understood in the art, the following definitions are set forth to facilitate explanation of the invention.
The terms “supercritical fluid carbon dioxide” or “SCF—CO 2 ” are meant to refer to CO 2 under conditions of pressure and temperature which are above the critical pressure (P c =about 73 atm) and temperature (T c =about 31° C.). In this state the CO 2 has approximately the viscosity of the corresponding gas and a density which is intermediate between the density of the liquid and gas states.
The terms “near-critical liquid carbon dioxide” or “NCL—CO 2 ” are meant to refer to liquid CO 2 under conditions of pressure and temperature which are near the critical pressure (P c =about 73 atm) and temperature (T c =about 31° C.).
The term “textile treatment material” means any material that functions to change, modify, brighten, add color, remove color, or otherwise treat a textile material. Examples comprise UV inhibitors, lubricants, whitening agents, brightening agents and dyes. Representative fluorescent whitening agents are described in U.S. Pat. No. 5,269,815, herein incorporated by reference in its entirety. The treatment material is, of course, not restricted to those listed herein; rather, any textile treatment material compatible with the introduction and treatment systems is envisioned in accordance with the present invention.
The term “dye” is meant to refer to any material that imparts a color to a textile material. Preferred dyes comprise sparingly water-soluble or substantially water-insoluble dyes. More preferred examples include, but are not limited to, forms of matter identified in the Colour Index, an art-recognized reference manual, as disperse dyes. Preferably, the dyes comprise press-cake solid particles which has no additives.
The term “disperse dye” is meant to refer to sparingly water soluble or substantially water insoluble dyes.
The term “sparingly soluble”, when used in referring to a dye, means that the dye is not readily dissolved in a particular solvent at the temperature and pressure of the solvent. Thus, the dye tends to fail to dissolve in the solvent, or alternatively, to precipitate from the solvent, when the dye is “sparingly soluble” in the solvent at a particular temperature and pressure.
The term “hydrophobic textile fiber” is meant to refer to any textile fiber comprising a hydrophobic material. More particularly, it is meant to refer to hydrophobic polymers which are suitable for use in textile materials such as yarns, fibers, fabrics, or other textile material as would be appreciated by one having ordinary skill in the art. Preferred examples of hydrophobic polymers include linear aromatic polyesters made from terephathalic acid and glycols; from polycarbonates; and/or from fibers based on polyvinyl chloride, polypropylene or polyamide. A most preferred example comprises one hundred fifty denier/34 filament type 56 trilobal texturized yarn (polyester fibers) such as that sold under the registered trademark DACRON® (E.I. Du Pont De Nemours and Co.). Glass transition temperatures of preferred hydrophobic polymers, such as the listed polyesters, typically fall over a range of about 55° C. to about 65° C. in SCF—CO 2 .
The term “crocking”, when used to describe a dyed article, means that the dye exhibits a transfer from dyed material to other surfaces when rubbed or contacted by the other surfaces.
Following long-standing patent law convention, the terms “a” and “an” mean “one or more” when used in this application, including the claims.
A critical step in the treating of textile materials in a supercritical fluid (e.g., SCF—CO 2 ) involves the introduction of textile treatment material (e.g., dyes and other chemicals). Current introduction methods employed in SCF—CO 2 textile dyeing systems are somewhat similar to those used in commercial aqueous dyeing systems.
An exemplary prior art system is shown schematically in FIG. 1 and generally designated 10 . As shown in FIG. 1, dyeing system 10 comprises a dyeing vessel 12 , a dyeing circulation loop 14 , a dyeing loop circulation pump 16 , a dye-add vessel 18 , and a series of SCF—CO 2 flow control valves 20 . Dye is introduced into system 10 by placing it in dye-add vessel 18 , which can accommodate flow of SCF—CO 2 . SCF—CO 2 flow is mediated by circulation pump 16 . At the appropriate time in the dyeing process, a portion of the main SCF—CO 2 flow (represented by arrows in FIG. 1) is diverted from dye circulation loop 14 via valves 20 into dye-add vessel 18 in order to effect dissolution of the dye. The diverted SCF—CO 2 flow, laden with dissolved dye, then re-enters and mixes with the main SCF—CO 2 flow in loop 14 for use in dyeing the textile material, which is placed in vessel 12 .
In marked contrast to prior art methods and systems, the textile treatment material introduction process and system of the present invention decouple the textile treatment material dissolution process from the treatment process. The dye introduction rate is used to effect control over the dyeing rate in order to minimize non-uniform dyeing behavior, such as shading and streaking. As such, the dye introduction rate is varied to achieve amounts of dye in solution ranging from near zero up to the equilibrium value at each set of dyeing conditions (CO 2 density and temperature). Though a variety of solvents or carrier fluids can be used in the method and system of the present invention, the preferred preparation fluid is pure CO 2 in supercritical or near-critical liquid form.
The dye is introduced as a solution or suspension (dispersion) in SCF—CO 2 or NCL—CO 2 , depending on the required dye injection rate and the degree of solvency of SCF—CO 2 in the textile treatment system at the existing treatment conditions. As such, the use of surfactants or dispersing chemicals is not required in the introduction process and system of the present invention. However, co-solvents or surfactants may optionally be used to enhance dye solubility and dispersing agents may optionally be used to facilitate the establishment of stable suspensions of textile treatment materials in CO 2 .
Preferably, the textile treatment material introduction process and system of the present invention is used in conjunction with a method for treating a textile material using supercritical fluid carbon dioxide (SCF—CO 2 ). More preferably, the textile treatment material introduction method and system of the present invention are used in the treatment of a hydrophobic textile material, such as polyester, in SCF—CO 2 . However, application of the process and system of the present invention to other textile treatment processes and systems is contemplated.
For example, the method and system of the present invention also can be used with conventional aqueous dyeing processes. This is particularly the case with respect to treatment materials that are sparingly soluble in water. The textile treatment material introduction method and system of the present invention are used to predissolve such treatment materials, and the treatment materials are then introduced into a conventional aqueous dyebath. The use of environmentally hazardous organic co-solvents is thus avoided.
The textile treatment material introduction process and system of the present invention facilitate introduction of a textile treatment material, such as a dye, into a textile treatment process in that the treatment material is already dissolved or suspended when it contacts the solvent used in the treatment process. Thus, problems, such as agglomeration of particles, that have been observed in prior art processes, including particularly prior art SCF—CO 2 dyeing processes, are avoided.
Referring now again to the drawings, a preferred embodiment of the textile treatment material introduction system of the present invention is generally designated 30 in FIG. 2 . Referring to FIG. 2, system 30 introduces textile treatment materials dissolved or suspended in NCL—CO 2 or SCF—CO 2 into a textile treatment system 32 (similar to the prior art system shown in FIG. 1 ), which preferably comprises a SCF—CO 2 textile treatment system. System 30 comprises dye-add or preparation vessel 34 , positive-displacement metering pump 36 , line sections 38 and 40 , control valves 42 , 43 and 44 , filter 46 and return line 48 . Treatment system 32 comprises a treatment vessel 50 , a circulation loop 52 and a circulation pump 54 .
Continuing with reference to FIG. 2, a textile treatment material is placed in preparation vessel 34 , which is equipped with a stirring device 56 capable of thoroughly mixing the contents of vessel 34 . Stirring device 56 comprises a motor-driven fan, but may also comprise a motor-driven shaft, a rotatably mounted shaft, or any other suitable stirring device as would be apparent to one of ordinary skill in the art after reviewing the disclosure of the present invention. Other stirring devices include a fan, propeller or paddle that is magnetically coupled to a motor rather than coupled to the motor by a solid shaft. Another approach, though mechanically more difficult, comprises placing the dye bed within a holding container within the preparation vessel that is both permeable to flow of the SCF—CO 2 and capable of being agitated within the fluid. The permeable holding container can thus be adapted for rotation via the flow of SCF—CO 2 to provide mixing of the dye bed with the SCF—CO 2 . Such devices, and equivalents thereof, thus comprise “stirring means” and “mixing means” as used herein and in the claims.
Continuing with reference to FIG. 2, in operation the preparation vessel 34 of system 30 is sealed and charged with NCL—CO 2 or SCF—CO 2 . The amount of CO 2 initially charged and the state of CO 2 (i.e., NCL—CO 2 or SCF—CO 2 ) depends on the CO 2 density desired at the introduction conditions. If a co-solvent, surfactant or dispersing agent is to be used, it is charged along with the textile treatment material, or introduced with a metering pump (not shown in FIG. 2) into the preparation vessel 34 at some point in the textile treatment material preparation process. The contents of the preparation vessel 34 are then heated with mixing to the introduction conditions (i.e., CO 2 density and temperature), which is contemplated to be a pressure that is near the textile treatment system pressure.
Preferably, introduction system 30 , and particularly preparation vessel 34 , is isolated from treatment system 32 when the solution or suspension of textile treatment material is prepared. Control valves 42 , 43 and 44 are used to isolate preparation vessel 34 and thus can be opened and closed for reversibly isolating preparation vessel 34 . Any other suitable structure, such as other valves, piping or couplings, as would be apparent to one of ordinary skill in the art after reviewing the disclosure of the present invention may also be used to isolate, preferably to reversibly isolate, preparation vessel 34 . Such devices and structures, and equivalents thereof, thus comprise “isolation means” as used herein and in the claims.
Continuing with FIG. 2, depending on the introduction conditions and amount of textile treatment material present, the textile treatment material resides in a suspension or in a combination of solution and suspension. If introducing of a textile treatment material solution is desired, the fluid is removed from preparation vessel 34 via line section 38 , which is equipped with a filter 46 , and via control valve 42 . The filtering media of filter 46 has pore sizes predetermined from the particle size distribution and solubility characteristics of the textile treatment material. If introducing of a textile treatment material suspension or combination of textile treatment material solution and suspension is desired, the fluid is removed from the preparation vessel 34 via line section 40 and control valve 43 .
Continuing with reference to FIG. 2, positive-displacement metering pump 36 introduces the textile treatment material-laden NCL—CO 2 or SCF—CO 2 into the circulation loop 52 of treatment system 32 using a introducing rate profile that is consistent with producing uniformly-treated textile materials in minimum processing time. In a preferred embodiment, pump 36 shown in FIG. 2 comprises a positive displacement pump with a reciprocating piston. Other representative pumps include a syringe type pump employing a mechanical piston (FIGS. 4-6) as described below and a syringe type pump employing an inert fluid as a piston (FIGS. 7 and 8) as described below. Thus, devices such as pumps, nozzles, injectors, combinations thereof, and other devices as would be apparent to one of ordinary skill in the art after reviewing the disclosure of the present invention, and equivalents thereof, comprise “introducing means” as used herein and in the claims.
Mixing of the preparation vessel 34 is continued throughout the introduction cycle via mechanical stirring with stirring device 56 . Introducing of the textile treatment material-laden NCL—CO 2 or SCF—CO 2 occurs at an introduction point 58 in the circulation loop 52 where fluid shear is very high. For example, point 58 may lie before or after circulation pump 54 or in a mixing zone that contains static mixing elements (not shown in FIG. 2) in order to facilitate mixing with the treatment medium (e.g. SCF—CO 2 ) flowing in circulation loop 52 of treatment system 32 . The term “high fluid shear” refers to a turbulent flow or a flow with high rate of momentum transfer. Preferably, the term “high fluid shear” refers to a flow having a Reynolds number greater than 2300, and more preferably, greater than 5000.
When the textile treatment material is introduced as a solution from preparation vessel 34 into a SCF—CO 2 treatment system 32 , CO 2 makeup to introduction system 30 occurs via return line 48 . This action is taken in order to maintain the CO 2 density in introduction system 30 . Makeup of CO 2 involves opening the control valve 44 in the return line 48 such that SCF—CO 2 is diverted from circulation loop 52 to preparation vessel 34 in quantities sufficient to maintain the operating pressure of the introduction system 30 . Thus, control valve 44 and return line 48 , or any other suitable structure, such as other valves or couplings, as would be apparent to one of ordinary skill in the art after reviewing the disclosure of the present invention may be used to divert SCF—CO 2 to preparation vessel 34 . Such devices and structures, and equivalents thereof, thus comprise “diverting means” as used herein and in the claims.
When textile treatment material is dosed as a suspension into the treatment system 32 , introduction system 30 operates with full or partial CO 2 makeup via return line 48 . When textile treatment material introducing is performed without CO 2 makeup, the control valve 44 in return line 48 remains closed throughout the introduction cycle, and preparation vessel 34 is emptied of its contents during the introduction cycle. For introduction of suspension with full makeup, control valve 44 operates as described above. In the case of partial makeup, control valve 44 is operated intermittently to return SCF—CO 2 from circulation loop 52 to preparation vessel 34 ; i.e., preparation vessel 34 is partially emptied and then refilled with return SCF—CO 2 .
In the case of full or partial makeup to introduction system 30 when NCL—CO 2 is utilized in system 30 , the pressure of the returning SCF—CO 2 stream is reduced substantially across control valve 44 and return line 48 to match the near-critical liquid pressure in preparation vessel 34 .
Referring now to FIG. 3, an alternative embodiment of the textile treatment material introduction system 30 shown in FIG. 2 is disclosed and generally designated 60 . In alternative embodiment 60 , treatment materials are introduced in NCL—CO 2 or SCF—CO 2 into textile treatment system 62 , which preferably comprises a SCF—CO 2 textile treatment process. System 60 comprises dye-add or preparation vessel 64 , positive-displacement metering pump 66 , line sections 68 and 70 , control valves 72 , 73 and 74 , filter 76 and return line 78 . Treatment system 62 comprises a treatment vessel 80 , a circulation loop 82 and a circulation pump 84 .
Textile treatment material is placed in the preparation vessel 64 of system 60 . Preparation vessel 64 is equipped with a mixing loop 86 as shown in FIG. 3 . Thus, mixing of the preparation vessel 64 is continued throughout the introducing cycle via fluid circulation (demonstrated by arrows in FIG. 3) by circulation pump 88 through mixing loop 86 . Such devices and structures, and equivalents thereof, thus comprise “circulation means” and “mixing means” as used herein and in the claims. Other aspects of alternative embodiment 60 function as described above, including the introduction of treatment material at high fluid shear introduction point 90 .
Referring again to FIGS. 2 and 3, the method and system of the present invention also contemplate treating a textile material after introduction of a textile treatment material from the introduction system to the treatment system. The treatment system comprises a treatment vessel, a circulation loop, and a circulation pump. In a preferred embodiment, the treatment system comprises a SCF—CO 2 treatment system. A textile material, such as a hydrophobic textile fiber, is placed in the treatment vessel. A solution or suspension of treatment material is introduced into the treatment system at an introduction point from the introduction system as described above. The flow, represented by arrows in FIGS. 2 and 3, of the medium used in the treatment system (e.g. SCF—CO 2 flow) is mediated by the circulation pump. The circulation pump directs the flow of treatment medium, which now includes the solution or suspension of treatment material, along the circulation loop to the treatment vessel. In accordance with a preferred embodiment of the present invention, if a suspension is introduced into the treatment circulation loop, the conditions in the loop are such that the suspended material is rapidly dissolved in the treatment flow of supercritical fluid and not carried further as a suspension. Thus, the introduction is preferably made into an area of high shear to promote rapid mixing and dissolution of any undissolved treatment material particles. Within the vessel the treatment material contacts the textile material for a suitable time to impart the desired characteristics to the textile material.
Referring now to FIG. 4, an embodiment of a syringe pump suitable for use as an introducing means in accordance with the present invention is disclosed and is generally designated 100 . Syringe pump 100 comprises syringe pump body 102 , piston 104 , high pressure hose section 106 , circulation pump 108 , and high pressure hose section 110 . Syringe pump body 102 comprises an internal void space 112 in which piston 104 is slidably mounted. Piston 104 comprises an axial channel 114 through which the flow 116 (represented by arrows in FIG. 4) of SCF CO 2 travels within syringe pump 100 .
Continuing with FIG. 4, circulation pump 108 is connected to syringe pump body 102 via high pressure hose sections 106 and 110 . Circulation within syringe pump 100 is thus provided via circulation pump 108 . Treatment material-laden SCF CO 2 118 enters syringe pump 100 from a preparation system via line 120 and valve 122 . Circulation, or other type of agitation, is preferred if further dissolution of the dye is being accomplished or if an unstable suspension of the dye is being introduced. If circulation or agitation is not required (e.g., when introducing a stable suspension of the dye), an inert gas piston might be substituted for the mechanical piston, as discussed below and as shown in FIGS. 7 and 8. Syringe pump 100 then propels treatment material-laden SCF CO 2 118 into a treatment system via line 124 and valve 126 .
Referring now to FIG. 5, an alternative embodiment of a syringe pump suitable for use as an introducing means in accordance with the present invention is disclosed and is generally designated 150 . Syringe pump 150 comprises a syringe pump body 152 having an internal void space 154 wherein a syringe pump piston 156 is slidably mounted. Syringe pump piston 156 comprises an axially mounted stirrer shaft 158 having a stirrer shaft magnet 160 mounted at the end of stirrer shaft 158 proximate to stirrer magnet 162 . Stirrer magnet 162 is also mounted within syringe pump piston 156 , and propeller stirrer 164 extends from stirrer magnet 162 into the internal void space 154 of syringe pump 150 .
Continuing with FIG. 5, treatment material-laden SCF CO 2 166 enters syringe pump 150 from a preparation system via line 168 and valve 170 . Agitation of treatment material-laden SCF CO 2 166 is accomplished within syringe pump 150 via propeller stirrer 164 . Syringe pump 150 then propels treatment material-laden SCF CO 2 166 into a treatment system via line 172 and valve 174 .
Referring now to FIG. 6, yet another alternative embodiment of a syringe pump suitable for use as an introducing means in accordance with the present invention is disclosed and is generally designated 200 . Syringe pump 200 comprises a syringe pump body 202 having an internal void space 204 , and a piston 206 slidably mounted within the interval void space 204 of syringe pump body 202 . Treatment material-laden dye 208 enters syringe pump 200 from a preparation system via line 210 and valve 212 . Syringe pump 200 then propels treatment material-laden SCF CO 2 208 into a treatment system via line 214 and valve 216 .
Referring now to FIG. 7, another alternative embodiment of a syringe pump suitable for use as an introducing means in accordance with the present invention is disclosed and is generally designated 250 . Syringe pump 250 comprises pump body 252 having an internal void space 256 , and a high pressure fluid inlet line 254 . A stirrer shaft 258 and a stirrer shaft magnet 260 are mounted at the end of the syringe pump body 252 opposite the line 272 and valve 274 that connect pump 250 with a treatment system. A stirrer magnet 262 is also mounted in pump body 252 proximate to stirrer shaft magnet 260 . A propeller stirrer 264 extends into the internal void space 256 of pump body 252 from stirrer magnet 262 .
Continuing with FIG. 7, treatment material-laden SCF C 2 266 enters pump 250 from a preparation system via line 268 and valve 270 . An inert material 278 (designated with a large arrow in FIG. 7 ), such as supercritical fluid nitrogen, is introduced into the internal void space 256 of pump body 252 via inlet line 254 while propeller stirrer 264 stirs the treatment material-laden SCF CO 2 266 . The in-flow inert material 278 drives treatment material-laden SCF CO 2 266 into a treatment system via line 272 and valve 274 .
Referring finally to FIG. 8, still another alternative embodiment of a syringe pump suitable for use as an introducing means in accordance with the present invention is disclosed and is generally designated 300 . Syringe pump 300 comprises pump body 302 having an internal void space 306 , and a high pressure inlet line 304 connected at the end of pump body 302 opposite from the line 314 and valve 316 that connect syringe pump 300 with a treatment system.
Continuing with FIG. 8, treatment material-laden SCF CO 2 308 enters syringe pump 300 from a preparation system via line 310 and valve 312 . An inert material 318 (designated with a large arrow in FIG. 8 ), such as supercritical fluid nitrogen, is introduced into the internal void space 306 of pump body 302 via high pressure line 304 . Inert material 318 thus drives treatment material-laden SCF CO 2 308 into a treatment system via line 314 and valve 316 .
The syringe pumps disclosed in FIGS. 4-8 can also be used in maintaining the SCF—CO 2 density in the preparation vessel by facilitating the addition of fresh SCF—CO 2 to the preparation vessel at the conditions in the preparation vessel without necessarily diverting SCF—CO 2 from the treatment system. For example, additional SCF—CO 2 can be introduced via high pressure lines 106 and/or 110 in FIG. 4 . This approach also adds additional SCF—CO 2 to the treatment system, and the treatment process is altered to include a different treatment process control strategy to accommodate the additional SCF—CO 2 . Thus, the pumps disclosed in FIGS. 4-8 also provide an alternative embodiment of the present invention in which SCF—CO 2 density is maintained in the preparation system without diverting SCF—CO 2 to the preparation vessel from the treatment system.
An advantage of the textile treatment material introduction process and system of the present invention is that it is used to introduce a variety of chemicals for treatment of a textile material. Thus, multiple operations can be performed concurrently or sequentially. For example, once a first textile treatment material, such as a dye, is introduced, the introducing system can be isolated and depressurized. Then, another textile treatment material, such as a UV inhibitor, can placed in the preparation vessel for introduction into the treatment system in accordance with the steps described herein above.
It will be understood that various details of the invention may be changed without departing from the scope of the invention. Furthermore, the foregoing description is for the purpose of illustration only, and not for the purpose of limitation—the invention being defined by the claims.
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A process for introducing a textile treatment material into a textile treatment system, particularly a supercritical fluid carbon dioxide (SCF—CO 2 ) treatment system. The process includes the steps of providing a preparation vessel in fluid communication with a textile treatment system; loading a textile treatment material into the preparation vessel; dissolving or suspending the textile treatment material in near-critical liquid carbon dioxide or supercritical fluid carbon dioxide in the preparation vessel; and introducing the dissolved or suspended textile treatment material into the textile treatment system. The textile treatment material can be selected from a group including a brightening agent, a whitening agent and a dye. A system suitable for use in carrying out the process is also disclosed.
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FIELD OF THE INVENTION
The present invention relates generally to a device that can be used to apply either a compressive force or a tensile force to a surface or object, and more particularly, to such a device that is attached to a surface using stretch releasing adhesive, whereby the device can be firmly attached to the surface but may be easily and cleanly removed from the surface without damaging the surface.
BACKGROUND OF THE INVENTION
Suction attachable clamps are known in the prior art. U.S. Pat. No. 5,820,116 (Haese), for example, discloses a suction attachable retaining clamp for holding an object such as a molding or mounting bracket against a surface such as a windshield. U.S. Pat. No. 4,457,503 (Conner) discloses a suction clamp for holding moldings in place on front or rear windshields of automobiles, while an adhesive material sets or dries, and it simultaneously prevents damage to the adjacent surface. Such clamps, however, are limited to producing clamping or compressive forces, and work best on clean, slightly moistened, non-porous surfaces such as metal and glass.
There is therefore a need for a device that can function not only as a clamp but also as a device to exert a pulling or tensile force when needed. There is also a need for such a device that can be used for a variety of end use applications and can be used on a variety of surfaces under a variety of conditions.
It would therefore be desirable to provide a simple and inexpensive single-sided clamp-like device that can be securely fastened to a surface and readily removed without damaging the surface or leaving unwanted residue that can be used as both a clamp to exert a compressive force, and as a device to produce a pulling or tensile force. It would also be desirable to provide a device that can be used on a wide variety of surfaces including metal, glass, paper, masonry and unfinished wood, and is not limited to use on non-porous surfaces such as metal and glass.
SUMMARY OF THE INVENTION
The present invention overcomes the above-identified limitations in the field by providing a simple and inexpensive single-sided clamp-like device that can be applied to a surface and can be used not only as a clamp, but can also be used to produce a pulling or tensile force at a selected location on a surface or an object. The present invention also provides a device that can be used on a wide variety of surfaces including paper, wood, and masonry, and is not limited to use on non-porous surfaces such as metal and glass.
In one embodiment, the present invention provides a device for applying a tensile or compressive force to an object or surface comprising a body, a plunger movably connected with the body, and a double-sided stretch releasing adhesive attached to at least one of the body and the plunger, whereby the body and/or the plunger can be firmly adhesively bonded to a surface and cleanly removed from the surface without damaging the surface by stretching the adhesive.
In a specific aspect of the invention, the stretch releasing adhesive is attached to the body. In another aspect, the stretch releasing adhesive is attached to the plunger.
In one embodiment, the body includes a connecting portion containing a through bore, a pair of legs extending in the same direction from opposite sides of the connecting portion, and a pair of feet portions arranged perpendicular at the end of each leg. Each foot portion is provided with stretch releasing adhesive to attach the body to a surface.
In one aspect of the invention, the plunger is threadably connected with the body, whereby the plunger can be rotated clockwise and counter clockwise to produce the compressive and tensile forces. In another aspect, the plunger is slidably connected with the body and the plunger is biased by a spring or the like to produce the forces.
In another embodiment, the body includes a main body portion and a cantilever portion extending laterally outwardly from the main body portion, wherein the plunger is movably connected with the cantilever portion.
In another aspect, the plunger is provided with a head that is adapted to receive a stretch releasing adhesive. The plunger may also include a handle opposite the head to facilitate manual actuation of the plunger.
In a particular aspect, the invention may be used interchangeably to produce either a compressive (i.e. clamping) force or a tensile (i.e. pulling) force where in the past, two separate devices were needed to create compressive and tensile forces.
The present invention can be used for a wide variety of uses and applications such as holding an object in place while an adhesive, such as a hot melt adhesive, glue, or epoxy sets, dries, or otherwise cures. This may be useful, for example, to mount a soap dish to a ceramic tile wall using epoxy. In addition, the device may be used to removably mount one or more items on a surface such as decorations, a banner, or a flag, whereby the item may be readily and repeatably removed and/or replaced by simply loosening the device to remove the item without removing the device itself from the surface. The device may also be provided with a pointed tip or drill bit to mark, pierce, or form a hole in a surface or object. The present invention may find use in woodworking, crafts, or other uses in the home, office, or in industrial applications. For example, the present invention may be used to stamp or emboss a piece of paper or piece of wood.
BRIEF DESCRIPTION OF THE DRAWINGS
The present invention will be further described with reference to the accompanying drawings, in which:
FIG. 1 is a perspective view of a device according to the invention;
FIG. 2 is a sectional view taken along line 2 — 2 of FIG. 1 ;
FIG. 3 is a side sectional view of a second embodiment of the invention; and
FIG. 4 is a side sectional view of a third embodiment of the invention.
DETAILED DESCRIPTION
Referring now to the drawings, FIGS. 1 and 2 show a device 2 including a body member 4 , a plunger member 6 rotatably attached to the body member 4 , a pair of double-sided stretch releasing adhesive strips 8 a attached to the body member 4 to removably adhesively bond the body member 4 to a surface 10 , and a double-sided stretch releasing adhesive strip 8 b attached to the plunger member 6 for adhesively bonding the plunger member 6 to either the surface 10 or an object (not shown) arranged between the plunger member 6 and the surface 10 .
Stretch releasing adhesives represent a class of high performance pressure-sensitive adhesives combining strong holding power with clean removal and no surface damage. Such stretch releasing adhesives are useful in a wide variety of assembling, joining, attaching, and mounting applications. The double-sided adhesive strips 8 a,b may be any conventionally known stretch releasing adhesive tape including a stretch releasing adhesive tape with an elastic backing, a stretch releasing adhesive tape with a highly extensible and substantially inelastic backing, or a stretch releasing adhesive tape comprising a solid elastic pressure sensitive adhesive.
Specific tapes suitable for use in the various embodiments of the present invention include the pressure sensitive adhesive tapes with elastic backings described in U.S. Pat. No. 4,024,312 (Korpman), the pressure sensitive adhesive tapes with highly extensible and substantially inelastic backings described in U.S. Pat. No. 5,516,581 (Kreckel et al.) and Bries et al. (U.S. Pat. No. 6,231,962), and the solid elastic pressure sensitive adhesive described in German Patent No. 33 31 016.
A suitable double-sided commercially available stretch releasing adhesive is the product sold under the trade designation COMMAND adhesive by 3M Company, St. Paul, Minn. This product is currently manufactured as discrete strips with one end of the strip including a non-adhesive pull tab to facilitate stretching of the strip during removal.
In the illustrated embodiment, the body member 4 includes a bridge portion 4 a containing a threaded opening 12 for receiving the plunger member 6 , a pair of parallel leg portions 4 b extending perpendicularly in the same direction from opposite sides of the bridge portion 4 a , and a pair of feet portions 4 c extending outwardly in opposite directions from the ends of the leg portions 4 b . The adhesive strips 8 a are affixed to the bottom surfaces of the feet portions 4 c to adhesively bond the body member 4 to surface 10 , and thereby securely bond the device 2 to the surface 10 .
Plunger 6 is arranged generally perpendicular to the bridge portion 4 a and includes a cylindrical threaded body portion 6 a rotatably engaging the opening 12 in the body member 4 , a handle 14 arranged at one end of the body portion 6 a to facilitate manual rotation of the plunger 6 , and a head 16 arranged at the end of the body portion 6 a opposite the handle 14 . The handle 14 is arranged above the bridge portion 4 a of the body member 4 to allow a user to readily access the handle 14 , and thereby manually rotate the plunger 6 . The head 16 is arranged below the bridge portion 4 a and is axially movable by rotational actuation of the plunger 6 via handle 14 either in the direction of the surface 10 , thereby to apply a compressive force to the surface, or away from the surface 10 , thereby to generate a tensile force relative to the surface. Head 16 is preferably connected with the plunger 6 with a slip fit type of connection to allow the body portion 6 a and the head 16 to move independently. That is, when the body portion 6 a of the plunger 6 is rotated, the head 16 may pivot to remain in contact with the surface but does not rotate.
To use the device 2 to apply a force to surface 10 or an object (not shown) arranged between the plunger 6 and the surface 10 , the plunger 6 is rotated such that the head 16 moves in the direction of the surface 10 . As the plunger 6 moves toward and engages the surface 10 , a compressive force will be exerted on the surface 10 or on the object. It will be recognized that when the device is used in this manner (i.e. as a clamp to generate a compressive force), adhesive strips 8 a are needed to maintain the device 2 in engagement with surface 10 , but that adhesive strip 8 b is not needed because the plunger 6 is maintained in contact with surface 10 via compression. Stated another way, when the device 2 is used as a clamp, the plunger 6 is forced against the surface 10 which, in turn, forces the body member 4 away from the surface 10 , and the adhesive strips 8 a serve to hold the body member 4 in contact with the surface 10 to allow the plunger 6 to exert a compressive force on the surface. To remove the device 2 from the surface 10 , each adhesive strip 8 a is stretched in the known manner to simultaneously debond the adhesive strip from the device and the associated surface.
Conversely, to use the device 2 to generate a pulling or stretching force on surface 10 or on an object (not shown) arranged between the surface 10 and the head 16 , stretch releasing adhesive strip 8 b is attached to the head 16 , thereby to adhesively bond the plunger 6 to surface 10 or to the object (not shown) arranged between the head 16 and the adhesive strip 8 b . When the plunger 6 is rotated such that the head 16 moves away from the surface 10 , a tensile force will be exerted on the surface 10 or on the object. When used in this manner (i.e. as a pulling device to generate a tensile force relative to the surface), adhesive strip 8 b is needed to attach the plunger 6 to the surface 10 or the object, but it will be recognized that adhesive strips 8 a are not needed to secure the device 2 to the surface because the device is maintained in contact with the surface 10 via compression.
FIG. 3 shows a device 102 in accordance with another embodiment of the invention. The device 102 is similar to the device 2 shown in FIGS. 1 and 2 except the device 102 includes a spring 120 for urging the plunger 106 toward or away from the surface 110 , thereby to produce a compressive or tension force on the surface 110 , respectively.
The device 102 includes a body member 104 , a plunger 106 movably connected with the body member 104 , a pair of double-sided stretch releasing adhesive strips 108 a attached to the body member 104 to removably adhesively bond the body member 104 to the surface 110 , and a double-sided stretch releasing adhesive strip 108 b attached to the plunger 106 for adhesively bonding the plunger 106 to surface 110 or an object (not shown) arranged between the plunger 106 and the surface 110 .
The body member 104 includes a bridge portion 104 a containing an opening 112 for slidably receiving the plunger 106 , a pair of parallel leg portions 104 b extending perpendicularly in the same direction from opposite sides of the bridge portion 104 a , and a pair of feet portions 104 c extending outwardly in opposite directions from the ends of the leg portions 104 b . The adhesive strips 108 a are affixed to the bottom surfaces of the feet portions 104 c to adhesively bond the body member 104 to surface 110 , and thereby securely bond the device 102 to the surface 110 .
Plunger 106 is arranged generally perpendicular to the bridge portion 104 a and includes a cylindrical body portion 106 a slidably engaging the opening 112 in the body member 104 , a handle 114 arranged at one end of the body portion 106 a to facilitate manual actuation of the plunger 106 , and a head 116 arranged at the end of the body portion 106 a opposite the handle 114 . The handle 114 is arranged above the bridge portion 104 a of the body member 104 to allow a user to readily access the handle 114 , and thereby manually actuate the plunger 106 .
Spring 120 is arranged between the bridge portion 104 a of the device 102 and the head 116 . When the plunger 106 is manually urged upwardly away from the surface 110 , the spring 120 is compressed and biases the head 116 in the direction of the surface 110 . It will be recognized that when the device is used in this manner (i.e. as a clamp to generate a compressive force), adhesive strips 108 a are needed to maintain the device 102 in engagement with surface 110 , but that adhesive strip 108 b is not needed because the plunger 106 is maintained in contact with surface 110 via compression. Stated another way, when the device 102 is used as a clamp, the plunger 106 is forced against the surface 110 via spring 120 which, in turn, forces the body member 104 away from the surface 110 , and the adhesive strips 108 a serve to hold the body member 104 in contact with the surface 110 to allow the plunger 106 to exert a compressive force on the surface. To remove the device 102 from the surface 110 , each adhesive strip 108 a is stretched in the known manner to debond the adhesive strip from the device and surface simultaneously.
Alternatively, the spring 120 can be a tension spring that is attached to the bridge portion 104 a and the head 116 , such that when the spring is urged downwardly in the direction of the surface 110 , the spring is put in tension. In this manner, when the head 116 is attached to the surface 110 via adhesive strip 108 b , a tensile force is produced on the surface 110 . When used in this manner (i.e. as a pulling device to generate a tensile force relative to the surface), adhesive strip 108 b is needed to attach the plunger 106 to the surface 110 or the object, but it will be recognized that adhesive strips 108 a are not needed to secure the device 102 to the surface because the device is maintained in contact with the surface 110 via compression.
As with the device 2 of FIGS. 1 and 2 , head 116 is preferably connected with the plunger 106 with a slip fit type of connection to allow the body portion 106 a and the head 116 to move independently.
FIG. 4 shows a device 202 in accordance with an alternate embodiment of the invention including a body member 204 , a plunger member 206 rotatably attached to the body member 204 , a pair of double-sided stretch releasing adhesive strips 208 a attached to the body member 204 to removably adhesively bond the body member 204 to a surface 210 , and a double-sided stretch releasing adhesive strip 208 b attached to the plunger member 206 for adhesively bonding the plunger member 206 to surface 210 or an object 218 arranged between the plunger member 206 and the surface 210 . The device of FIG. 4 is particularly suited for generating a tensile or compressive force in a tight location such as a corner, where the devices shown in FIGS. 1–3 would not fit.
The body member 204 includes a main body portion 204 a and a cantilever portion 204 b containing a threaded opening 212 for receiving the plunger member 206 . The cantilever portion 204 b extends laterally outwardly from the main body portion 204 a . Adhesive strips 208 a are affixed to the bottom of the main body portion 204 a to adhesively bond the body member 204 to the surface 210 , and thereby secure the device 202 to the surface 210 .
Plunger 206 is arranged generally perpendicular to the cantilever portion 204 b and includes a cylindrical threaded body portion 206 a rotatably engaging the opening 212 in the body member 204 , a handle 214 arranged at one end of the body portion 206 a to facilitate manual rotation of the plunger 206 , and a head 216 arranged at the opposite end of the body portion 206 a . The handle 214 is arranged above the cantilever portion 204 b of the body member 204 to allow a user to readily access the handle 214 , and thereby manually adjust the plunger 206 . The head 216 is arranged below the cantilever portion 204 b and may be rotatably urged either in the direction of the surface 210 to apply a force to the surface, or urged away from the surface 210 to generate a tensile force relative to the surface by rotating the plunger 206 via handle 214 .
Device 202 is used to apply a force to object 218 in the same manner as the device of FIGS. 1 and 2 , that is, the plunger 206 is rotated such that the head 216 moves in the direction of the surface 210 . As the plunger 206 moves toward and engages the object 218 , a compressive force will be exerted on object 218 . And to use the device 202 to impart a pulling or stretching force on object 218 , stretch releasing adhesive strip 208 b is attached to the head 216 , thereby adhesively bonding the plunger 206 to the object 218 . In this manner, when the plunger 206 is rotated such that the head 216 moves away from the surface 210 , a tensile force will be exerted on the object 218 .
Because of its cantilevered design, the device 202 of FIG. 4 is less stable than the device 2 of FIGS. 1 and 2 . Consequently, when the device 202 of FIG. 4 is used as either a clamping device to generate a compressive or as a pulling device to generate a tensile force, it is desirable to include stretch releasing adhesive strips 208 a to firmly bond and thereby secure the body member 204 to the support surface 210 . As with the device 2 of FIGS. 1 and 2 , when the device 202 is used to generate a tensile force, adhesive strip 208 b is required, but when the device is used as a clamp, adhesive strip 208 b may be omitted.
The device, including both the body member and the plunger, may be formed of a variety of materials depending on the particular intended end use application of the device. Suitable materials include metals such as steel, synthetic plastic materials such as polycarbonate and polyvinyl chloride, and wood. The particular material selected is not significant to the invention hereof, so long as it provides the desired combination of properties such as adequate strength, low cost, and ease of manufacture.
It will be apparent to those of ordinary skill in the art that various changes and modifications may be made without deviating from the inventive concept set forth above. For example, it will be recognized that the size and shape of the device may be modified to adapt the device for certain specific end use applications, that the body member and plunger may be movably attached by means other than a threaded connection, that the number and size of the adhesive strips may be varied, that the plunger may be provided with a pointed tip, drill bit, or other implement depending on the specific end use application intended for the device, and that the location of the cantilever portion 204 b may be moved. Thus, the scope of the present invention should not be limited to the structures described in this application, but only by the structures described by the language of the claims and the equivalents of those structures.
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An adhesively mounted single-sided clamp-like device for producing a compressive force or tensile force includes a body, a plunger movably connected with the body, and a double-sided stretch releasing adhesive attached to at least one of the body and the plunger. The body and/or plunger can be firmly adhesively bonded to a surface or object and later cleanly removed from the surface or plunger without damaging the surface and without leaving adhesive residue by stretching the adhesive.
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The present invention relates to the treatment of flowable food products for at least partially sterilizing of the same.
BACKGROUND OF THE INVENTION
Conventional pasteurizing method uses plate heat exchangers, where the transmission of heat is carried out through a surface that is heated to a temperature far above the temperature required to obtain the proper heat treatment. Beside being energetically very inefficient, this method is causing many problems to the users, such as off-flavour, browning, cooked flavor and burnt deposits on the heating surfaces. Even though pasteurization is considered as the most efficient means to conical bacteria contamination, heat-resisting bacteria are not destroyed by the pasteurizing temperatures and processing times practical for this type of method. If sterilization is required for long-time conservation, one must add chemical preservatives.
OBJECTS OF THE INVENTION
It is the general object of the present invention to provide a process and apparatus for at least partially sterilizing flowable food products, which obviate the above-noted disadvantages in that heat is instantaneously transmitted through the mass of the food product to thereby eliminate off-flavour, browning, caramelization, cooked flavour and burnt deposits on the heating surface of the conventional heat-treating system.
It is another object of the present invention to provide a heat-treating proces which is applicable to various flowable food products and, more particularly, milk and cream.
It is another object of the invention to provide an apparatus for hot-treating food products, which is compact, requires about 40% less energy than the conventional pasteurization apparatus; does not require a boiler, steam and condensate piping and other appliances, such as de-aerators, steam valves, piping insulation; and which does not require maintenance, such as adjusting and retrofitting of oil burners and re-tubing of the boiler.
Another object of the invention is to provide an apparatus of the character described, which is of simple and inexpensive construction and operation, and which can treat food products in a continuous flow.
SUMMARY OF THE INVENTION
The process in accordance with the invention consists of continuously flowing a flowable food product as a relatively thin layer, while exposed to a source of electro-magnetic radiations. For pasteurizing the food products, the source of electro-magnetic radiations is an infra-red source, while for sterilizing the product, ultra-violet radiations are used.
The apparatus in accordance with the invention comprises a treatment cell, of tubular shape, including an elongated radiation-emitting element spacedly surrounded by a tubular jacket completely transparent to the electro-magnetic radiations and in turn spacedly surrounded by an outer tube, forming with the jacket, an annular passage for the flow of the food products to be treated.
In accordance with the present invention, the apparatus further comprises a holding chamber to complete pasteurization and heat exchangers to pre-heat the food products and to recuperate the heat therefrom after treatment.
The foregoing will become more apparent during the following disclosure and by referring to the drawings, in which: dr
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is an elevation of a typical apparatus in accordance with the invention;
FIG. 2 is a longitudinal section of an infra-red heating cell;
FIG. 3 is a longitudinal section of a holding chamber;
FIG. 4 is a longitudinal section of an ultra-violet sterilizing cell;
FIG. 5 is a cross-section of a multi-tube ultra-violet sterilizing coil;
FIG. 6 is a longitudinal section of a heat-exchanger module;
FIG. 7 is a flow diagram of a pasteurizing-sterilizing unit;
FIG. 8 is a flow diagram of a pasteurizing unit;
FIG. 9 is a flow diagram of a pasteurizing-sterilizing unit fitted with pre-cooling or pre-heating and cooling system; and
FIG. 10 is a flow diagram of a pasteurizing unit fitted with a pre-heating section.
DETAILED DESCRIPTION OF THE INVENTION
FIG. 1 shows an apparatus for pasteurizing and sterilizing a food product, such as milk. The flow diagram of the apparatus shown in FIG. 1 is illustrated in FIG. 7. The apparatus comprises one or more infra-red heating cells 1, a holding chamber 2, heat exchangers 3 and 3', an ultra-violet sterilizing cell 4, a control module 5, a volumetric pump 6 with its electric motor, a turbine flow meter 7, a receiving tank 8 and suitable piping with three-way valves 89 and 89'. The untreated food product enters at 88 and exits at 86.
In normal operation, the food product is circulated through pump 6 through one pass of heat exchanger 3' and 3, through the infra-red heating cell 1, through the holding tank 2, through the other pass of the heat exchanger 3, through the ultra-violet sterilizing cell 4, through the other pass of the heat exchanger 3' and, finally, to be discharged at 86 where it may be further cooled down by the cooling unit 87.
To start the pasteurizing and sterilizing operation, the food product is circulated for a few minutes in a closed loop through the system until the product has been heated sufficiently by the infra-red heating cell 1. For this purpose, once the system is filled with a product, the three-way valves 89 are operated so that the product will recirculate through the receiving tank 8 and back through the pump 6.
As shown in FIG. 7, a cooling unit 87 may be added to the outlet 86 if the liquid at not sufficiently cooled.
A three-way valve 89', with a discharge to a drain, may be added at the outlet of the holding chamber 2 to drain this part of the system.
One of the infra-red cells is shown in FIG. 2. It comprises an elongated infra-red radiations emiting element 11 spacedly surrounded by a tubular jacket 12, made of quartz or other material, which is completely transparent to infra-red radiations. The jacket 12 is in turn spacedly surrounded by an outer tube 13, made of metal, the interior surface of which is polished, so as to be reflective to the radiations. Two similar end cell bodies 14 hold the above-described assembly. One and cell body defines inlet chamber 15 in communication with an inlet port 22 and with the annular space 27, while the other end cell body 14 defines a similar outlet chamber 24 with an outlet port 25 and in communication with the annular space 27. End cell bodies 14 hold the infra-red element 11 by means of holding plates 17 and a support element 26. The infra-red element 11 is connected to an electrical power source by electrical socket 19 and electrical wire 21. The socket 19 is enclosed in a chamber formed by one end cell body 14 and closed by a screwed-cap 18. The cap carries a screwing head 20 for the passage of electrical wire 21. The infra-red radiations-emitting element 11 can be removed without stopping the flow of liquid in the infra-red cell.
The element 11 is completely isolated from the liquid and can be reached by removing the screwed caps 18 and the holding plates 17. The jacket 12 is sealed to both end cell bodies 14 by means of a gasket 16 held in place by a threaded compression disc 23.
The liquid or semi-liquid food product to be treated flows through the annular space 27 as a relatively thin layer, while being irradiated by the infra-red element 11. The food product is heated to the required pasteurization temperature without being exposed to heated surface, since the jacket 12, being made of quartz, does not become hot.
FIG. 3 is a longitudinal section of the holding chamber 2, which chamber consists of an inner shell 31 spacedly surrounded by an outer shell 32 with the interposition of insulating material 34. The ends of the two shells are fitted on end shell rings 33, which support an end casing 35. One end casing has an outlet port 36, while the end casing has an inlet port 37. The outer shell 32 is preferably provided with expansion ribs 38. The inside diameter of inner shell is of larger cross-sectional area than the cross-sectional area of the annular space 27 of he infra-red cell 1, so that the food product will slow down in the holding chamber 2 for sufficient time to allow completion of pasteurization, the food product being then at the pasteurizing temperature as obtained by exposure in the infra-red cell.
FIG. 4 illustrates the ultra-violet cell 4. This cell includes an ultra-violet radiation-emitting tube 41 spacedly surrounded by a quartz tubing, or jacket 42, completely transparent to ultra-voilet radiations. The jacket 42 is in turn surrounded by an outer tube 43, which defines with the jacket 42 an annular space 46. The jacket 42 and tube 43, together with the ultra-violet 41, are held in end cell bodies 44, of similar construction and of a construction similar to the end cell bodies 14 of the infra-red cell 1. One end cell body 44 defines inlet chamber 45 provided with an inlet port 54, while the other body 44 defines outlet chamber 55 and outlet port 55. One end of the ultra-violet tube 41 is supported by a tube socket 51 and socket bearing plate 47. The tube is connected to electrical wire 50, which extends through a screwing head 49 attached to the screwed cap 48. The other end of the ultra-violet tube 41 is supported by a tube support 57 and a tube socket 58 secured to the socket bearing plate 47. As with the infra-red cell, the ultra-violet radiation-emitting tube 41 can be removed without stopping the flow of liquid.
The tube 41 is completely isolated from the liquid and can be reached by removing the screwed caps 48 and the socket bearing plates 47. The quartz jacket 42 is sealed to the respective end cell body 44 by means of a watertight gasket 53 held in place by a threaded compression disc 52. Here again, the food to be treated which enters inlet port 54 into inlet chamber 45 will flow as a relatively thin layer through the annular space 46 to exit at 55. Since the quartz jacket 42 is completely transparent to the ultra-violet variations, it will not heat up and sterilization will be effected without substantially increasing the temperature of the food product. Sterilization is enhanced since the outer tube 43, which is made of metal, has an interior polish to reflect the ultra-violet radiations.
For increased capacity, the ultra-violet cell can take the form shown in FIG. 5, wherein a multi-tube cell is shown in cross-section. Each ultra-violet tube 41 is partly surrounded by a transversely-curved reflector 62, for instance made of polished aluminum. The reflectors 62 are joined two by two by a non-scratch edge protector 63 engaging the inside surface of the quartz jacket 64, which is in turn spacedly surrounded by the outer tube 66, again made of metal with an interior surface polish. Obviously, the number of tubes and associated reflectors may vary to meet treatment requirements.
FIG. 6 shows a typical heat exchanger 3 which comprises an inner metal tube 71 surrounded by an outer metal tube 72 defining an annular space therebetween. The two tubes 71 and 72 are supported at their ends by two similar end cell bodies 73. One body 73 defines an inlet chamber 73 with its inlet port 75, while the other body 73 defines and outlet chamber 78 with its outlet port 79. The inner tube 71 is held in sealing engagement with the cell bodies 73 by means of watertight gaskets 76 held in place by screwed compression ring 77. The inner tube 71 protrudes from the end cell bodies 73 and is provided at its two ends with a coupling 80 for coupling to the piping of the apparatus. One path of the food product is through the inner tube 71, while the other path is through the annular space between the inner and outer tubes 71 and 72.
In the arrangement of FIG. 1, there are two series-connected infra-red heating cells 1 followed by one holding chamber 2, four series-connected heat-exchanger modules 3, two series-connected ultra-violet cells 4 and four series-connected heat exchangers 3 installed in the respective order.
The elements are all horizontally oriented and are secured side by side in a vertical plan to obtain a compact apparatus.
It is energically efficient, since the whole operation requires 40% less energy than pasteurization effected with conventional systems.
The entire apparatus may be mounted on casters, so that the unit may be transported to different areas of the same plant.
The control center 5 serves to control the operation of the three-way valves 89, the pump 6 at the required rate of flow as measured by the flow meter 7. Also, temperature sensors are provided and a warning light is installed to indicate whether or not the sterilizer cells 4 are in operation.
Infra-red radiations will heat rapidly the food product throughout its mass without overheating the tube walls in contact with the flowable food product.
Ultra-violet radiations are used to destroy the thermophyllic and thermoduric bacteria that survive pasteurization, and this makes up most of the residual bacteria count legally permitted in pasteurized products.
In the treatment cells, unabsorbed infra-red or ultra-violet energy will strike the highly-polished enclosures and will be mostly reflected back into the mass of the food product to be eventually absorbed by the same.
The low temperature sterilization assures the destruction of spores reproducing bacteria, while avoiding the cooked taste caused by high temperature treatment.
The holding chamber 2 downstream from the infra-red heating cells 1 serves to hold the product at the pasteurizing temperature for sufficient time to complete the pasteurization process.
When sterilizing a chemically-unstable liquid, the time exposure of the liquid of the ultra-violet rays must be carefully controlled, in order to prevent photo-chemical reactions which may have an adverse effect on flavour.
Preferably, operation of the infra-red emittng tubes is controlled by an electronic modulator located in the control center 5.
Referring to FIG. 7, after leaving the holding tank 2, the food product to be treated at first cooled down in the heat-exchanger section 3 to the heat suitable temperature for sterilization in the ultra-violet cells. Thereafter, the treated flowable food product is further cooled down in the second heat-exchanger stage 3. It is then discharged in cooled condition at 86, or further cooled in a cooling unit 87.
The holding chamber 2 is mainly required for milk, cream, syrup, fruit juice, alcohol. Some other products, like wines, do not need such a holding chamber.
Sterilization may not be required every time; therefore, the ultra-violet generating tubes 41 may be de-energized from the control center 5. A flashing warning signal will inform the operator that the sterilization is in operation. Sterilization by the ultra-violet cells is applicable to alcohol, beer, brandy, cider, coffee extract, cooking oil, egg mixture, egg white, fruit juice, honey, herring brine, molasses, must, peptic juice, syrup, tomato ketchup, vinegar, water, wine, whisky, yolk and similar products.
The apparatus can handle liquid, semi-liquid or even pulpous products. It is applicable to the partial aging of wines, brandy, whisky, etc. No change of color or taste has been found when treating fruit and vegetable juice.
If only sterilization is required, then the infra-red heating cells 1 may be simply cut off.
FIG. 8 shows a flow diagram of a pasteurizing unit without the sterilizing function. Otherwise, this unit is the same as in FIG. 7.
FIG. 9 is a flow diagram of a pasteurizing and sterilizing unit fitted with a pre-cooling or pre-heating section and a cooling section. It is similar to the flow diagram of FIG. 7, with the addition of a pre-cooling and/or heating section 91 fed by cooling of heating liquid circulated by pump 90. There is another cooling section, indicated at 92.
FIG. 10 represents a flow diagramof a pasteurizing unit fitted with a pre-heating section. This is similar to the flow diagram of FIG. 8, with the addition of a pre-heating exchange section 93 fed with hot water from a hot water tank 93 and hot water circulating pump 95. This section 93 can be bypassed by operation of the three-way valve 89.
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There are disclosed an apparatus for pasteurizing and/or sterilizing food products by exposing the latter to electro-magnetic radiations, namely: infra-red radiation for pasteurization and ultra-violet radiations for sterilization. The apparatus enables continuous treatment of the food products.
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CROSS REFERENCE TO RELATED APPLICATIONS
[0001] This application claims priority of German application No. 10 2007 041 729.4 filed on Sep. 4, 2007, the entire disclosure of which is hereby incorporated herein by reference
BACKGROUND ART
[0002] The invention relates to a method for producing a processing atmosphere for producing and processing layers on substrates, with processing gas being supplied to a processing chamber and exhausted in a defined manner. The invention also relates to devices for executing the method.
[0003] This method is predominantly applied in CVD-processes (chemical vapor deposition) for precipitating an individual layer or a system of individual layers under defined processing atmospheres in such pressure ranges that allow the creation of gas flows. Here, the processing atmospheres for the production of the individual layers may deviate from each other.
[0004] For the purpose of coating, substrates are moved passing in a substrate level one or more coating sources in a coating chamber or in a sequence thereof. Both the production as well as the processing of layers occurs either continuously or discontinuously depending on the applicable coating method and depending on the embodiment of the coating arrangement. This principle processing sequence is the same for appropriate embodiments of the coating source and/or the coating source environment even for the processing of layers already precipitated on a substrate, for example a modification of the layer composition or the layer features. For this reason the following descriptions related to coatings shall also relate to the processing of existing layers. This method can also be used in a particular embodiment for PVD-processes (physical vapor deposition).
[0005] It is known from various application fields to produce or to process both individual layers as well as layered systems on substrates, with the latter comprising several layers positioned over top of each other, which in turn have been precipitated under different precipitation conditions and/or using different coating materials, e.g., thin-layer solar cells or optic systems of functional layers. In any case it is necessary for the precipitation of the individual layers to separately produce the processing atmospheres necessary in the coating chamber, if applicable deviating from each other. A deviation of the processing atmospheres can relate to various parameters, e.g., the material to be precipitated, the pressure, or the composition of the processing gas. Further, for the creation of homogenous and low-defect individual layers it is essential for each processing atmosphere to keep the pressure and the composition of the atmosphere perpendicular in reference to the direction of transportation, i.e., homogenously over the width of the substrate.
[0006] For this purpose, in known coating arrangements, such as described in DE 10 2004 014 323 A1, particularly for the coating of large substrates with long coating sources, seen in the direction perpendicular in reference to the direction of transportation, gas supply systems are used by which processing gas is supplied in the environment of the coating source distributed over the width of the substrate. In U.S. Pat. No. 5,096,562 it is also described to feed inert and reactive gas over the entire length of the tubular cathode as the coating source in order to homogenously operate the cathode. Here, any gas supplied or exhausted for the execution of the respective coating method in a coating chamber shall be included, e.g., an inert carrier gas such as argon, or a reactive gas, such as oxygen or nitrogen, for a reactive coating and also additional gaseous additives or a mixture of these components.
[0007] Furthermore, it is necessary to keep the substrate and the processing atmosphere free from contamination, clusters of coating material, and condensate, because such contaminations considerably influence the quality of the layers.
[0008] In the following, such a connected volume of a coating arrangement shall be considered a coating chamber which is not separated by tightly sealing valves but is provided with separating or dividing walls having openings for transporting the substrate through the coating chamber. Using such separating walls, which protrude at one side or at both sides of the substrate almost to the substrate in the coating chamber, the coating chamber can be divided into at least two compartments following each other in the direction of transportation. A coating compartment comprises one or more coating sources. For producing a defined processing atmosphere the coating compartment can be evacuated either directly via a connection of a vacuum pump provided in the chamber wall of the compartment or indirectly via an exhaust opening in the dividing wall using an adjacent pumping compartment. The operating gas can be inserted into the coating compartment via a gas inlet.
[0009] The number and the sequence of the different compartments within the coating chamber differ according to the layer or the layer systems to be produced. In complex layer systems, with their individual layers having to be applied with distinctly varying layer parameters and coating atmospheres, the entire separation of the various coating atmospheres occurs by way of gas separation, conditional for ensuring the features of the layer to the extent possible.
[0010] For this purpose, the transportation room in a pumping compartment, in which the substrate is moved through the arrangement, is separated from the exhaust room by separating walls arranged in the close proximity of the substrate and approximately parallel in reference to the substrate. This way a tunnel-shaped chamber is formed in the area of the substrate, the pumping channel, which based on its cross-section as well as the low and particularly the comparable gas pressure of the compartments, adjacent to the pumping channel at both sides, represents a flow resistance. A maximum passive gas separation can be ensured between these two adjacent compartments by appropriately designing the flow resistance. Such installations in a coating chamber require a lot of space and maintenance expense, particularly in complex coating systems, and are always exposed sites for undesired precipitations as well as sources of contaminations.
[0011] The problem of undesired precipitations and the partially resulting increased maintenance expense is increased when the coating method is executed at high temperatures, at which perhaps even the substrate is heated by a separate heating element.
[0012] Based on the high temperatures in the coating chamber, coating material or condensate introduced when the arrangement is opened collects, particularly at installations that are not heated themselves or that are mechanically and thermally connected to unheated or cooled components, e.g., the chamber wall of the coating chamber, which must be removed in a time consuming and energy intensive manner.
[0013] Therefore the object of the invention is to provide a method and a device for executing the method by which a variable processing atmosphere can be adjusted within a coating chamber of a coating arrangement in a flexible, reliable, and homogenous manner, using a reduced maintenance and energy expense, namely using the heated substrate as well.
BRIEF SUMMARY OF INVENTION
[0014] In the method according to the invention a defined atmosphere of processing gas is produced for coating a substrate inside a coating chamber by creating a flow which is aligned alternatively away from the substrate or aligned towards the substrate. Such a flow can act like a gas curtain or a gas meter in the coating chamber, depending on the flow speeds and the pressure conditions. It can be adjusted very limitedly within the coating chamber with conditions deviating from the environmental atmosphere of the processing gas and thus serve various functions.
[0015] In order to realize such particular functions, as a gas curtain or a gas meter or local eddies one embodiment of the method provides for exhausting the processing gas or inserting the processing gas through the gas channel or both in addition to the common gas inlets and gas outlets which are regularly realized by sockets or similarly suitable inlets and outlets in the chamber wall.
[0016] Based on the lateral extension of one or more flows over the width of the substrate, the homogeneity of the layer precipitation is not influenced or even improved over the width of the substrate. In one embodiment both flows, i.e., one running towards the substrate created by feeding processing gas and one aligned away from the substrate by way of suction, can be created even jointly in one coating chamber. Such a combination is also possible in the same compartment, of course if the coating chamber is divided into compartments by way of separating walls. This combination of supply and exhaustion in one volume can be used, e.g., to produce a particularly homogenous atmosphere of processing gas.
[0017] In the following, for a better overview and thus not described in greater detail, the claimed process is described for a coating chamber without any division into compartments. The method can however be used just as well for an individual compartment or several ones within a coating chamber.
[0018] The described flows of processing gas are created with the help of at least one gas channel, which is located above the side of the substrate over which a coating source is located as well. It extends over the width of the substrate and is provided with one or more openings in that extension. This gas channel is designed such that it can be optionally used both for the supply as well as for exhaustion.
[0019] In the present description the terms “above the substrate” and “upstream the coating source” are not to be understood in reference to an external system, but merely as a distanced position in reference to the substrate and/or in reference to the coating source. Thus, “above” relates both to above as well as underneath the substrate in reference to the vertical extension of the coating chamber. Therefore, the methods include coatings of substrates according to the following description, both at the top as well as the bottom and also two-sided ones. Similarly, “upstream” can represent both upstream as well as downstream the coating source. The direction of reference is here the direction of transportation of the substrate.
[0020] For the arrangement of one or more gas channels extending laterally in the coating chamber for supplying processing gas and/or exhausting processing gas closely connected to the motion and processing of the substrate performed in the chamber, of course, very different designs, arrangements, and combinations are possible depending on the motion and the processing of the substrate. Therefore, both exhausting as well as simultaneously supplying are possible in different gas channels upstream and downstream in reference to the coating source or a graduated arrangement at one or both sides of the coating source. Furthermore, a supplementary arrangement at the side of the substrate where no coating source is arranged is possible as well.
[0021] A gas channel is heated in an embodiment of the method for exhausting the processing gas and the device for performing the method. This way each surface of the exhaustion device in the coating chamber, which is cold due to the thermal connection of a gas channel to a frequently cooled chamber wall, and thus the attachment of coating material at these cold surfaces is reduced. In addition to the reduction of loss of coating material the reliability of the exhaust device is also improved and its maintenance expense is reduced, by which the energy expense is reduced for regular operation. The reduction of the precipitating coating material is of particular importance for high-rate coating methods, because the precipitating layers particularly deposit at cold surfaces.
[0022] Due to the fact that the gas channel of the processing gas supplied and thus the processing gas supplied itself can be heated it impinges the substrate at a temperature which may range approximately to that of the temperature of the substrate. This way, the precipitation of the layer and its features can be positively influenced.
[0023] In a particular embodiment of the gas channel, embodied as a heating element, in order to avoid disturbing precipitations cold surfaces are geometrically arranged such that the flow conditions are preferably not influenced in the exhaust device. For this purpose, for example cross-sections of pipelines are expanded at a location where temperatures occur below the condensation point. This creates a geometric space as large as possible, which prevents constriction in the cross-section of the flow if precipitation of the exiting coating material occurs. Such an expansion can occur in an area, e.g., in which the gas channel passes through the chamber wall and thus is in a thermal contact therewith. The determination of the relevant temperature ranges of the gas channel is to be determined by way of simulation, e.g., when knowing the temperature at which the coating process is performed, and the temperature and materials of adjacent parts.
[0024] Another advantageous embodiment of the method of the invention combines the heating of the substrate with the heating of the exhaust device by the substrate and the exhaust device being heated jointly by one or more surface heaters. This way the temperatures of the gas channels and the supplied processing gas are well approximated to the substrate temperature and simultaneously the necessary space and energy requirements are optimized.
[0025] In addition to an arrangement of a laterally extended supply of processing gas and exhaustion of processing gas the openings of the gas channel themselves are also to be designed very differently in order to yield various effects. While the openings for exhausting the processing gas should regularly be of such size that no damaging pressure drop occurs, i.e., that the performance of the vacuum pump is not reduced by a cross-section of the opening or openings being too small the flow speed then can be adjusted via the size of the opening or openings for the supply of processing gas or via the flow rate of the processing gas passing. In this case, not every pressure drop is to be considered a damaging pressure drop, because it always occurs both via the openings as well as the length of the gas channel. Rather a pressure drop is to be considered damaging when the intended special function of the flow is no longer ensured. A damaging pressure drop is to be avoided, e.g., by the diameter of the channel being large in reference to the diameter of the openings.
[0026] Depending on the pressure ratios in the coating chamber and the flow rate, various functions can be realized with the flow of the processing gas. For example, the flow of a gas curtain created adjacent to the coating source or an aperture slot in the chamber wall can be varied up to a so-called gas meter by which based on very high flow speeds the atmospheres can be influenced in a targeted manner at a defined location, e.g., in the proximity of the substrate, or contaminants or loose condensate can be removed from the substrate or kept at a distance therefrom.
[0027] Due to the fact that the gas channel can be used both for supplying processing gas as well as exhausting processing gas, adjustable openings are advantageous in the gas channel. The function of the gas channel, regardless if it is used for supplying processing gas or exhausting processing gas, is created such that a gas supply source or an exhaust device is connected to this gas channel at the side of the atmosphere.
[0028] Additionally or alternatively, in another embodiment of the device the gas channel is rotational around its longitudinal axis to adjust the lateral flow of the supplied processing gas. This way it is possible to create a flow with a variable angle in reference to the substrate level and to locally differentiate the described effects.
[0029] The creation of a laterally extended flow of the processing gas by way of its exhaustion and/or supply via the width of the substrate and the locally differentiated exhaustion also allows the coating under, for example, two processing gas atmospheres, deviating from each other with regard to their pressures, inside the same coating chamber. For this purpose, the coating chamber is divided into two coating compartments, in this case with a dividing wall, which is provided in the substrate level with a gap-shaped penetrating opening to transport the substrate through the chamber. Both coating compartments are each provided with at least one coating source and one of the above-described devices for supplying processing gas and exhausting processing gas using one or more gas channels. This way, the above-described possibilities for adjusting the processing atmosphere can be adjusted separately for each compartment.
[0030] The exhaustion is realized in both compartments over the width of the substrate and thus over the width of the penetrating openings of the chamber wall and perhaps supplemented by a gas curtain in the proximity of the penetrating opening, so that a pressure compensation between the two compartments does not occur caused by the targeted flow of the processing gas in the proximity of the slot. For the coating, based on the cooperation of the gap-shaped penetrating opening in the dividing wall and the targeted flow of the processing gas, extending parallel in reference to the penetrating opening, the embodiment of a tunnel-shaped flow resistance, extending parallel in reference to the substrate over an extended distance, as known from prior art, is unnecessary so that the device according to the invention provides considerable space savings in this case.
[0031] In order to separate the gas of adjacent compartments the described measures for producing an atmosphere of processing gas and the gas channels and heating elements used for this purpose can also be combined with the known methods for gas separation. For example, for separating gas frequently a compartment is inserted between two coating compartments, into which only inert gas is inserted, e.g., distributed over the width of the substrate. This way, via the described gas channels for exhausting processing gas, the gas coming from the intermediate chamber is exhausted in the adjacent coating compartments and an overflow of processing gas from one of the coating chambers to the next one and vice versa is prevented or at least considerably reduced.
BRIEF DESCRIPTION OF THE DRAWING FIGURES
[0032] In the following the invention shall be explained in greater detail using an exemplary embodiment. The corresponding drawing shows in
[0033] FIG. 1 a spatial section of a coating chamber in a cross-sectional illustration parallel in reference to the direction of transportation,
[0034] FIG. 2 a spatial section of a coating chamber in a cross-sectional illustration perpendicular in reference to the direction of transportation,
[0035] FIG. 3 a cross-section of a heating element with a gas channel for supplying gas, and
[0036] FIG. 4 an enlarged illustration of a section of a gas channel with a condensation chamber in a cross-sectional illustration.
DETAILED DESCRIPTION
[0037] FIG. 1 shows a section of an inner chamber of a coating chamber, through which a substrate 1 for coating is transported via a multitude of transportation rollers 2 and other suitable transportation elements of a transport system. In the following, the method shall be described using a vacuum coating, however, it is also applicable to coating methods occurring under atmospheric pressures, such as thermal gas phase reactions in so-called diffusion furnaces.
[0038] The coating chamber is divided into two coating compartments 7 via a dividing wall 4 , which abuts the upper and the lower chamber wall 5 of the coating chamber or alternatively a horizontal separating wall. Both coating compartments 7 are each provided with a coating source 6 , for example a gas phase reactor.
[0039] Due to its size and thermal load in the exemplary embodiment the dividing wall 4 is made from a carbon fiber-compound material, however, it may also comprise stainless steel, ceramics, or another material inert in reference to the processing media. In the substrate level 8 the dividing wall 4 is provided with a slot-shaped penetrating opening 10 . The penetrating opening 10 is selected of such size that the dividing wall 4 approaches the substrate 1 close enough in the circumferential direction that the vaporous coating materials are largely separated from each other and ensures an unhindered transportation of the substrate 1 .
[0040] Two heating elements 12 are arranged each at both sides of the dividing wall 4 and thus adjacent to the respective coating source 6 as well as at both sides of the coating source 6 . Each heating element 12 serves, in addition to other heating devices not shown, to heat the substrate or at least to maintain a previously adjusted substrate temperature and is arranged perpendicular in reference to the direction of transportation 3 of the substrate 1 and thus approximately parallel in reference to the coating source 6 , which extends over the entire width of the substrate (perpendicular in reference to the drawing level).
[0041] A heating element 12 is shown in detail in FIG. 3 , in a cross-sectional representation. It comprises a heat-radiating source 14 , which may provide an arbitrary suitable embodiment in order to heat the substrate via heat radiation. In the exemplary embodiment shown it is represented by the jacket surface of a cylinder, which surrounds a gas channel 16 arranged inside thereof. The heat radiation source 14 is mounted to the gas channel 16 via a suitable fastener (not shown). Based on this arrangement of the gas channel 18 in reference to the heat radiation source 14 the heat radiation source 14 simultaneously heats the substrate 1 and the gas channel 16 .
[0042] In the exemplary embodiment shown, the gas channel 16 is of a tubular shape and comprises an external tube 17 and an internal tube 18 arranged concentric in reference thereto, however it may also show a different cross-section or another shape suitable for the purposes described above. The gas to be supplied flows through the internal tube 18 and exits through one or more openings 21 into an annular gap 19 , located between the external tube 17 and the internal tube 18 , and therefrom through one or more openings 20 in the external tube out of the gas channel 16 . The annular gap 19 is adjusted to an even thickness, e.g., via spacers (not shown). The openings 21 , 22 in the internal and the external tube are offset in reference to each other such that the gas has to travel a distance in the annular gap 19 as long as possible. Due to the fact that the external tube 17 is almost entirely surrounded by the cylindrical heat radiation source 14 , the gas flowing in the annular gap 19 is to be heated to the necessary temperature. In the cylindrical heat radiation source 14 a section of the jacket surface, located opposite the opening in the external tube, i.e., the opening in the gas channel 20 , is cut such that gas exiting the gas channel can be aligned unhindered to the substrate.
[0043] By designing the geometry of the tubular diameter and the openings in the tubes the gas flow can be adjusted to the potential functions described above. In order to regulate the gas flow the size of at least the openings 20 in the external tube can be adjusted. Various shapes are suitable as openings. Either a multitude of small openings, arranged on a jacket line of the tube, or one or more slot-shaped openings are located on the jacket line of the gas channel for a lateral gas flow, i.e., extending over the width of the substrate, according to FIG. 3 of the external tube.
[0044] When in another embodiment of the heat radiation source the heating of the gas is ensured in a different manner or the flow to be adjusted requires it and also when the gas channel 16 is used for exhausting the gas, the gas channel 16 can alternatively comprise a simple, one-layer hollow body. When the gas channel 16 is used for exhausting gas, the direction of flow, shown in FIG. 3 by arrows, is to be reversed appropriately.
[0045] According to FIG. 1 , gas channels 16 according to FIG. 3 are components both of a device for supplying as well as a device for exhausting the processing gas of the coating process. The other components of both devices, not shown in greater detail, by which the processing gas is supplied to or exhausted from the coating chamber, follow the gas channel 16 . In both coating compartments 7 , one of the gas channels 16 shown serves to supply processing gas and the second one to exhaust processing gas.
[0046] As already shown, such an arrangement is only one of the numerous potential combinations of gas channels and heating elements. Additionally, it is possible that one gas channel is installed at one or both sides of the coating source for the supply and one gas channel for the exhaustion of processing gas. This way it is possible to create eddy-like gas flow adjacent to the coating source. In another embodiment, e.g., left and right from the coating source, one gas channel and one exhausting channel can be installed.
[0047] Each gas channel 16 extends over the entire width of the substrate 1 , together with the heat radiation source 14 , and is provided at least in the area in which it is located opposite the substrate 1 , with one or more of the openings 20 , described in FIG. 3 , and used for the supplying processing gas and exhausting processing gas such that a flow of processing gas develops which extends perpendicular in reference to the substrate 1 and over its entire width.
[0048] For the coating process, the substrate 1 is first moved via transportation rollers 2 in the direction of transportation 3 underneath a first heating element 12 and heated there. A gas flow 22 is aligned towards the substrate from the gas channel 16 in the first heating element 12 , by which the processing gas is supplied. The substrate is continuously moved further through the coating chamber. Underneath the first coating source 6 the coating occurs with the first coating material, using a first pressure p 1 of the processing gas. By another movement of the substrate 1 , said substrate 1 passes the second heating element 12 of this coating compartment and thus the exhaust of the processing gas, which is realized by the second gas channel 18 arranged in the heat radiation source 14 .
[0049] Subsequently the substrate 1 passes the slot-shaped penetrating opening 10 of the dividing wall 4 and thereafter the second coating compartment 7 having two additional heating element 12 and a second coating source 6 arranged between the heating elements 12 for another material precipitation. The coating of the substrate 1 with the second layer occurs at a second pressure p 2 of the processing gas, which is different from the first pressure p 1 . In the second coating compartment 7 a gas flow 22 is also created via the two gas channels 18 connected to the heating elements 12 at both sides of the coating element 6 , each extending over the entire width of the substrate 1 , flowing towards and away from the substrate 1 . The aligned gas flows 22 of the processing gases in both coating compartments 7 in the proximity of the dividing wall 4 largely prevent any gas exchange through the penetrating openings 10 of the dividing wall 4 . Such a division of the coating chamber into coating compartments 7 with different processing atmospheres may also comprise more than two coating compartments 7 .
[0050] FIG. 2 shows a heating element 12 with a gas channel 16 inside the coating compartment perpendicular in reference to the direction of transportation of the substrate. The gas channel 16 , which extends inside the heat radiation source 14 , is extended beyond the heat radiation source 14 in order to realize an assembly of the device at the lateral chamber walls 5 of the coating chamber as well as to implement the power and voltage supply and a connection 24 to a vacuum pump or alternatively to a gas supply for supplying the processing gas via this chamber wall 5 . In this case, the gas channel 16 comprises a heat conducting material so that even in this area, outside the heat radiation source 14 , it is warm enough to prevent precipitations of the coating material. At its second end, located opposite the connection 24 , the gas channel 16 is closed.
[0051] In order to maintain defined thermal conditions in the coating area and to protect the area of the chamber wall 5 with penetrations, supply units, or drives arranged thereat, heat protection devices 26 , usually heat insulating walls, are arranged at both sides of the substrate between the substrate and the chamber wall 5 . Depending on the temperature to be adjusted for the coating and the embodiment of the chamber wall 5 as well as their above-described components the heat protection devices 26 may also be omitted alternatively.
[0052] In order to perhaps precipitate transported remnants of coating material in a targeted fashion, in a particular embodiment, cold surfaces are geometrically arranged to avoid disturbing precipitations such that the flow conditions in the gas channel particularly in the exhausting device are not influenced. For this purpose, cross-sections of pipelines are expanded for example at a position where temperatures occur below the condensation point. This creates a geometric space as large as possible, which in case of precipitations of exiting coating material prevents any constriction in the conduit to develop.
[0053] According to FIG. 2 , for this purpose the gas channel 16 is provided with a condensation chamber 28 in its progression between a heat protection device 26 and the chamber wall 5 and thus the unheated and cooler section of the coating compartment, which based on its lower temperature of the jacket surface of the gas channel acts as a condensation trap. It is formed by an expanded cross-section of the gas channel 16 so that precipitations of condensed coating material influence the gas flow to a negligible extent.
[0054] Furthermore, the condensation chamber 28 is embodied separable from the gas channel 16 (shown schematically by a slot between the two of them). This results in a better thermal separation of the heated part of the gas channel 16 inside the heat radiation source 14 and thus an improved function as a condensate trap. Furthermore, the condensation chamber 28 requires less maintenance and expense for the removal of condensate.
[0055] An embodiment of the section of the gas channel 16 serving as a condensation chamber 28 is shown in FIG. 4 in an enlarged illustration. This embodiment serves such a thermal separation between the warm section of the gas channel 16 , in which no condensation shall occur, and the condensation chamber, with its temperature to be kept below the condensation temperature of the coating material.
[0056] For this purpose, in the area from the internal surface and outside the heat protection device a highly heat-conducting socket 32 is pushed onto the warm internal tube 18 of the gas channel 16 , which extends to the heat radiation source 14 and is thus heated thereby. The entire internal tube 18 is maintained at a temperature above the condensation point by this socket 32 . Alternatively, this can also occur by a separate heater, which is to be designed such that it fails to influence the function of the condensation chamber 28 adjacent thereto.
[0057] The condensation chamber 28 is thermally uncoupled from the internal tube 18 and the socket 32 of the separate heater and is located outside the heat protection device 26 . In order to support the thermal uncoupling the socket 32 or the alternative separate heater is covered by heat insulation 34 . In case such measures fail to ensure the temperature of the wall of the condensation chamber 28 , it is possible to achieve this via a thermal coupling to a cooling chamber wall 5 or an active cooling.
[0058] Of course, the penetrations of the gas channel 16 or a flange through the chamber wall 5 , shown in the schematic representations of 2 and 5 in dot-dash lines, are embodied in a completely tight fashion. The selected representation only serves to illustrate the individual components of the coating device.
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A method is provided for producing a processing atmosphere for coating substrates, with this method primarily being used in CVD-processes for precipitating an individual layer or a system of individual layers under defined processing atmospheres, in which processing gas is supplied to a coating chamber in a defined manner and exhausted. Via the method and related devices, a variable processing atmosphere is adjustable inside the coating chamber in a flexible, reliable and homogenous manner, and requiring a reduced maintenance and energy expense, even when the substrate is heated. The processing gas is created by at least one gas channel extending perpendicular in reference to the substrate by way of supplying gas flow or exhausting, with a lateral extension being equivalent to the width of the substrate.
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CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] This application claims priority to U.S. Provisional Application No. 61/026229 filed Feb. 5, 2008 which is incorporated herein by reference in its entirety.
BACKGROUND
[0002] 1. Field of the Invention
[0003] The present invention is directed to tubing, piping, conduit and the like. More particularly, the present invention relates to the coating of the interior wall or surface of pipe used in fire sprinkler or non-potable water transfer systems where the coating has a low friction composition to provide low flow resistance, both immediately and over time.
[0004] 2. Discussion of Related Art
[0005] The art of forming and coating tubes, pipes and conduits (hereinafter referred to generally as “pipe” and or “pipes”) is well-established. To form a pipe, strip steel in the form of coils is supplied from a pay-out reel in a pipe forming mill or line. The strip steel is supplied to one or more tube forming rollers in a tube forming station to bring the longitudinal edges of the strip steel together. The edges are then welded together to form a pipe having a generally circular cross-section. The pipe may be subsequently treated (e.g. galvanized) and cut to a desired length. The various steps in this process are provided are aligned along the central axis of the pipe and is continuous within a mill to produce pipe at relatively high rates of speed.
[0006] Galvanizing is a process where the formed pipe is exposed to a zinc coating on the outside wall of the pipe. Galvanizing takes advantage of the protective properties of zinc which is more resistant to corrosion than the underlying steel pipe. Advances in pipe manufacturing and galvanizing have resulted in the production of continuous pipes at rapid speeds on the order of six hundred feet per minute. Galvanizing has also progressed through the elimination of secondary or elevated zinc containers in favor of zinc pumped through cross-tees, spray nozzles and drip nozzles. Application dwell times of zinc during galvanizing have been reduced to tenths of seconds and contact zones of the pipe upon which the zinc is applied have similarly been reduced to inches. Preferred methods for coating pipes are described in U.S. Pat. Nos. 6,063,452 and 6,197,394, herein incorporated by reference. However, these processes are related to coating on the outside walls of the pipe not the inside wall of the centrally disposed pathway.
[0007] U.S. patent application Ser. No. 5,718,027 (“the '027 patent”) discloses an apparatus for the interior painting of tubing during continuous formation of the pipe which is assigned to the assignee of the present invention the contents of which are herein incorporated by reference. The '027 patent teaches the use of a spraying means which is introduced into the pipe upstream of the welding station while providing the spraying means downstream of the processing stations for forming the pipe.
[0008] Fire protection systems (e.g. sprinkler systems) employ these types of coated pipes for installation within buildings or structures to provide fire suppression liquids or suppressants throughout the premises. These sprinkler systems are engineered and designed to provide the requisite amount of fire suppression fluid (e.g. water) to the desired area. However, the pipes used in these systems degrade over time. This is due, at least in part, to the theoretical eventual roughening of the pipe's internal diameter (I.D.) surface from oxidation (rust) or microbiological induced corrosion (M.I.C.) over the life of the pipes and systems. As such, higher hydraulic friction levels (i.e., greater resistance to flow values) are designed into these systems. One method used by manufacturers of fire sprinkler piping to overcome this degradation problem is to produce plastic lined piping with a separate plastic insert sleeve within the interior pathway of the pipe. However, such plastic lined piping has poor heat resistance to fire combustion temperatures, causes changes in the dimension of the I.D. of the piping, has a high potential for delamination, and requires special tooling and fittings for pipe fabrication not routinely found in the fire protection industry. Thus, there is a need to provide a pipe that has a low hydraulic friction level for employment in fire sprinkler systems.
SUMMARY OF THE INVENTION
[0009] Exemplary embodiments of the present invention are directed to a low friction fluid transport device or pipe. In an exemplary embodiment, the low friction fluid transport device comprises a length of conduit which defines a pathway therethrough. At least one inner surface surrounds the pathway where the pathway has a transverse inner dimension. A coating of fluoropolymeric, silicone or epoxy material is disposed at least partially over the inner surface of the conduit. The material is configured to maintain the inner dimension of the conduit.
[0010] The present invention relates to the in-line coating of a continuously moving pipe or tube, preferably of the type used for applications such as fire sprinkler piping. The present invention includes a fire sprinkler pipe having a wall defining a pathway therethrough. The pathway has an inner dimension and at least one surface surrounding the pathway defined by the wall. A coating is at least partially disposed over the inner surface of the wall. The coating is configured to reduce the resistance to flow of liquid media within the pathway. The low friction coating includes, but is not limited to a fluoropolymer, silicone or epoxy composition.
BRIEF DESCRIPTION OF THE DRAWINGS
[0011] FIG. 1 is a schematic diagram of an exemplary process in accordance with the present invention;
[0012] FIG. 2 is a perspective view of an exemplary apparatus used to coat the inner surface of a pipe in accordance with the present invention;
[0013] FIG. 3 is a cross sectional schematic diagram of an exemplary conduit or pipe having a coated inner surface in accordance with the present invention.
DESCRIPTION OF EMBODIMENTS
[0014] The present invention will now be described more fully hereinafter with reference to the accompanying drawings, in which preferred embodiments of the invention are shown. This invention, however, may be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the invention to those skilled in the art. In the drawings, like numbers refer to like elements throughout.
[0015] The present invention includes a sprinkler pipe, and methods of manufacturing the sprinkler pipe having a pathway having an internal diameter (I.D.) or internal dimension where the surface surrounding the pathway is coated to maintain the I.D. and maintain the internal diameter or dimension, resistance to heat associated with fire combustion as well as providing a low hydraulic friction surface as compared to known internally painted pipes and conduit. As such, incorporation of a coating to the interior surface of the sprinkler pipe pathway results in a low resistance to flow of liquids therein for extended periods of time to maintain the operation of associated sprinkler systems. Additionally, the lower friction factor (less resistance to flow) results in conservation and reduction in the required liquid handling equipment such as the required liquid pumping power and pipe diameter for these systems.
[0016] FIG. 1 is a schematic diagram of an exemplary process for continuous fabrication of pipe. Strip steel 5 is uncoiled from a supply role 10 , cleaned and prepared in a cleaning station 20 . The strip steel 5 is then provided to a forming station 30 which includes one or more rollers to form the strip steel. The longitudinal edges of the strip steel 5 are brought together by the rollers. When the edges are contiguous, they are welded together, in line, in a seam welding station 40 to form a pipe 50 having a substantially circular cross-section and an internal pathway. Alternative cross sections including, for example, oval, square, rectangle, oblong, etc., may also be employed depending on the desired application. Typical welding temperatures for the strip steel are in the range of 2500° F. The welded pipe 50 undergoes a quench weld where water is applied around the outside of the pipe to provide sufficient cooling after the welding process. A coating is applied to the surface of the internal pathway of the pipe at station 70 . This coating may be, for example, a fluoropolymer, silicone or epoxy composition applied as liquid paint. Of these, fluoropolymers are particularly preferred. The pipe is then moved to a galvanizing station 80 in which a zinc coating is applied to the exterior of the pipe at or above the melting point of zinc which is in the range of 850° F. The fluoropolymer applied to the interior surface of the pipe can withstand the heat range associated with galvanizing. In addition, because the fluoropolymer, silicone or epoxy is applied as a liquid paint, the solvents associated with the paint must be evaporated or volatilized. This is accomplished during the galvanizing process. Alternatively, if galvanizing is not desired for a particular application, the outer surface of the pipe (which has an outer diameter (O.D.) or outer dimension) is painted at station 90 . This O.D. paint is then cured at a given temperature at station 95 as required for the particular paint. This O.D. curing process also acts to evaporate the solvents associated with the paint used for the coating applied to the interior surface of the pathway. The fluoropolymer used to coat the interior surface of the pipe may be a thermoset or a thermoplastic. If the fluoropolymer is a thermoset, the heat from the galvanizing process or the heat used to cure the O.D. paint is also used to cross-link the thermoset fluoropolymer. If the fluoropolymer is a thermoplastic, no cross-linking is required to cure the interior surface coating. After galvanizing at station 80 or paint curing at step 95 , the coated pipe 50 is cut to the desired length. In this manner, a continuous process is used to form strip steel into pipe having in which a low friction coating is applied to the interior surface of the pipe.
[0017] A fluoropolymer is preferred for coating the interior pathway of the pipe because it provides low hydraulic friction which results in less resistance to fluid flow through the pipe. In addition, the fluoropolymer coating provides a non-degrading barrier protection to the interior steel surface. A fluoropolymer is a fluorocarbon based polymer with relatively strong carbon-fluorine bonds. Because fluoroploymers have low surface energy these chemical compounds demonstrate non-stick and friction reducing characteristics. Similarly, due to the low viscosity and surface tension of the liquid paint, the coating fills in microscopic roughness of the base metal surface profile to provide a smoother, lower roughness profile which lowers water flow resistance without significantly affecting the internal flow pathway diameter of the pipe. This provides the interior pathway of the sprinkler pipe with less resistance for the flow of fire suppressant liquids therein. Consequently, less pressure is needed to displace the liquid within the fire sprinkler system and smaller diameter pipes may replace larger diameter pipes. In addition, the fluoropolymer coatings prevent the interior surface of the pipe pathway from degradation due to rusting, natural water borne minerals, water treatment chemical additives or byproducts and/or microbially influenced corrosion (M.I.C.). Moreover, the fluoropolymer coating has greater heat resistance than common paints and better resists the fire combustion temperatures subjected to steel sprinkler piping during operation.
[0018] The present invention is particularly useful in fire sprinkler piping systems needing corrosion protection, lower hydraulic friction and greater heat resistance. The Hazen-Williams equation is typically used in the design of fire sprinkler systems as well as other water piping systems. This equation is an empirical formula which relates the flow of water in a pipe with the physical properties of the pipe and the pressure drop caused by friction therein. In particular, the Hazen-Williams equation provides a relationship of the mean velocity of water in a pipe with the geometric properties or shape of the pipe and the slope of the energy line in which V=kCR 0.63 S 0.54 where k is the conversion factor the unit system (k=1.318 for US units); C is the roughness coefficient of the interior of the pipe, R is the hydraulic radius and S is the slope of the energy line. It is current sprinkler systems design practice to use the Hazen-Williams friction design factor of 120. This is used despite the fact that the actual physically occurring factor is 140-160 (lower resistance to flow than 120) because of the expected degradation of the smoothness of the interior pathway of the pipe to 120. The present invention prevents degradation of the smoothness of the internal diameter surface of the pipe. In addition, the expected 140-160 friction factor may be preserved over the life of the system without the need to design future degradation into the sprinkler system parameters. This lower resistance to flow within the pipes conserves fluid handling resources, such as lower horsepower or kilowatt pumps to provide identical flow through the pipes at lower pressure or the use of smaller diameter piping within the system. Other applications include systems having liquid flow of corrosive liquids such as, but not limited to, sewage, acidic food ingredients and/or associated by-products.
[0019] FIG. 2 illustrates an exemplary device, referred to as a lance 100 , used to apply the fluoropolymer, silicone or epoxy coating to the interior surface of a pipe 50 at station 70 (shown with reference to FIG. 1 ). The lance 100 includes a spray nozzle portion 138 connected to a hose 150 . The lance is inserted into the pipe 50 downstream of the seam weld station 40 a sufficient distance to allow the weld point to cool using the quench weld station 60 . This cooling period is needed to allow the fluoropolymer paint coating to be successfully applied to the interior surface 51 of the interior pathway 52 of pipe 50 . Otherwise the interior surface 51 will be too hot to obtain a continuous coating and will compromise the desired low friction characteristic of the interior pathway of the pipe. It has been found that a distance of approximately 15-30 feet is needed from the weld point to cool the pipe sufficiently to apply the interior coating. This distance is dependent on the pipe wall thickness where pipe walls which are thicker or heavier contain more heat than thin wall pipe due to the greater mass/unit area, and thus more heat/unit area. Transferring heat out of the heavier wall through quenching takes longer times and distances as more heat must be removed from thicker/heavier pipe. The spray nozzle portion 138 includes a spray head 140 having a hollow cone shape with a circular cross section to impart a circular pattern of the coating onto the interior surface 51 of pipe 50 . It is important to note that the coating may be applied directly to the interior steel surface of the pipe 50 or may be applied on intermediate coatings applied to the interior surface 51 prior to or in combination with application of the fluoropolymer coating. The spray device also includes a plurality of bow supports 152 which project laterally out from the spray nozzle portion 138 a consistent distance toward the interior surface 51 . This allows the spray head 140 to be centered within the interior pathway 52 for even application of the coating to the interior surface 51 of pipe 50 .
[0020] FIG. 3 illustrates a schematic cross-section of pipe 50 defined by interior pathway 52 having a central axis extending the length of the pipe. Again, although pipe 50 is shown with a generally circular cross-section, alternative geometries may also be employed having an internal pathway dimension. Pipe 50 includes a wall 53 formed from rolled strip steel having a desired thickness ‘T’ and an outer surface 54 . The interior surface 51 of wall 53 includes a coating 55 disposed thereon. The coating 55 is applied sufficiently to the interior surface to provide a low hydraulic friction surface which results in less resistance to fluid flow through the internal pathway 52 of pipe 50 . As described above, the coating 55 may be a fluoropolymer composition which is filtered and adjusted to a proper viscosity range for the application equipment described with reference to FIG. 2 . It has been found that the enhanced smoothness of the interior pathway 52 provided by the coating 55 prevents bacteria from attaching to the interior surface 51 of the pipe, as evidenced by negligible bacteria growth on tested samples. Similarly, fluoropolymers are non-biodegradable and do not act as a nutrient medium to support bacterial, viral or fungal growth. Additionally, pipes so treated had more favorable hydraulic coefficients than uncoated pipe, which may be attributable to there being no or at least significantly less microbially influenced corrosion as a result of the coatings employed in the present invention.
[0021] While the present invention has been disclosed with reference to certain embodiments, numerous modifications, alterations and changes to the described embodiments are possible without departing from the sphere and scope of the present invention, as defined in the appended claims. Accordingly, it is intended that the present invention not be limited to the described embodiments, but that it has the full scope defined by the language of the following claims, and equivalents thereof.
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The present invention relates to in-line coating of a continuously moving substrate, such as a tube or conduit, preferably of the type used for applications such as fire sprinkler piping. The present invention includes a fire sprinkler pipe defining an internal pathway. The interior surface of the pipe is coated with a low friction material such as a fluoropolymer, silicone or epoxy composition.
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BACKGROUND OF THE INVENTION
1) Field of the Invention
The present invention relates to a fluoran compound which is useful as a color forming compound in recording materials such as pressure-sensitive and heat-sensitive recording materials. More particularly, the invention relates to crystal of the fluoran compound, to a process for the preparation of said crystal and to the recording materials comprising said crystal.
2) Description of the Prior Art
Pressure-sensitive recording, heat-sensitive recording and electroheat-sensitive recording have conventionally been used as systems for recording transferred information through the mediation of external energy, such as pressure, heat or electricity, by utilizing a color reaction between a colorless or pale colored electron donative compound (color forming compound) and an organic or inorganic electron acceptor (developer).
In these recording systems, many fluoran compounds have widely been used as the color forming compound.
For example, 3-N-n-butyl-N-methylamino-7-anilino-fluoran compound has been disclosed in Japanese Laid-Open Patent SHO 59-68373(1984).
The fluoran compound represented by the formula (I): ##STR2## has been disclosed as a color developing compound in Japanese Laid-Open Patent SHO 60-47066(1985) and described to have a melting point of 101° to 103° C.
When the compound is used as a color developing material for recording materials such as a heat-sensitive recording material and mixed with a developer such as bisphenol A, the compound itself colors dark gray and provides only a dark gray colored (soiled) paper by applying the compound to a paper. Further the compound has a disadvantage of poor storage-stability such as light resistance and leads to difficulty in practical use.
OBJECT OF THE INVENTION
An object of the present invention is to improve the disadvantages of the fluoran compound of the above formula (I) as a color forming agent of the recording materials and to provide crystalline form of the fluoran compound of the formula (I) having excellent properties for use in the pressure-sensitive and heat-sensitive recording materials, particularly in the heat-sensitive recording materials.
SUMMARY OF THE INVENTION
The present inventors have carried out an intensive investigation on the properties of the recording material, heat-sensitive recording material in particular, obtained by using the compound of the formula (I). As a result, they have found that a stable crystal having a melting point higher than the conventionally known melting point exists in the compound of the formula (I) and that the stable crystal has excellent properties as a color forming compound for use in the pressure-sensitive and heat-sensitive recording materials. They have also found a process for isolating the crystal and completed the invention.
One aspect of the present invention relates to a crystal of the fluoran compound represented by the formula (I): ##STR3##
Another aspect of the invention relates to a process for preparing the crystal of the fluoran compound.
Further aspect of the invention relates to a recording material comprising the crystal.
The crystal of the fluoran compound of the formula (I) has excellent properties as a color forming compound of recording materials.
BRIEF DESCRIPTION OF THE DRAWINGS
In the drawings, FIG. 1 is a X-ray diffraction diagram of a crystal of the fluoran compound of the formula (I) which was prepared and isolated in Example 1.
FIG. 2 is a X-ray diffraction diagram of a fluoran compound of the formula (I) which was prepared and isolated in Comparative Example 1, and had a melting point of 101° to 103° C.
In each drawing, the axis of abscissa indicates an angle of diffraction (2θ) and the axis of ordinate indicates strength of diffraction.
DETAILED DESCRIPTION OF THE INVENTION
The fluoran compound represented by the formula (I) can be prepared by reacting a benzoic acid derivative of the formula (II) with a diphenylamine derivative represented by the formula (III): ##STR4## wherein R is a lower alkyl group having from 1 to 4 carbon atoms, in the presence of a dehydrating condensation agent, for example, concentrated sulfuric acid, mixture of oleum and concentrated sulfuric acid, polyphosphoric acid, phosphorus pentoxide and anhydrous aluminum chloride, preferably concentrated sulfuric acid, and thereafter bringing the reaction mixture to an alkaline pH.
The time and temperature of the dehydrating condensation reaction is not critical and is usually carried out at 0° to 100° C. for from several hours to 100 hours.
When the reaction is carried out in concentrated sulfuric acid, the preferred reaction temperature is in the range of 0° to 50° C. The reaction time depends upon the selected reaction temperature and hence the reaction is conducted for a sufficient time to permit the reaction to go to completion.
After the dehydrating condensation reaction is completed, the alkali treatment is usually carried out by addition of a base, e.g., aqueous potassium hydroxide or sodium hydroxide solution to adjust the pH to an alkaline value, e.g., 9 to 12. The treatment can be conducted in a temperature range of 0° to 100° C. The alkali treatment may be conducted in the presence of an organic solvent other than water, for example, benzene or toluene.
The reaction product thus obtained is precipitated in the form of a crystal from aromatic hydrocarbon solvents such as benzene, toluene and xylene, alcohol solvents such as methanol, ethanol, isopropanol and n-butanol, polar solvents such as acetonitrile and dimethylformamide or a mixture of these solvents. The crystal of the fluoran compound of the invention can be successively isolated in the form of a stable crystal.
Alcohol solvents or polar solvents, in particular, may be used as a solvent mixture with water. In these cases, water content in the solvent mixture is preferably 50% by weight or less, more preferably 30% by weight or less, and most preferably 10% by weight or less. When the water content exceeds 50% by weight, it becomes difficult to isolate the stable crystal.
The crystal is usually precipitated by cooling the solution obtained by completely dissolving the fluoran compound in the solvent. If desired, the fluoran compound may be completely dissolved by heating to a temperature range of from room temperature to the boiling point of the solvent. After complete dissolution, the crystal is precipitated with stirring or on standing.
No particular method is required for isolation of the precipitated crystal. Conventionally known methods such as filtration can be suitably carried out.
After isolation, the crystal may be washed with an organic solvent, for example, the above solvent containing 50% by weight or less of water, or may be dissolved again in the same solvent and precipitated in the form of the crystal.
Thus obtained crystal is dried by a usual method to obtain the crystalline fluoran compound.
In preparing the compound of the formula (I), a dehydrating condensation reaction of the compound of the formula (II) with the compound of the formula (III) is carried out in the presence of a dehydrating condensation agent such as concentrated sulfuric acid and successively alkali treatment is carried out by an aqueous alkaline solution in the presence of a substantially water-insoluble organic solvent such as benzene or toluene. The compound of the formula (I) thus formed is dissolved in the organic solvent. Consequently, in the case of conducting the alkali treatment, the crystal of the fluoran compound of the formula (I) can be suitably isolated by separating the layer of the organic solvent from the aqueous layer and successively precipitating the crystal of the fluoran compound from the solution of organic solvent.
The fluoran compounds having similar structure to the formula (I) have been known to have a different crystalline form, that is, so-called crystal modification as described in, for example, Japanese Laid-Open Patent SHO 60-202155(1985) and 62-167086(1987).
The term "crystal of the fluoran compound of the formula (I) of the invention" includes crystal modification which can exist in the fluoran compound of the formula (I) in the invention.
The crystal of the fluoran compound of the formula (I) which is suitably isolated by the above method exhibits in the powder X-ray diffraction diagram high peak at the diffraction angle (2θ) of 6.9° and relatively high peak at 19.4° as illustrated in FIG. 1. (Errors of about ±0.2° can be permitted in the indication of diffraction angle.)
The compound of the formula (I) isolated by the method disclosed in Japanese Laid-Open Patent SHO 60-47066(1985) exhibits the powder X-ray diffraction diagram illustrated in FIG. 2. FIG. 2 indicated substantially amorphous substance having a low degree of crystallinity.
This is, the crystal of the invention remarkably differs from that disclosed in Japanese Laid-Open Patent SHO 60-47066.
The crystal of the fluoran compound of the invention has a melting point of from 159° to 161° C. On the other hand, the melting point of the fluoran compound disclosed in Japanese Laid-Open Patent SHO 60-47066 has a melting point of from 101° to 103° C. Consequently, the melting point of the crystal obtained by the present invention is more than 50° C. higher than the melting point of the fluoran compound obtained by known methods.
Further, the crystal of the invention can also be prepared with ease from the above amorphous compound of the formula (I).
That is, the amorphous compound of the formula (I) is dissolved in an organic solvent having water content of 50% by weight or less, preferably 10% by weight or less. Thereafter the compound is precipitated in the form of a crystal and isolated to prepare the crystal of the invention.
The above isolated crystal of the fluoran compound of the formula (I) can be used as a color forming compound for various recording materials.
The recording materials of the present invention include pressure-sensitive recording material and heat-sensitive recording material. The crystal of the present invention is particularly suitable for use in the color forming compound of the heat-sensitive recording materials.
In such case, the fluoran compound can be used singly or as a mixture with other color forming compounds such as triphenylmethane, lactones, fluorans and spiropyrans in order to adjust the developed hue, if desired.
When preparing pressure-sensitive recording material, the crystal of the invention is dissolved in the selected solvent or a mixture of the solvent. Exemplary solvents which are commonly used in the field include alkylbenzenes such as n-dodecylbenzene, alkylbiphenols such as triethylbiphenyl and diisopropylbiphenyl, hydrogenated terphenyls, alkylnaphthalenes such as diisopropylnaphthalene, diarylenthanes such as phenylxylylethane and styrenated ethylbenzene, and chlorinated paraffins. The resulting solution is sealed by a coacervation method or an interfacial polymerization method into micro-capsules having an external wall comprised of gelatin, melamine-aldehyde resin, urea-aldehyde resin, polyurethane, polyurea and polyamide or the like. Aqueous dispersion of the micro-capsules is mixed with a suitable binder, such as starch and latex, and applied to a suitable substrate such as paper, plastic sheet or resin coated paper. The coated back sheet for pressure-sensitive recording is thus obtained.
The capsule dispersion can, of course, be used for a so-called middle-sheets by applying the above capsule dispersion to one side of a substrate and applying a coating liquid primarily containing a developer to the other side of the substrate. A so-called self contained sheets can also be prepared by applying a coating liquid containing both the above capsule and the developer to one side of a substrate, or by applying a coating liquid of the capsule to a substrate and successively applying a coating liquid of the developer on the coated layer of capsule to exist the above capsule and the developer on the same side of the substrate.
Exemplary developers suitable for use in pressure-sensitive recording material include copolymers of salicylic acid, phenols and aldehydes, for example, formaldehyde resin; alkyl, aryl or aralkyl substituted salicylic acid such as 3,5-di-α-methylbenzylsalicylic acid; polycondensate of substituted salicylic acid and styrene; alkylphenols such as octylphenol; phenol aldehyde resin such as p-phenylphenol novolak resin; metal salts of these compounds such as zinc, magnesium, aluminium, calcium, tin and nickel salts; and activated clays.
When preparing a heat-sensitive recording material of the invention, the crystal of the fluoran compound of the formula (I) and the developer are pulverized in water to form an aqueous dispersion. The fine particle dispersion thus obtained is then mixed with a binder and a filler.
Representative examples of the developer which are suitable for use in the heat-sensitive recording material include bisphenol A, halogenated bisphenol A, alkylated bisphenol A, dihydroxydiphenyl sulfone, halogenated dihydroxydiphenyl sulfone, alkylated dihydroxydiphenyl sulfone, hydroxybenzoic acid esters, hydroquinone monoethers and other phenol derivatives; salicylic acid derivatives, salicylamide derivatives, urea derivatives, thiourea derivatives and other organic developers; and acid clay, attapulgite, activated clay, aluminum chloride, zinc bromide and other inorganic developers.
Exemplary binder used for the heat-sensitive recording material includes polyvinyl alcohol, modified polyvinyl alcohol, methylcellulose, hydroxyethylcellulose, carboxymethylcellulose, gum arabic, salt of styrene-maleic anhydride copolymer, and isobutylene-acrylic acid-maleic anhydride copolymer. Exemplary fillers which can be used include talc, kaolin and calcium carbonate.
Other additives can also be employed, if necessary. Exemplary additives include sensitizers such as higher fatty acid amides, aromatic carboxylic acid esters, aromatic sulfonic acid esters, aromatic ethers, aromatic substituted aliphatic hydrocarbons ethers, aromatic hydrocarbons, aromatic substituted aliphatic hydrocarbons and other generally known sensitizers for the heat-sensitive recording material; UV-absorbers; and defoaming agents.
The coating liquid obtained by the addition of the above additives can be applied to a suitable substrate such as paper, plastic sheet and resin coated paper, and used as the heat-sensitive recording material. The heat-sensitive recording system of the invention can of course be used in a solvent system without any problem in place of the above aqueous dispersion system. The system of the invention can also be employed for other end use applications using color forming materials, for example, a temperature-indicating material.
In the pressure-sensitive recording material, the crystal of the present invention gives high solubility in capsule oil and excellent weatherability of developed image which are important characteristics strongly desired for the color forming compound of the pressure-sensitive recording material.
Solubility of the crystal of the present invention in marketed capsule oil was compared with the solubility of the fluoran compounds of the formulas (A), (B) and (C), respectively. Results are illustrated in Table 1.
In the test, 5 parts by weight of each compound were respectively dissolved by heating in 100 parts by weight of each capsule oil. The solutions obtained were allowed to stand at 5° C. for a week. Thereafter existence of precipitated crystal was observed. ##STR5##
TABLE 1______________________________________Capsule oil SAS - 296 KMC - 113______________________________________Crystal of the Invention ◯ ◯Compound of the formula (A) X XCompound of the formula (B) X XCompound of the formula (C) X X______________________________________
In Table 1, ◯ means that no crystals are precipitated and × means that precipitation of crystals is observed.
SAS-296 is a capsule oil produced by Nippon Petrochemical Co., and KMC-113 is a capsule oil produced by Kureha Chemical Co.
As clearly illustrated in Table 1, the crystal of the present invention has higher solubility in each capsule oil, in contradistinction to the fluoran compounds of the formulas (A), (B) and (C).
These results means that crystal precipitation does not occur during storage in capsule oil in the preparation of the pressure-sensitive recording material, and further that crystal precipitation in the microcapsules is not liable to occur after preparation of the microcapsules. The property is a remarkable characteristic of the crystal of the present invention.
The heat-sensitive recording material prepared by using the crystal of the present invention has extremely excellent properties as compared with the recording material obtained by using the compound of the formula (I) which is prepared by the process disclosed in Japanese Laid-Open Patent SHO 60-47066(1985) and has a melting-point of 101° to 103° C., or by using the known compound of the formula (D). For example, when bisphenol A is used as a developer, the heat-resistant recording paper obtained by the process of the invention is very excellent in whiteness (brightness) of paper immediately after application of the coating liquid and in storage stability, i.e., resistance to light, moisture and heat, of uncolored portion of the coated paper, as illustrated in Table 2. ##STR6##
TABLE 2______________________________________ Immediately Moisture after Light and heatCompound application resistance resistance______________________________________Crystal of ◯ ◯ ◯the inventionFluoran X X Xcompound ofm.p. 101-103° C.Compound of X X Xformula (D)______________________________________
Results were evaluated by visual observation. Evaluation at immediately after application was conducted by observing the brightness of the paper.
______________________________________ ◯ . . . High brightness X . . . Soiled to dark gray______________________________________
Evaluation of light resistance was conducted by inspecting the degree of yellowing in the uncolored portion after exposure to sun-light for 10 hours.
______________________________________◯ . . . Almost no yellowing and maintain high brightnessX . . . Remarkable yellowing or discolored to yellow brown.______________________________________
Evaluation of moisture and heat resistance was conducted by examining the soiling of the uncolored portion after storage at 60° C. for 24 hours in 90% relative humidity.
______________________________________◯ . . . Almost no soiling and high brightnessX . . . Remarkably soiled to dark gray______________________________________
Further, the heat-sensitive recording material prepared by using the crystal of the present invention provides a developed image having very excellent storage stability. For example, when bisphenol A is used as a developer, the heat-sensitive recording paper prepared by using the crystal of the present invention as a color forming compound provides a developed image having very excellent water resistance as compared with the image obtained by using the compound of the formula (E) as illustrated in Table 3. ##STR7##
The water resistance test was carried out by using the heat-sensitive recording paper prepared by using each compound. The recording paper having a developed color density of 0.9 measured with a Macbeth reflection densitometer (Trade Mark; TR-524) was immersed in water at 25° C. for 24 hours.
Color density after water resistance test and residual rate are illustrated in Table 3. ##EQU1##
TABLE 3______________________________________ Color density ResidualCompound after test rate (%)______________________________________Crystal of the 0.65 72inventionCompound of 0.14 16formula (E)______________________________________
As clearly seen in Table 3, the heat-sensitive recording paper prepared by using the compound of the formula (E) developed image having poor water resistance. By visual inspection, the image had been almost disappeared after the water resistance test.
The present invention will hereinafter be illustrated further in detail by way of examples. However, it is to be understood that the invention is not intended to be limited to the specific embodiments.
EXAMPLE 1
In 720 g of 96% sulfuric acid, 107 g of 2-(4'-N-isobutyl-N-methylamino-2'-hydroxybenzoyl)benzoic acid was dissolved at 10° to 15° C., and then 70 g of 4-methoxy-2-methyldiphenylamine (the compound of the formula (III) wherein R is methyl) was added at the same temperature. The mixture was stirred at 10° to 15° C. for 24 hours and poured into 4000 ml of ice water. Precipitated solid was collected, washed with water, and added to 1000 ml of a 10% aqueous sodium hydroxide solution. Further 1000 ml of toluene was added to the mixture thus obtained and stirred for 2 hours at 60° to 70° C. Toluene layer was seperated, washed with warm water until the wash water becomes neutral, and the resulting toluene layer was concentrated at 40° C. under reduced pressure. Precipitated crystal was filtered, washed with a small amount of toluene, further washed with methanol, and dried at 60° C. for 24 hours to obtain 126 g of the fluoran compound of the formula (I) as a colorless crystal having a melting point of 159° to 161° C.
The toluene solution of the compound was colorless and transparent, and quickly developed reddish black color on silica gel.
In 95% acetic acid solution, the compound had maximum absorption at 455 nm and 594 nm.
Powder X-ray diffraction diagram is illustrated in FIG. 1.
COMPARATIVE EXAMPLE 1
(Preparation of the compound of the formula [I] by the process disclosed in Japanese Laid-Open Patent SHO 60-47066).
In 150 g of 96% sulfuric acid, 16.4 g of 2-(4'-N-isobutyl-N-methylamino-2'-hydroxybenzoyl)benzoic acid was dissolved at 10° to 15° C., and then 10.7 g of 4-methoxy-2-methyldiphenylamine was added at the same temperature. The mixture was stirred at 10° to 15° C. for 24 hours and poured into 800 g of ice water. Precipitated solid was filtered, washed with water, and added to 800 ml of water. To the resulting mixture, 200 ml of a 10% aqueous sodium hydroxide solution was added and stirred for 2 hours at 60° to 70° C. The solid was filtered, washed with water and dried to obtain 24 g of dried product. The dried product was washed with 30 g of ethylene glycol and then dissolved in 500 g of a 60% aqueous methanol. Thereafter, solid reprecipitated from the solution was filtered and dried at 30° C. to obtain 13.5 g of white solid powder like having a melting point of 101° to 103° C.
Powder X-ray diffraction diagram is illustrated in FIG. 2.
EXAMPLE 2
Ten grams of the amorphous compound of the formula [I] prepared in Comparative Example 1 were added to 80 ml of isopropanol and dissolved at 60° C. The solution was cooled to room temperature. Precipitated crystal was filtered and dried to obtain 9 g of colorless crystal having a melting point of 159° to 161° C.
Powder X-ray diffraction diagram was the same as in Example 1.
EXAMPLE 3
(Preparation of heat-sensitive recording paper by using the crystal of the invention)
A mixture composed of 10 g of the crystal obtained in Example 1, 5 g of a 10% aqueous polyvinyl alcohol solution and 37.5 g of water was pulverized with a sand mill to a particle size of 3 μm.
Separately, bisphenol A was dispersed similarly to obtain a 38% aqueous developer dispersion. A mixture was prepared by mixing 65.8 g of the developer dispersion, 50 g of the above dispersion of the crystal, 18.3 g of a 60% aqueous dispersion of precipitated calcium carbonate, 88 g of a 10% aqueous polyvinyl alcohol solution and 51.9 g of water.
The mixture was applied to a white paper with a wire rod No. 10 and dried at room temperature to obtain heat-sensitive recording paper having high brightness without soil. The heat-sensitive recording paper very quickly developed slightly reddish black color by heating.
After exposing the heat-sensitive recording paper to sunlight for 20 hours, the uncolored portion caused almost no yellowing and retained high brightness. After storing at 60° C. for 24 hours under 90% relative humidity, the uncolored portion caused no soil and retained high brightness as illustrated in Table 2.
When the heat-sensitive recording paper was developed to an image density of 0.9 and immersed into water at 25° C. for 24 hours, residual rate of the image was good as illustrated in Table 3.
COMPARATIVE EXAMPLE 2
(Preparation of heat-sensitive recording paper by using the fluoran compound of the formula (I) which was obtained in Comparative Example 1 and had a melting point of 101° to 103° C.).
A heat-sensitive recording paper was prepared by carrying out the same procedures as described in Example 3 except that the crystal isolated in Example 1 was replaced by the compound obtained in comparative Example 1. The paper was already soiled to dark gray immediately after coating. After exposing the recording paper to sunlight for 20 hours, remarkable yellowing was found on the uncolored portion.
After storing the recording paper at 60° C. for 24 hours under 90% relative humidity, the uncolored portion was remarkably soiled to dark gray as illustrated in Table 2.
COMPARATIVE EXAMPLE 3
(Preparation of heat-sensitive recording paper by using the fluoran compound of the formula (D))
A heat-sensitive recording paper was prepared by carrying out the same procedures as described in Example 3 except that the crystal isolated in Example 1 was replaced by the fluoran compound of the formula (D). The paper was already soiled to dark gray immediately after coating. After exposing the recording paper to sunlight for 20 hours, remarkable yellowing was found on the uncolored portion.
After storing the recording paper at 60° C. for 24 hours under 90% relative humidity, the uncolored portion was remarkably soiled to dark gray as illustrated in Table 2.
COMPARATIVE EXAMPLE 4
(Preparation of heat-sensitive recording paper by using the fluoran compound of the formula (E)).
A heat-sensitive recording paper was prepared by carrying out the same procedures as described in Example 3 except that the crystal isolated in Example 1 was replaced by the fluoran compound of the formula (E). The recording paper was developed to image density of 0.9 and immersed into water at 25° C. for 24 hours. After immersion, the image density was remarkably decreased and the image was almost disappeared as illustrated in Table 3.
EXAMPLE 4
(Preparation of pressure-sensitive recording paper by using the crystal of the invention)
Coated back sheet (CB) and coated front sheet (CF) were prepared by the following procedures.
A mixture of 100 g of a 10% aqueous solution of ethylene-maleic anhydride copolymer and 240 g of water was adjusted to pH 4.0 with a 10% aqueous sodium hydroxide solution and mixed with 200 g of a solution containing 5% by weight of the crystal obtained in Example 1 in phenylxylylethane (SAS-296; Trade Mark of Nippon Petrochemical Co.). Afters emulsifying the resultant mixture with a homomixer, 60 g of an aqueous methylolmelamine solution containing 50% of solid (Uramine T-30; Trade Mark of a product of Mitsui Toatsu Chemicals Inc.) was added, and stirred at 55° C. for 3 hours to obtain a microcapsule dispersion having an average particle size of 5.0 μm.
To 100 g of the microcapsule dispersion, 40 g of wheat starch particle, 20 g of a 20% paste of oxidized starch and 116 g of water were added and dispersed.
The dispersion thus obtained was applied on a paper having a basis weight of 40 g/m 2 so as to obtain a coating of 5 g/m 2 as solid. CB sheet was thus obtained.
On the other hand, CF sheet was prepared by using zinc salt of substituted salicylic acid-styrene copolymer as a developer. The zinc salt was pulverized in water with a sand grinding mill in the presence of a small amount of a high molecular weight anionic surfactant to obtain an aqueous dispersion with a 40% by weight of solids content.
Using the aqueous dispersion, a coating compound (30% solid content) having the below described composition was prepared and applied on a woodfree paper having a basis weight of 40 g/m 2 so as to obtain a coating weight of 5.5 g/m 2 after drying. A CF sheet was thus obtained.
______________________________________ Weight of solidAqueous Coating Composition (g)______________________________________Precipitated calcium carbonate 100Developer 20Binder(Oxidized starch) 8(Synthetic latex) 8______________________________________
The microcapsule coated CB sheet and the developer coated CF sheet were overlapped so as to bring both coated surfaces into contact with each other.
When pressure was applied on the overlapped sheets with a pencil, a reddish black image emerged on the developer coated surface. The developed color image had no problem on resistence to light, moisture and NOx in practical use.
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Disclosed are novel crystal of the fluoran compound represented by the formula ##STR1## , characterized by a specific X-ray diffraction diagram; preparation process thereof; and recording materials comprising the crystal.
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This is a division of application Ser. No. 885,377, filed Mar. 10, 1978, now U.S. Pat. No. 4,177,740.
BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention pertains to methods and apparatus for generating heat from particulate-laden gas or directly from waste fuels such as wood waste.
2. Description of the Prior Art
Wood waste fuel burners, commonly known as hog fuel burners, have generally been extremely inefficient in combustion, discharging undesirable amounts of gaseous and particulate pollution. In addition, when these burners are coupled to a boiler the gases emitted to the boiler for heating are dirty causing depositions on the heat transfer tubes of the boiler which require frequent and expensive cleaning. Frequently, the particulate matter in the exhaust gases is also highly abrasive to the boiler heat transfer elements. As a result, conventional practice is to build an extremely large furnace chamber for a boiler allowing the discharge gases from the burner to reach a very low velocity so that particulate matter in the exhaust can drop out of the gas stream. Also, because of retained particulate matter, the gas passages in the tube banks of conventional boilers are generally made wider to minimize passage obstruction. Gas velocities of 50 to 60 ft./sec. are common in hog or wastewood fuel boilers while velocities of 110 to 120 ft./sec. are the rule in oil and gas fired packaged or field erected boilers. And lastly, once through the boiler, the economizer and the air preheater, the exhaust gases in conventional hog fuel boilers have to be cleaned in multiple cyclones (multicones) followed, typically, by electrostatic precipitators. What the industry has long needed is a clean burning waste fuel burner which can deliver exhaust gases as clean as those produced by oil and gas burners. The same burner could also replace oil and gas burners on lime kilns, plywood veneer dryers, particle board dryers, lumber dry kilns, etc.
SUMMARY OF THE INVENTION
It is an object of this invention to provide a waste fuel burner which emits discharges of very minimal quantities of particulate materials within the levels permitted by local environmental regulations.
It is another object of this invention to provide a waste wood fuel burner which operates producing little slag or clinkers.
It is another object of this invention to provide a waste wood fuel burner which can effectively burn wet wood of 70% moisture content (wet basis).
It is still another object of this invention to provide a waste fuel burner that is self-regulating, easy to control and has fast response times to changes in the load comparable to conventional gas and oil burners.
It is another object to provide a waste fuel burner that burns wood of nominal ash content (e.g. 5% ash) and produces a residue that is free of clinkers (assuming the ash fusing temperature is not lower than 1700° F.)
Basically, these objects are met by method and apparatus which forms a conical pile of waste fuel, fed from below, with preheated underfire air percolating up through the pile in controlled amounts, drying and gasifying the waste fuel in the pile. The volatile gases driven off the pile by heat generated by the oxidation of the fixed carbon on the surface of the pile are then partially oxidized by additional combustion air introduced tangentially with a very vigorous swirl in a first or primary combustion chamber with the total amount of combustion air admitted to the primary chamber being maintained at less than stoichiometric proportions so that the temperature in the primary combustion chamber remains lower than the necessary to melt the natural ash, dirt or other inorganic substances in the fuel. The additional or swirl air is introduced in an amount necessary to maintain a steady temperature at the exit of the primary chamber and is dependent upon the moisture content and type of fuel. The swirl air also forces particulate out of the gas stream leaving the primary chamber. The volatile gases are discharged from the throat of the primary combustion chamber around an air cooled disc or flame holder which forces the gases, and any entrained particulate matter, out to the walls of the throat, thereby causing such entrained matter, if any, to centrifugally separate and fall back into the primary chamber. That is, the flame holder serves as a barrier against the particulate but allows passage of gases therearound. The volatile gases move around the disc shaped flame holder into a second combustion chamber where secondary combustion air is introduced to an amount above stoichiometric proportions for complete combustion. The secondary air introduced in the secondary combustion chamber is directed tangentially. Preferably, the combustion air introduced to the primary and secondary chambers is introduced on the outside of a refractory lining to cool the lining and increase its life. Preferably, also, the secondary combustion air introduced in the secondary combustion chamber can be introduced at various axial locations in that chamber to regulate the position of the flame within the chamber. Finally, if desired, additional blend air can be added to the discharge of the secondary chamber to cool the air for industrial purposes other than boiler heat.
The swirl air and secondary combustion air combine or interact dependent upon moisture content of the fuel to maintain good separation of the particulate from the gas stream leaving the primary chamber thus keeping the particulate out of the secondary chamber where high temperatures could cause slag formation. For example, as moisture content rises the temperature in the primary chamber will drop causing a demand for more swirl air to raise the combustion temperature in the primary chamber. This swirl air will vigorously separate the particulate by centrifugal separation. If moisture content drops, the temperature in the primary chamber will increase thus reducing the need for swirl air to maintain the steady exit temperature. As swirl air is reduced however the secondary air begins to shift downwardly because of the reduced pressure in the primary chamber thus diverting particulate trying to leave the primary chamber back into the primary chamber. That is, the secondary combustion air travels down in a spiral along the wall of the secondary chamber, then moves across the exit of the primary chamber and joins with the upwardly rising inner vortex of combustion gases above the flame holder. Particulate is swept back down into the primary chamber by this action.
In a second embodiment a cylindrical restriction or pressure isolator fitted with a multiplicity of radial vanes is coupled to the air cooled flame holder. The restriction serves to isolate the primary chamber from the secondary chamber air by imposing an additional resistance to tangential secondary combustion air movement into the two primary chamber but, at the same time permits the free fall of any separated particulate matter back into the primary chamber.
A unique aspect of the invention is that while advantageously used for a wood waste burner the primary and secondary chambers can be added to any source of dirty particulate-laden combustible gas and effectively burn the gas to provide a source of useful heat and remove the particulate for meeting environmental emission standards. As an example the primary chamber can be coupled directly to the exhaust of a coking operation for burning the gases and removing particulate from the exhaust.
BRIEF DESCRIPTION OF THE FIGURES OF THE DRAWING
FIG. 1 is an axial partial section of a waste fuel burner embodying the principles of the invention.
FIG. 2 is a fragmentary section taken along the line 2--2 of FIG. 1.
FIG. 3 is a fragmentary detail section of a second embodiment incorporating a pressure isolator.
FIG. 4 is a schematic pneumatic control diagram.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
The burner includes a primary combustion chamber 10 having an internal side wall 11, a discharge opening 12 and a bottom 13. The chamber is lined with refractory material 14 which is spaced from an outer metallic shell 15 by an air cooling passage 16.
Fuel (where the combustible material is a solid wood waste rather than merely particulate-laden gas) is fed from a hopper by a conveyor 18 of conventional construction either of the screw or ram type and is pushed into the form of a conical pile F. Preheated underfire combustion air is carried by a conduit 20 and directed into two chambers 20a and 20b. The chambers are in effect concentric rings each being fed a regulated desired amount of air to percolate or blow up through the pile. This air is preheated to about 500° F. The ring 20a being located beneath the outer less thick level of the conical pile is held to a lower air pressure so that blow holes will not be formed in the pile. Blow holes disturb the gasification and result in underfire air completing the combustion of the volatiles generated in the region of the blow hole, leading to high temperatures in the same region with attendant ash fushion and clinker generation.
High pressure swirl air is admitted through tuyeres 22. The tuyeres are at an angle to the side wall 11 so that the air is admitted tangentially and the resulting swirl generates centrifugal forces which drive the heavier non-combusted materials to the outer wall 11 while allowing the volatile gases to pass upward through the throat of the primary chamber. The tuyeres 22 are located high up in the chamber side wall so that the air introduced will not disturb the surface of the pile of fuel. The tuyeres have a wedge-shaped portion 23 with a plug wedge 24 that is externally adjustable by a handle 26. Thus each of the tuyeres which are circumferentially spaced around the primary combustion chamber are individually adjustable to regulate the exact amount of air and the velocity of this air introduced into the primary combustion chamber.
The secondary chamber also is provided with a side wall 33, a roof 34, an outlet 36 and a refractory lining 38 on the side walls and roof. The refractory lining is separated from the outer shell by an air passage 39 for cooling the refractory lining. Additional or secondary combustion air is introduced at tuyeres 40a, 40b, and 40c which are circumferentially and axially spaced within the secondary combustion chamber. These tuyeres are all adjustable in the same manner as the tuyeres of the primary combustion chamber. The axial positioning of the tuyeres is effective for adjusting the location where the air is introduced into the secondary chamber and assists in positioning the flame for various types of fuels and moisture contents of fuels.
As best shown in FIG. 1, the volatile gas passing through discharge 12 from the primary chamber works its way past an air cooled horizontal, disc shaped flame holder, 44, upon entering the secondary chamber. The flame holder is positioned in the center of the secondary chamber, below the bottom row of tuyeres 40c and causes the primary chamber gases to flow radially outward and around the flame holder forming again directly above the flame holder in an inner vortex. The flame holder could be ceramic but in the preferred embodiment is air cooled by admitting secondary air via hollow support pipes 43, the flow of cooling air being established by bleeding such air from the outer surface of the flame holder via a plurality of small diameter bleed holes 45.
Secondary combustion air is admitted tangentially to the secondary chamber via three rows of adjustable tuyeres 40a, 40b, and 40c. Because of the roof 34 and choke 36, the secondary combustion air spirals down the walls of the secondary chamber to meet the mixture of volatile gases and moisture spiraling up around the flame holder from the primary chamber. The two flows merge and, still swirling, flow radially inward above the flame holder where final combustion takes place.
Combustion is completed in this inner vortex of upward spiralling flame centered above the flame holder and along the axis of the secondary chamber. The inner vortex is surrounded, and the refrectory is protected, by the outer vortex of downward spiraling combustion air. The final products of combustion leave the secondary chamber through the choke 36 still spiraling, at temperatures which, depending upon the moisture content of the waste fuel and the quantity of excess air, can reach 3000° F.
The flame holder also serves as a barrier and prevents the secondary chamber inner vortex from drawing primary chamber particulate material up into the secondary chamber.
Should some primary chamber particulate find its way out of the primary chamber into the primary chamber throat and then past the flame holder into the secondary chamber, the flame holder forces it out towards the walls where it is acted upon by the various outer vortex of the secondary chamber. Because of the smooth and continuous transition of the secondary chamber walls with those of the throat of the primary chamber, such elusive particles then fall back down into the primary chamber where the combustible portion will later be removed.
In the embodiment of FIG. 3 a pressure isolator 33 is shown in the throat of the primary chamber below the flame holder 44. The isolator shown is a thin walled circular cylinder supported by a plurality of radial vanes 64 of the same axial length as the circular cylinder which extend from the outer surface of said cylinder to the throat walls. The entire pressure isolator can be air cooled in a similar manner to the flame holder.
The purpose of the pressure isolator is to isolate the primary chamber from secondary chamber combustion air. Because of the radial vanes the resistance presented to the downward spiraling secondary combustion air is high (the radial vanes destroy the angular momentum) the tendency for this air to enter the primary chamber is minimized. The primary chamber volatiles, however, readily find their way up through the center of the pressure isolator and into the secondary chamber. Any particulate matter brought with these gases into the secondary chamber is thrown outwards as before and because of the open passages between the refractory walls and the outer surface of the central cylinder, falls back down into the primary chamber.
The quantity of high pressure swirl air admitted to the primary chamber is varied according to the primary chamber exit temperature measured by thermocouple 70. Should this temperature fall too low and jeopardize either the rate of gasification in the primary chamber or continuous ignition in the secondary chamber, then the amount of primary swirl air is increased by the burner controls. Similarly, if the primary chamber exit temperature rises above an acceptable limit, and possibly melt, or, at least, cause to coalesce some of the noncombustible matter in the fuel, then the amount of primary swirl air is decreased by the burner controls.
In the latter case the reduction of swirl air will reduce the centrifugal separation forces on primary chamber particulate matter. However, this reduction will be offset by an increase in the centrifugal separation forces in the secondary chamber as follows: the increase in volatile matter reaching the secondary chamber will produce higher temperatures in this chamber as measured by thermocouple 72. The secondary chamber controls will then call for more secondary air to lower the secondary chamber exit temperature. This additional secondary air results in higher tengential velocities at the walls of the secondary chamber leading to an increase in centrifugal separation forces in this chamber.
Conventional gas burners 28 are mounted in the sides of the primary and secondary chamber. The primary chamber gas burner serves to ignite the fuel pile on start-up while the secondary chamber burner serves to preheat the secondary chamber and complete the combustion of the initial low temperature gases coming from the primary chamber during start-up.
To summarize the principle of operation, most conventional hog fuel or waste fuel burners are run with an air supply considerably greater than that necessary for stoichiometric combustion. Stoichiometric combustion, as is well known, is the precise amount of air necessary to obtain complete combustion of the organic materials in the waste fuel. This quantity of air will vary depending on moisture content and the nature of the fuel. Conventional hog fuel burners burn intentionally with about 80% more combustion air than is needed for stoichiometric combustion. The reason for this is that because the moisture content, and nature of the fuel is continuously varying the prior art burners overcompensate to assure that they get above stoichiometric so that combustion is complete and no undesirable smoke is formed. Generally, however, in operation these prior art burners reach excess air levels of up to 200%. This is extremely wasteful since the air must be delivered by blowers and reduces the final exhaust temperature because of the dilution of the heated gas with excess cool air. The invention described in this application burns considerably below stoichiometric proportions in the primary combustion chamber where slag-forming non-combustible material is found and only about 20% excess of stoichiometric in the secondary chamber. Furthermore, since all of the drying of the fuel occurs in the primary combustion chamber the gases reaching the secondary combustion chamber are uniform in nature allowing fuels up to 70% moisture content to be burned with good performance. By running at such a low excess air the temperatures in the primary chamber can be easily maintained below 1600° F.
Other advantages of this invention are that it can be adjusted to operate with a low volume of fuel or a high volume of fuel being variable from approximately x million Btu/hr to x/5 million Btu/hr where x is the burner rating; since not only can the feed of fuel be controlled quickly, but the underfire air coming in through conduit 20 can also be shut down quickly giving a response time in changing the output Btu/hr of the heater of less than 1 minute. This is to be compared to conventional prior art pile burners which require as must as 30 minutes to change their Btu output. The advantage of the quick response time is that the demands of the boiler can be more quickly met. Still another advantage is that since very little clinker or slag formation is formed in the primary and secondary chambers only very infrequent cleaning is needed and the cleaning is primarily limited to dry ash removal. Since the combustion air is passed over the refractory lining the lining has a much longer life because it seldom exceeds temperatures of about 1200° F. Even when the highest temperature region of the flame in the secondary chamber is as high as 3000° F. Still further, with applicant's invention, the size and quality of the pieces of fuel fed to the pile is not critical whereas in the prior art, many systems require that the fuel be first pulverized or made of uniform size before it can be efficiently burned.
The discharge gases from the secondary chamber 32 can go direct to the boiler and because of their cleanliness the boiler can be small and obtain high heat transfer by maintaining the high velocity of the gases. If used for other industrial purposes requiring a lower temperature the gases can be mixed with additional outside air in a blend chamber 50 with its discharge going to a kiln dryer or other industrial use. Part of the hot gases are tapped off via conduit 54 and used to preheat underfire air in a heat exchanger 65.
The description of the control schematic shown in FIG. 4 wil further illustrate the principle of operation.
BTU demand of the heat consuming process or equipment such as a boiler establishes burner output. In an actual installation steam pressure (boiler), dry bulb temperature (dry kiln) or tail end temperature (rotary dryer) alter the burner's BTU demand set point.
BTU demand controls the air and wood feed rate. There are three fans supplying underfire, swirl and secondary air. Each fan's output is affected by the demand signal. Fan output is controlled by an outlet damper at each fan.
The BTU demand signal is fed in parallel to: (1) an hydraulic pump 69 which powers an hydraulic motor 80, the motor 80 drives a wood supply conveyor which delivers wood waste to a conventional reciprocating ram stoker 81; (2) the underfire fan damper actuator 84; (3) the swirl air fan damper actuator 85; and (4) the secondary air fan damper actuator 86.
As demand increases, each of the fan outputs and the wood flow increase. Conversely, as demand decreases the wood and air supplied decrease.
The speed of the hydraulic motor (i.e. wood flow) is maintained constant for that demand setting by comparing the output of a tachometer 90 with the demand setting and automatically adjusting the hydraulic pump actuator accordingly (via a conventional controller 81).
Overrides or trims are provided on the swirl air and secondary air quantities. The swirl air is trimmed by the temperature at the outlet from the primary chamber. This temperature is measured by a probe 70 at the outlet of the primary chamber 10. The secondary air is trimmed by either the temperature at the outlet from the secondary chamber or the oxygen level at that point. This temperature, for example, is measured by a probe 72 above the outlet of the secondary chamber 32.
The swirl air trim drops the primary chamber outlet temperature by providing less combustion air and thus burning less of the volatiles in this chamber. That is, as the temperature gets higher than a preset set point the quantity of swirl air is reduced to lower the primary chamber exit temperature. Since the reduced swirl air will reduce particulate separation due to less cyclonic action, particulate separation from the volatile gases is maintained by the cyclonic action of the secondary air immediately above the primary chamber outlet. Advantageously as swirl air is reduced because of high temperatures in the primary chamber (a condition of low moisture content in the wood) the quantity of secondary air is increased to prevent excessive temperatures in the secondary chamber. The additional secondary air will increase cyclonic action in the secondary chamber thus driving the particulate outwardly and downwardly back into the primary chamber. Finally the secondary air trim increases the secondary air to maintain outlet temperatures from the secondary chamber compatible with long refractory life. When oxygen is used to trim the secondary air (for example, on a boiler) then the secondary air is normally reduced to maintain a fixed excess air (15 to 20% nominally).
The underfire air is the gasifying air, that is, the air which provides the volatiles to be burnt above the pile and especially, in the secondary chamber. In fact, while all other air controls operate only on the cruder accuracy outlet damper position, the underfire air control operates on the pressure drop across an inlet orifice 104 to determine actual air flow. BTU demand calls for a certain underfire air flow which is then established by the outlet damper actuator 84.
The fresh underfire air is pre-heated in a heat exchanger 90. The underfire air supply temperature is controlled from a thermocouple 91 which controls an exhaust damper 92 from the hot gas side of the heat exchanger.
Manual or automatic selection controls 98 are provided in each control circuit to allow manual override of each trim control. The embodiment of the control system disclosed is pneumatic. However, electrical controls are also satisfactory.
While the preferred embodiments of the invention have been illustrated and described it should be understood that variations will be apparent to one skilled in the art without departing from the principles herein.
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A combustion method in which heat is generated from particulate laden combustible gas containing mineral matter created from gasifying waste wood, coke or other combustible material in which the waste is fed into a pile, under-fire combustion air dries and gasifies the waste, oxidizing the fixed carbon in a first chamber to generate heat at a temperature less than the melting temperature of the non-combustible material so as not to form slag, adding air in the first chamber in an amount less than stoichiometric with the air introduced in a swirling fashion to move the particulate laterally away from the discharge of the primary chamber, impeding the movement of this particulate also by adding secondary combustion air in a downward swirling direction in the secondary chamber so that very little non-combustible material reaches the second chamber where melting can occur.
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BACKGROUND OF THE INVENTION
[0001] If the plates of a capacitor are separated and a thin conductor is placed between the plates and does not touch either plate the overall capacitance is equal to the capacitance created by the distance between each plate and the thin conductor. As seen in FIG. 1 , if a capacitor 12 is placed in series with an inductor 14 and a resistor 16 and the circuit is caused to resonance with an alternating current the current is the same in all parts of the circuit. A thin conductor placed between the separated plates of the capacitor in an RLC circuit acts just like a conductor in the circuit separated by two separate capacitors in an RLC circuit. Since the thin conductor acts like another conductor in the circuit separated by two separate capacitors, it is now part of a new RLC circuit and a current will be induced on it as if it was just another conductor in the resonating circuit.
[0002] When the reactance of the inductor is equal to the reactance of the capacitors in the circuit the circuit will resonate at a natural frequency and there is only resistance in the circuit. This resistance can be varied externally. Since all the current is uniform in a resonating circuit the externally varied current will vary the current induced in the thin conductor between the plates of the capacitor because the thin conductor is now part of the circuit. This concept can be demonstrated experimentally by placing a fine wire 22 , separated by air space, between two conductors 24 , 26 as shown in FIG. 2 . The conductors are then placed in series with an inductor 28 and caused to resonate using a signal generator 30 connected in series. It can then be shown using an oscilloscope 32 that at resonance the current in the isolated thin wire is the same as any other point in the circuit and its amplitude can be controlled externally by varying the signal generator current output.
SUMMARY OF THE INVENTION
[0003] A procedure electrically stimulates a nerve or group of nerves. Unlike conventional systems this procedure is tuned to target a large or small group of neurons using noninvasive electromagnetic induction. This system is capable of doing this by using the principles of the alternating current in a capacitance inductance series resonance circuit. In this system the nerve resonator treats the neuron like a thin conductor placed between the plates of a capacitor in series with an inductor and then tuned to resonate with the appropriate frequency of alternating current. The system could also be inductance tuned for a given frequency. Once the system is tuned, the current amplitude in the entire circuit including the thin conductor or nerve fiber can be externally controlled.
[0004] This electrical medical device is based on three physical phenomena. Examining the equations for a series resonate RLC circuit illustrates the first. For a given resonate natural frequency (ω 0 ) there is a unique inductor (L) for a given capacitance (C). This relationship is shown in the equation for a resonating RLC circuit.
ω 0 2 = 1 LC .
The second physical phenomenon is that alternating currents with frequencies of the order of 10 6 Hz do not interfere appreciably with nerve processes and can be used for therapeutic heating. The nerve axon is conductive due to fact that it contains an electrolyte and once it is exposed to changing electromagnetic field it experiences electrolysis.
The third physical phenomenon is that a dielectric material between the plates, of the parallel plate capacitor, decreases the potential. This phenomenon is because a charge builds up on the surface of the dielectric. Some of the field lines pass through the dielectric material and some do not. The field lines that do not pass through the dielectric are responsible for the voltage decrease and the dielectric surface charge.
This disturbance can cause displacement currents in the dielectric material. These displacement currents would affect a conductive fiber in the dielectric. This conductive fiber represents the target nerve axon and the dielectric represents the surrounding tissue. Since the charge Q dose not change and the voltage (V 0 ) is greater than (V) the capacitance is increased by the dielectric. Since the tissue act like a dielectric it only increases the capacitance between the electrode and target nerve. The following equation, for a capacitor with constant charge Q, shows that a decrease in voltage results in an increase in capacitance.
C = Q V
[0005] The applications for neutral resonating are numerous. For example, using the applied resonating electric field to target and incinerate the infected neuron could cure genital herpes. The applied current will cause electrolysis on the electrolyte conductor. Placing one electrode over the appropriate ganglion and the other electrode on the lesion targets the infected neuron. The ganglion contains the nucleus of the neurons for a certain sensory system. Therefore a disk shaped electrode is placed over the ganglia on the back. The lesion indicates the point on the skin where the infected nerve is closest. A point electrode is placed over it. The system can also be used for pain relief anywhere on the body. The area treated could be large or small according to the size of the electrodes. It could be used to treat other infections of the nervous system. Unlike other systems the neuron can be targeted and the current in the neuron can be tuned and externally adjusted. This system can also indicate the conductivity of the neuron because as its changes the system capacitance will change, changing the natural frequency of the system.
BRIEF DESCRIPTION OF THE DRAWINGS
[0006] FIG. 1 depicts a conventional RLC circuit;
[0007] FIG. 2 depicts an RLC circuit having an alternative capacitor;
[0008] FIG. 3 depicts a capacitance model using a nerve;
[0009] FIG. 4 depicts electrodes used with the invention;
[0010] FIG. 5 depicts the targeting a nerve;
[0011] FIG. 6 depicts a second use of the invention on a nerve;
[0012] FIG. 7 schematically shows an instrument to treat a nerve;
[0013] FIG. 8 depicts a system to treat a nerve; and
[0014] FIG. 9 depicts current through a capacitor.
DETAILED DESCRIPTION OF THE INVENTION
[0015] Referring back to FIG. 2 , the thin wire 22 acts as the thin conductor and two cylinder conductors 24 , 26 represent the plates of the capacitor. These cylinders are separated and held in space in a wood fixture. The thin wire is placed between the cylinders. This fixture is a replication of the capacitance model. The conductive cylinders are the original capacitors plates and the thin wire is the thin conductor between the plates of the original capacitor. The thin conductor acts like the target nerve because the nerve is conductive. The capacitance was calculated using the area of the end of each cylinder and the distance between them. For this model the capacitance was calculated to be 1.93×10 −15 F. This capacitance was calculated from the following formula.
C = ∈ 0 A d
Since the system will be eventually tuned only an approximation of the capacitance is necessary to establish an appropriate inductance. Therefore the affect of the air and wire can be excluded from the equation.
[0016] Once the capacitance is known an inductance can be calculated for a natural frequency. A frequency of 20 MHz is above the range of nervous system perception. So for this experiment an inductance of 0.033 H will be needed to make this circuit, containing a capacitance of 1.93×10 −15 F, resonate at a natural frequency of 20 MHz. This can be shown by using the equations for an RLC series resonate circuit and solving for inductance for a given natural frequency and capacitance.
f r = 1 2 π LC
In the experiment the capacitance model was connected in series with the inductor 28 and a variable RF signal generator 30 , as seen in FIG. 2 . The circuit was tuned to resonate by adjusting the frequency on the signal generator. The signal was monitored using an oscilloscope 32 with two probes 34 , 36 connected on the circuit. At approximately 20 MHz the circuit starts to resonate and both probes start to have the same reading. This is consistent with the fact that the current is equal across the circuit of a resonating RLC circuit. Once resonance is achieved, by tuning the frequency, the amplitude of the current, anywhere on the circuit, obeys Ohms law and can be controlled by varying the resistance anywhere in the circuit.
V=IR
This is consistent with the equations for a resonating RLC series circuit. Placing the oscilloscope probe anywhere on the experimental circuit at resonance, and obtaining the same results, experimentally verifies this equation. These results prove that a thin conductor, representing a conductive nerve isolated in space, can be targeted with two electrodes and tuned to resonate. At resonance the thin conductor essentially becomes part of the circuit and its current amplitude can be adjusted externally. This targeted current can be used to directly electrically stimulate the nerve.
[0017] If the circuit is resonating the equations for can be defined by the following equations for a resonating RLC circuit.
Series Resonance
X L = X C
ω 0 L = 1 ω 0 C
ω 0 2 = 1 LC
Z = R
V L = V C
V L = IX L
V C = IX C
V R = IR
V = Voltage ( V ) ( volts )
I = Curren t ( A ) ( amps )
R = Resistanc e ( V · A - 1 ) ( Ω ) ( ohm )
L = Inductance ( H ) ( V · s · A - 1 )
C = Capacitance ( F )
f = Frequency ( Hz ) ( cycles / sec . )
ω = Angular - frequency ( rad . / sec . )
ω 0 = Natural - frequency ( rad . / sec . )
X - Reactance ( V · A - 1 ) ( Ω ) ( ohm )
Z = Impedance ( V · A - 1 ) ( Ω ) ( ohm )
[0018] The following equations are for resistance, capacitance and inductance.
Resistance
R = ρ l A
V = IR
Capacitance
C = Q V ab
C = ɛ A d
i = C ⅆ v ⅆ t
Inductance
L = μ 0 N 2 A l
v = L ⅆ i ⅆ t
ρ = Resistivity ( Ω · m )
A = Area ( m 2 )
l = Length ( m )
ɛ 0 = Premittivity ( 8 . 854 × 10 12 C 2 · N - 1 · m - 2 )
μ0 = Permeability ( 4 π × 10 - 7 Wb · A - 1 · m - 1 )
K = Dielectric - constant
Q = Charge ( C ) ( columb )
N = Number - turns
[0019] If the two plates of the original capacitor in the RLC circuit 10 are replaced with electrodes 42 , 44 and if the two electrodes are placed correctly along a target nerve 45 , the nerve acts like the thin conductor 22 placed between the separated plates of the original capacitor. The comparison is depicted in FIG. 3 . This total capacitance can then be placed in series with the proper inductance and caused to resonate at their natural frequency with an alternating current. The nerve 45 will then act like the thin conductor connecting two capacitors in series in the RLC circuit. For a given natural frequency this capacitance will act like one total capacitance and can be caused to resonate if connected in series with the proper inductance.
[0020] Resonance is achieved in this constant capacitance series circuit by tuning the inductance or by tuning the frequency. Because the nerve fiber is conductive it becomes part of the circuit separated by two capacitors in series just like the thin conductor placed between the separated plates of the capacitor in the RLC circuit. Once resonance is achieved we can externally control the current in the nerve by controlling an external resistance for a given voltage. This is because at resonance the AC current in the RLC circuit obeys ohms law as if it was a DC circuit.
V=IR
[0021] It does not matter if there is tissue separating the electrodes from the nerve. The ends of the electrodes themselves are electrically insulated. This is because a capacitor with a dialectic placed between its plates still has capacitance. The capacitance of a capacitor is found to increase with the presents of a dielectric between its plates and the tissue acts as a dielectric.
[0022] The nerve resonator is tuned to optimize the current on the target nerve similar to the way a radio is tuned to receive a given signal. This system views the nerve as conductor separated by two capacitors in a circuit. A current in the nerve can then be resonated at a certain frequency using the proper inductance. This is similar to inductance tuning a radio receiver for a given capacitance and a certain frequency.
[0023] Resonance can be achieved by vibrating a system at its natural frequency. The most common example of mechanical resonance is when a wine glass is shattered with sound waves. If a wine glass is vibrated at its natural frequency even sound waves of relatively low amplitude can cause the glass to shatter. It could be possible to destroy the axon of a nerve cell with the same phenomenon because a system can be electrically resonated. The nerve axon could be destroyed using an alternating current. If the system is oscillated with an alternating current at its natural frequency the nerve axon could be destroyed much the same way as the wine glass.
[0024] Insulated and shielded conductors can be used as electrodes 42 , 44 , depicted in FIG. 4 . If the electrodes are placed at opposite sides of the target axon an alternating current could be induced on that axon by varying the frequency or inductance. Tuning the frequency or inductance in the circuit will accommodate the new capacitance created between the electrodes with the target axon between them. The electrolyte in the neuron is conductive. As the current is increased in the electrolyte it will experience electrolysis. The electrolysis will cause the electrolyte to become a dielectric due to thermal breakdown.
[0025] The neural resonator can be used to target infected neurons. One example of a neural infection is the herpes virus. The herpes virus penetrates the skin, at the site of a lesion, and enters the nervous system through the sensory nerve endings. Then it follows the nerve axon to a single nerve cell nucleus located in the ganglion. Once the virus reaches the nerve cell nucleus it multiplies. The viral offspring then follow the same nerve axon back to the skin surface. They show up as a lesion. The nerve axon is electrically conductive. Therefore it is a conductive path between the lesion and the infected nerve cell nucleus. In the case of genital herpes the lesion is located on the genitals. The infected nerve cell nucleus is located in the ganglion at the base of the spine, seen in FIG. 5 .
[0026] Referring to FIG. 5 , the electrodes 42 , 44 are analogous to the electrodes 24 , 26 on either side of the capacitor 12 of FIG. 2 , in the resonating RLC circuit. Each electrode is placed in close proximity to each end of the target nerve axon. An example would be placing one disk shaped electrode on the surface of the back over the appropriate ganglia and placing the other point shaped electrode on the lesion. This could target a neuron infected with the herpes virus.
[0027] The herpes example only demonstrates how a neuron or group of neurons can be targeted for any application. By studying the anatomy of the nervous system. It can be see that any sensory or motor nerve could be targeted. If one electrode is placed over its ganglia and the other electrode is place over the area of pain. The nerve could be incinerated or only numbed depending on the applied current. This means the nerve resonator could have numerous applications. For example in density it could replace conventional Novocain. Technicians in the field could use it to instantly numb an injured victim as well as surgeons could use it to perform surgery. It could be used in sports medicine to treat arthritis or other injuries. It could also be used to treat other viruses of the nervous system. It could also be used to replace conventional shock treatments making it less painful for the mental patient. The placement of the electrodes used for the nerve resonator is much like the placement of pins used in acupuncture. The system could also be used in place of conventional TENS and NMES devises. Its main difference is the nerve resonator is tuned in each application. This device could also be used to stimulate neural pathways in the brain. Regardless of the condition of the neurotransmitters they will have a unique capacitance and can be matched with the proper inductance for the given natural frequency.
[0028] Applying a voltage across the electrodes and measuring the capacitance can find the precise location of the electrode that is placed on the back. With one electrode on the lesion the other electrode can be moved around on the back, in close proximity to the location over the appropriate ganglia, until a maximum capacitance is measures for a given voltage. A dielectric may be needed on the skin to eliminate a conducting surface charge. The electrodes will have a maximum charge for a given voltage because the capacitance is a maximum and charge is directly proportional to capacitance.
C = Q V
[0029] The following equation shows capacitance is directly proportional to the area and inversely proportional to the distance.
C = ɛ A d
If electrode 42 has a very small area (A), and the distance (d) between the electrodes is relatively large, the capacitance would be extremely small. When the body is placed between the electrodes the capacitance increases and can be broken down into two components. One component is the 42 to nerve capacitance and the other component is the b 44 to nerve capacitance. These distances are much smaller than the free space distance between the electrodes with no body present. The total capacitance is composed of the individual capacitance components. The capacitance model in FIG. 5 shows this. The capacitance model also shows how the displacement current will affect the conductive nerve axon since it has a smaller resistance (R) than the surrounding tissue.
[0030] The conductive material in the nerve axon is known to be an electrolyte. The electrolyte is potassium ions. When an electrolyte is exposed to a current the result is electrolysis. If the current destroys the nerve with electrolysis or if the current destroys the nerve with heating the net result is the nerves conductivity is destroyed. This will change the capacitance (C bd ) and the system will no longer resonate with the same inductance (L) and natural frequency (ω 0 ). This condition will indicate the nerve axon is incapacitated.
[0031] Although, a single nerve axon has a very small cross section, a nerve is made up of hundreds of axons as shown in FIG. 6 . This should significantly increase the area of the conductive cross section through the tissue in the capacitance model shown in FIG. 3 . Although the model is simplified it makes the point that there exists a unique capacitance (C bd ) between the electrodes 44 and 42 . The capacitance (C bd ), connected in place of the capacitance (C), will become the new capacitance of the RLC circuit. The new capacitance (C bd ) has a unique natural frequency (ω 0 ) for a unique inductance (L).
[0032] As shown in the schematic in FIG. 7 , the system consists of a variable frequency oscillator, a variable resistor, an oscilloscope, a variable inductor, and the capacitance between the two electrodes 44 and 42 . The variable-frequency oscillator generates the alternating current. This frequency could be around 20 6 Hz or more. Once the electrodes are placed on the body the capacitance between electrode 44 and 42 (C bd ) becomes the new capacitance (C). After the electrodes are placed on the body the capacitance between them can be measured. For the herpes example the maximum capacitance for a given voltage will indicate the optimum position of the electrode placed on the back over the ganglia. This capacitance will indicate a unique inductance (L) required for the system to resonate at a given natural frequency (ω 0 ). The oscilloscope will indicate when the system is resonating. The circuit can be tuned by adjusting the inductance for a unique frequency. Once the system is resonating at the natural frequency the variable resistor can be used to adjust the current in the system
[0033] At resonance the increasing displacement current induced in the axon will cause it to become an insulator. This will change the capacitance (C bd ) of the system. The change in capacitance will result in a change in the systems natural frequency and the system will no longer resonate. This change indicates the neuron has been disabled. The same result could be achieved by varying the frequency (ω) for a given inductance (L).
[0034] The simplest way to view this system is to remember it is basically a simple resonating RLC circuit. Two electrodes are placed at designated positions relative to a target nerve axon. In a resonating RLC circuit the current obeys Ohm's law and can be set with voltage and resistance.
V R =IR
In other words the nerve fiber becomes part of the circuit. For example if current required is in the range from 0.1 A to 1 A you would use a variable resistor with a range of 10Ω-1Ω and a voltage of 1V.
[0035] The displacement current density (J D ) as seen in FIG. 9 , between the plates of a capacitor, is related to the conduction current (I C ) in the circuit. The plates can be viewed as the electrodes as shown in the capacitance model seen in FIG. 3 . As seen in the following equation the conduction current (I C ) going into one electrode equals the product of the displacement current density (J D ) and the area between the electrodes.
I C =J D A
The displacement currents will affect a conductor, in the dielectric, between two electrodes. The displacement current density (J D ) between the electrodes is directly proportional to the electric field rate of change
( ⅆ E ⅆ t )
between the electrodes. This relationship is illustrated in the following equation.
J D = K ɛ 0 ( ⅆ E ⅆ t )
This equation indicates that since there is an electric field rate of change between the plates in a resonating RLC circuit there will be a displacement current affecting the area between the plates. Since electrode 44 and electrode 42 act like the two plates of a capacitor the nerve axon between the electrodes will see displacement currents. If a capacitor was made with a conductor in it and an increasing alternating current was applied to the capacitor it would eventually short across the conductor. This example illustrates how the displacement currents affect a conductor in changing electric field.
[0036] To test this device the RLC circuit system schematically shown in FIG. 7 could be used. A frequency of around 10 6 Hz can be used on the nervous system. Therefore it could be used as a starting point. The electrodes 44 and 42 are placed in the closest proximity to the target nerve. Electrode 44 is an insulated and shielded disk and electrode 42 is an insulated and shielded point, as seen in FIG. 4 . Electrode 44 is placed over the approximate area of the target ganglia. The ganglion is located along the spine. Electrode 42 is a disk to minimize the distance to the cell nucleus in the ganglia. Electrode 44 is a point because it is placed over the target area, on the skin, and is designed to target the nerve axon ending at that point. We could target more neurons by making electrode 44 a disk. This would depend on the application. Both electrodes are insulated on the ends but not shielded on the ends. The precise location of the 42 electrode, placed on the back over the ganglia, is found by applying a voltage across the electrodes with the electrode 44 placed on the targeted skin area. The capacitance can then be measured in real time. The location of the electrode 42 is where maximum capacitance is measured.
[0037] This capacitance has a unique inductance for a set natural frequency. An oscilloscope can be used to indicate when resonance is achieved by adjusting the inductance for the set natural frequency. Once resonance is achieved, with the electrodes on the body, the variable resistor can control the displacement current. When the displacement current increases in the nerve axon it will heat up until it thermally breaks down and becomes an insulator. This can be illustrated by the example of a shorting capacitor. The oscilloscope will then indicate when the system is no longer resonating because the capacitance has been changed. This indicates that the nerve has been incapacitated. As seen in FIG. 8 the actual electronic device could be lightweight and portable. An operator could easily operate the device by following simple instructions:
[0038] The following shows the instructions for this device.
[0000] 1: Turn device on
[0000] 2: Switch to DC mode.
[0000] 3: Place point electrode on lesion.
[0000] 4: Place disk electrode on back over the ganglion.
[0000] 5: Move the disk electrode around until the capacitance is at its maximum.
[0000] 6: Make sure both adjustment knobs are in the start position.
[0000] 7: Switch to AC mode.
[0000] 8: Rotate the variable inductance knob until resonance lamp comes on.
[0000] 9: Rotate the variable resistance knob until the resonance indicator lamp goes off.
[0000] 10: When the resonance indicator lamp goes off the nerve has been incapacitated.
[0039] The alternating current can be analog or digital. An inductor and a capacitor can cause an electric circuit to resonate just as a spring and a mass can cause a mechanical system to resonate. Two electrodes places near each end of the target axon have their own unique capacitance. If this capacitance replaces the capacitor, in a resonating RLC circuit, the circuit has a new natural frequency and or inductance. In order for the new circuit to resonate it must be oscillated at its new natural frequency or the inductance must be adjusted to achieve the original natural frequency. Once the circuit is resonating the alternating field change between the electrodes can cause a displacement current between them. This current can be manipulated with a variable resister because, when an RLC circuit is resonating, the current obeys Ohm's law. The displacement currents affect any dielectric between the electrodes. This affect can be used to create a current in the conductive nerve axons within the dielectric tissue. This current can then be used to disable a targeted nerve.
[0040] The basic concept is that an alternating current can be induced on the axon of a neuron by use of an RLC circuit. The target can a single nerve axon or multiple nerve axons and will be affected by two electrodes creating the capacitance in the circuit. The circuit can then be tuned to resonate and a current induced on the target nerve axon. The alternating current can be used for heating or any other purpose. It is also noticed that a similar resonating system could be built with one electrode or multiple electrodes.
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A procedure electrically stimulates a nerve or group of nerves. Unlike conventional systems this procedure is tuned to target a large or small group of neurons using noninvasive electromagnetic induction. This system is capable of doing this by using the principles of the alternating current in a capacitance inductance series resonance circuit. In this system the nerve resonator treats the neuron like a thin conductor placed between the plates of a capacitor in series with an inductor and then tuned to resonate with the appropriate frequency of alternating current. The system could also be inductance tuned for a given frequency. Once the system is tuned, the current amplitude in the entire circuit including the thin conductor or nerve fiber can be externally controlled.
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The invention described in this specification is the subject of Invention Disclosure Document No. 326,587.
TECHNICAL FIELD
The present invention relates to a portable bumper golf game. More particularly, the invention relates to a miniature golf system that is easily constructed, challenging, conveniently transportable and durable. Each hole of the system is independently constructed of durable and rigid materials and has no moving parts. The units can be neatly stacked on a truck or trailer for transport, and the system can be set up for use in a short period of time since assembly and adjustment steps are kept to a minimum. A typical system would be comprised of a number (usually nine) of different holes, but a complete inventory could include many more individually unique and different holes. Thus a nine-hole system could readily be tailored to the preferences and degree of difficulty desired by those who will be using the system at a given time. The foregoing characteristics are particularly attractive to those who will be operating the games at many different locations.
BACKGROUND OF THE INVENTION
There are, of course, numerous miniature golf games, permanent and portable, in use and otherwise know in the prior art, U.S. Pat. No. 5,067,716 discloses a self-contained system wherein all playing greens are attached to a transport means, and remain so attached during play. A portable miniature golf board game is disclosed in U.S. Pat. No. 4,098,507. The board game has a single green, but it does offer the option of playing any one of three holes. Portable golf games having a single green and a single hole are disclosed in U.S. Pat. No. 4,596,391 and in U.S. Pat. No. 3,944,232. A combination of golf and billiards is disclosed in U.S. Pat. No. 4,957,388 wherein a golf ball and putter are used to play on a pool table type setting. U.S. Pat. No. 4,877,250 discloses a portable putting course containing a single green having a plurality of holes. None of the foregoing games provides the combination of variety, portability and durability that is provided by the bumper golf system of the present invention.
SUMMARY OF THE INVENTION
It is an object of the present invention to provide a unique and improved bumper golf game that is unique and interesting to play due to the variety of holes offered.
Another object of the present invention is to provide a bumper golf game that can easily be transported, and readily set up for play at any of various locations.
Still another object of the present invention to provide a bumper golf game that is durable and resistant to the detrimental effects of various outdoor environmental conditions such as water, extreme temperatures and UV rays.
These and other objects of the present invention are achieved by a bumper golf game wherein each hole is different from all others. Each hole is independently and sturdily constructed in such a manner as to allow for convenient transport and quick set-up of the system at any suitable location.
A major aspect of the invention is the durability of the materials used in its construction. Most known miniature golf systems are used and/or stored out of doors, and are therefore subjected to various detrimental environmental conditions that promote degradation of the materials of which they are made. All materials used in construction of the present invention are immune or resistant to the effects of water, extreme temperatures and UV radiation. The sides, ends, braces and floor are made from 1/4 inch and 1/2 inch sheet plastic. One especially satisfactory material is cutting board stock made by C & K Manufacturing & Sales in Westlake, Ohio. The playing surface is a synthetic carpet especially made for outdoor use. Screws used in assembling the units are made of corrosion-resistant aluminum or stainless steel.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a general perspective view of a representative hole, or unit, of the bumper golf system.
FIG. 2 is a sectional view taken across the lines 2--2 of FIG. 1.
FIG. 3 is a detailed view showing how the sides and floor are assembled.
FIG. 4 is a perspective view of a bumper used as an obstacle on the playing surface.
FIG. 5 is a plan view of a bumper.
FIG. 6 shows the relationship of a bumper and a golf ball in close proximity to each other.
FIGS. 7 and 8 are top and side plan views of a non-limiting example configuration non-limiting, for a playing hole to make up the bumper golf system of the present invention.
FIG. 9 is a top plan view of a further example configuration for a playing hole.
FIGS. 10 and 11 show top and side plan views of a further example for a playing hole.
FIGS. 12 and 13 show top and side plan views of a further example of a playing hole in accordance with the invention.
FIGS. 14 and 15 show top plan views of further examples of playing holes to make up the bumper golf system of the invention.
DETAILED DESCRIPTION OF THE INVENTION
FIG. 1 illustrates a typical hole, designated generally as 1. Ends 2 and sides 3 are joined to form the boundaries of the hole, and the base, or floor, for the playing surface 4 is placed at a plane below the top edge of the sides and ends. The sides and ends thus act as a border and confine the ball in the playing area. The structure is shown in more detail in FIGS. 2 and 3.
The tee box 5, where the ball is placed in play, is defined by broken line 6 and can optionally be marked by any appropriate means. One such means is a golf ball on a tee on the top edge of side 3. At the opposite end of the hole is cup 8 having one or more bumpers 9 placed nearby to make it more difficult to put the ball in the cup.
FIG. 2, a cross-sectional view across the lines 2--2 of FIG. 1, shows details of construction. The floor 10 of the playing surface is fixed at a level between the upper and lower edges of sides 3. The floor is flexible to a limited degree to allow for variations in the level of the playing surface (see FIGS. 11 and 13, for example), which variations will cause rolls and contours along the length of holes as selectively desired. The floor is supported by, and rests on top of horizontal brace, or stringer, 11. A plurality of braces, or stringers, are provided as needed to provide necessary support for the floor along the length of the unit. It is the variations of the height along each stringer which will provide for rolls and contours in the playing surface because of the inherent flexibility of the floor 10. The floor 10 is secured to the stringers 11 by adhesive or other suitable means. Playing surface 4 is a weather resistant carpet material such as a miniature golf carpet. A typical unit would be about 2 feet by 8 feet having sides and ends of 1/2 inch thick material and a height of 4 inches. The braces, or stringers, are typically 2 inches high, the floor 1/4 inch thick and the carpet 1/8 inch thick, thus causing the top of the carpet to be about 15/8 inches below the top edge of the sides and ends. The dimensions are not critical, but it is convenient to have the sides and ends at a sufficient height above the playing surface to provide a barrier around the playing surface to prevent the ball going out of bounds, and also because it is desirable to have the playing surface only about 2 inches above the surface upon which each hole is positioned to be played to facilitate playing the game by a player.
FIG. 3 shows additional details of construction of the units. Sides 3 are attached to braces 11 by means of rust-resistant screws 12 which are typically either aluminum or stainless steel. Floor 10 can also be attached to braces 11 by similar means.
An optional feature that can be provided around at least part of the interior side wall is a linear bumper 13. The bumper, usually a rubber material having a triangular cross section, is adhesively or otherwise attached in a groove 14 in the face of side 3. The linear bumper can be placed around the entire periphery of the unit, or it can be placed only in certain places as desired. Typically, the bumper will be provided at locations in close proximity to the cup. It is important that the height of the linear bumper (i.e., the vertical distance from point 13a to the top surface of carpet 4) be within a specified range. The placement of the bumper should be such that the ball contacts point 13a at a point about the middle of the ball or at its largest circumference. For a conventional golf ball, the point of contact can be in the range of about 50/64 inch to about 55/64 inch above the playing surface in the preferred embodiment. The height of the bumper is such that the point of contact is at the widest circumference of the ball, or slightly above the circumference of the ball. Contact of the circumference of the ball with the linear bumper at, or just below point 13a provides a good rollback. If point 13a is too high or too low the ball will skip rather than roll smoothly across the playing surface after striking the bumper.
FIG. 4 is a perspective view of a bumper assembly 9 comprising a rigid core member 22 and a tire-like member 23 surrounding a portion of the core. The core is commonly a molded hard plastic, but could also be fabricated from a metal, wood or other suitable material. The tire-like member is usually made from a rubber.
FIG. 5 is a plan view of bumper assembly 9. At the bottom of core 22 is a threaded shaft 24 that is embedded in the core as shown by broken lines 25. The threaded shaft is inserted through a hole in the floor 4 at any desired location, and the bumper assembly is secured by a nut, not shown.
FIG. 6 shows a bumper assembly 9 and a conventional golf ball 27 in close proximity to each other as they will frequently be when the game is being played. Line 26 represents the circumference of the tire in the bumper assembly, and line 28 represents the circumference of ball 27. The height of the bumper assembly should be such that line 26 is in the range of about 50/64 inch to about 55/64 inch above the playing surface. Ideally, line 26 is in the same plane with, or slightly higher than line 28 on the ball such as a distance of about 1/64 inch. Proper alignment of the bumper assembly with respect to the ball assures a proper roll-back after the ball strikes the bumper assembly in the same manner as previously described with respect to the linear bumper in FIG. 3.
FIGS. 7 and 8 show one of the many optional plans that can be used for each unit of the system of the present invention. As can be seen graphically in FIG. 8, a portion of the unit at one end, and containing the cup, is angled upward at point 15, resulting in cup 8 being located on an incline.
FIG. 9 shows a hole having a dogleg right, and, of course, an alternative to this is a dogleg left.
FIGS. 10 and 11 show a plan having to hills 17 between the tee box and the cup. As mentioned earlier, floor 4 is flexible, and the hills are made by using braces 11 of varying heights as illustrated particularly in FIG. 11.
FIGS. 12 and 13 show a further example of the type of holes which may form a part of a "course" constructed in accordance with the invention.
FIGS. 14 and 15 show additional variations of designs wherein the differences from previously described ones are self-evident. Many additional designs are also within the range of this specification, and should not be considered to be patentably distinct therefrom.
In compliance with the statutes, the invention has been described in language more or less specific as to structural features. It is to be understood, however, that the invention is not limited to the specific features shown, since the means and construction herein disclosed comprise a preferred form of putting the invention into effect. The invention is, therefore, claimed in any of its forms or modifications within the proper scope of the appended claims, appropriately interpreted in accordance with the doctrine of equivalents.
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The invention is directed to a bumper golf game wherein each hole is different from all others, providing unique playing characteristics. The invention uses durable materials in its construction, which are immune or resistant to the effects of water, extreme temperatures and UV radiation. The playing surface is a synthetic carpet especially made for outdoor use.
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BACKGROUND OF THE INVENTION
1. Field of the Invention
The invention relates to an ozone generator with a tubular outer electrode and a plurality of inner electrodes which exhibit a dielectric layer on their surface facing the outer electrode, means for spacing the inner electrodes from the outer electrode for forming an annular discharge gap and means for electrically connecting all electrodes to an alternating current source.
Ozonizers of this type are known, for example, from Swiss Patent Specification No. 648,534.
2. Discussion of Background
The increasing use of ozone for chemical and physical purposes has led to the ozone tube, which is based on work by Siemens, being decisively improved in technical and economic respects in the recent past. Thus, it is proposed in U.S. Pat. No. 2,811,217, to increase the ozone yield by means of the fact that particular characteristics of the ozonizer (frequency of the feed voltage, dielectric constant of the dielectric material, amplitude of the feed voltage, thickness of the dielectric layer and size of the discharge gap) must comply with particular laws.
For the same purpose, special cooling measures are proposed in other publications for increasing the ozone yield, thus, for example, in addition to the liquid cooling of the outer electrode, the internal cooling of the high voltage electrode with gas or liquid in German Offenlegungsschrift No. 2,357,392, or the intermediate cooling of the ozone-enriched feed gas in the case of cascaded ozonizers in German Offenlegungsschrift No. 2,436,914.
It is generally known that the mean temperature in the discharge gap can be lowered by reducing the discharge gap width in a tubular ozone generator. It can be demonstrated theoretically and experimentally that the mean temperature in the discharge gap is proportional to its gap width.
A low temperature in the discharge gap is desirable since this significantly increases the efficiency of ozone generation.
At present, discharge gap widths of around 1 mm are the state of the art. With a further reduction in gap width, the limits of geometric tolerances of the metal and dielectric tubes used are reached. Particularly in the case of relatively great tube lengths, a further reduction in gap width is limited by the ever present bending of the dielectric and metal tubes.
SUMMARY OF THE INVENTION
Accordingly, one object of this invention is to provide a novel ozone generator which makes it possible to have small gap widths and provides the possibility of having ozone generators of relatively great constructional length.
To achieve this object in an ozone generator of the generic type initially mentioned, it is provided in accordance with the invention that the inner electrodes consist of a plurality of cascaded mechanically decoupled electrode segments which are electrically connected to one another in groups, and each electrode segment is supported spaced independently of the outer tube. In this manner, both simplex and duplex ozonizers of almost any constructional length can be implemented. Bending of the outer tubes has no influence on the gap width tolerance. The insertion of the inner tube is considerably facilitated.
The electrode segments can be glass tubes closed at one end with a metallic lead-through in the bottom for electrically connecting the next element. However, plastic dielectrics are advantageously used as they were described in German Offenlegungsschrift No. 3,442,121 or U.S. Pat. No. 4,650,648. In the case of plastic dielectrics, a metallic lead-through through the bottom can be produced relatively simply.
The use of a segmented dielectric leads to further advantages. The metal tubes may exhibit a bending of up to some mm. The length of the metal tubes is not fixed to approximately 2 m as is currently usual, lengths of up to 6 m are conceivable and required. Long metal tubes bring advantages in cooling them with water: The cooling water can flow along the metal tubes which leads to a required increase in the cooling water flow and thus to a better cooling. As a result, unwanted depositions on the water side of the metal tubes are also reduced.
BRIEF DESCRIPTION OF THE DRAWINGS
A more complete appreciation of the invention and many of the attendant advantages thereof will be readily obtained as the same becomes better understood by reference to the following detailed description when considered in connection with the accompanying drawings, wherein:
FIG. 1 shows a greatly simplified longitudinal section through an ozonizer tank with a large number of ozone generators;
FIG. 2 shows a detail of FIG. 1 with an ozone generator with a ceramic dielectric;
FIG. 3 shows a detail from FIG. 2 with an alternative contact arrangement between adjacent inner electrodes;
FIG. 4 shows a detail from FIG. 1 with an ozone generator with glass dielectric in the form of glass tubes closed at one end;
FIG. 5 shows a detail from FIG. 1 with an ozone generator with glass dielectric in the form of open glass tubes.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
Referring now to the drawings, wherein like reference numerals designate identical or corresponding parts throughout the several views,
FIG. 1 shows in a greatly simplified representation an ozonizer as it is currently constructed for industrial use.
A large number of ozone generators are accommodated in a tank 1. The tank 1 exhibits at its end tube-sheet-like partition walls 2,3 into which metal tubes 4 are welded. These metal tubes form the outer electrodes (which are connected to ground potential) of each ozone generator. For reasons of clarity, only five of these tubes 4 are drawn in; in practice, it can be 100 and more tubes. The tubes are sealed with respect to the interior of the tank where they are clamped into the partition walls 2, 3. A coolant, for example water, which is used for external cooling of the metal tubes 4, is conducted into and removed from the interior of the tank via connectors 5, 6 in the tank wall. Segmented inner electrodes 7 which are spaced from the metal tubes 4 by spacers 8 and leave annular discharge gaps 9 free between themselves and the metal tube walls are inserted from both sides into the metal tubes 4.
Contact with the inner electrodes 7 is established via contact elements 10 of brush-like construction. These are each connected at the front ends to one busbar 11, 11'. These busbars 11, 11' are connected via electric lead-throughs 12 to an alternating current source 13 of adjustable frequency and/or amplitude and/or curve shape, the other connection of which is connected to ground potential.
The oxygen-containing feed gas is supplied to ozone generators via a gas inlet connector 14 and leaves the tank again through the gas outlet connector 15.
As can be seen from FIG. 1, two inner electrodes 7 in each case are electrically directly connected to one another in the left and right tank section, respectively. For this purpose, the connection part 16 of the contact elements of the inside inner electrodes leads to the front end of the outside inner electrodes 7.
FIG. 2 shows the detailed configuration of the inner electrodes 7 and their mutual electric contacts on an enlarged scale. The inner electrode essentially consists of a metal tube 17 which is closed with a cover 18 at its end facing away from the tank front end. This cover 18 can also be constructed of one piece with the metal tube 17. The outer wall of the metal tube 17 plus cover 18 is coated with a typically 2 mm thick dielectric 17 of ceramics. At the open end, the dielectric 19 covers the edge zone of the metal tube in order to prevent unwanted discharges. The coating of the cover 18 fulfils the same function. In this arrangement, this dielectric layer 19 preferably consists of dielectric powders of different grain size and resin bonding. Details on their structure and advantageous characteristics are described in German Offenlegungsschrift No. 3,442,121 or U.S. Pat. No. 4,650,648 to which reference is expressly made here.
On the cover 18 of the outside inner electrode, the connection part 16 of the contact element 10 associated with the inside inner electrode is attached which can be effected by means of soldering, welding, screwing or clamping. Instead of the brush-like contact elements 10 with connection part shown, a contact arrangement 20 can also be used which is directly attached to the cover of the outside inner electrode and is provided with contact fingers of beryllium bronze is similar to brush-type or tulip-type contacts.
It is essential that, on the one hand, the electric connection between the individual inner electrodes 7 is ensured but that, on the other hand, there is a machanical decoupling, that is to say non-rigid connection between adjacent inner electrodes.
If these prerequisites are met, ozone generators of almost any length with low gap values (typically 0.5 mm) and supportable gap value tolerances can be produced.
The present invention is excellently suitable, in particular, for ozone generators having so-called ceramic dielectrics. As is shown by the embodiments according to FIGS. 4 and 5 however, it is also suitable for ozone generators with a glass dielectric: Ozone generators with ceramic dielectric are now replaced by those with glass dielectric in FIG. 1. According to FIG. 4, these essentially consist of a glass tube 21 which is closed at one end and the entire inner surface of which, apart from an area d at the open end which has a length of a few millimeters, is covered with a metal layer 22 and to this extent, apart from the shortened constructional length, thus correspond to the inner tubes hitherto used. So that an electric connection can then be created between the metal layers 22 of the segments which must be (electrically) connected in series, the outer glass tube 21 exhibits at its closed end a metallic lead-through 23 which is electrically connected to the metallic layer 22. On the outside, the lead-through 23 is connected, for example screwed, to the connection part 16 of the contact element 10 associated with our glass tube.
As is seen in FIG. 5, glass tubes closed at one end can be dispensed with. The glass tubes 21 exhibit a plug 24 at the inner end in each case. The connection part 16 of contact element 10 is extended to the plug 24 and ends in a bush 25 arranged in the plug and is, for example, screwed into the latter. The connection part 16 of adjacent contact element 10 is inserted into this bush from the other side (from outside), for example also screwed to it. Apart from holding the bush, the plug 24 is also used as blocking element which prevents the feed gas from flowing through the interior of the glass tube 21.
Instead of a (sealing) plug 24, thin sleeves of an ozone-resistant plastic, for example teflon, can also be used as is indicated in dashes in FIG. 5. These also ensure that two cascaded tubes are sufficiently mechanically decoupled.
In the case of the ozone generators having a glass dielectric, too, the inner electrodes are mechanically decoupled from one another and electrically connected in series in each tank half, all ozone generators of one tank half being connected to one busbar 11 each. Such an arrangement is frequently called "duplex arrangement".
Naturally, the principle of segmentation on which the invention is based can also be used for so-called simplex ozone generators, that is to say those which are fed from only one tank front end, since the number of segments to be mechanically connected in series basically only depends on the tank length.
The length of a segment is between 10 cm and 50 cm both in the simplex and in the duplex arrangements. Such short segments have negligible bending. Tolerance deviations, either those at the metallic outer tube 4 and/or in the inner tubes 7 or glass tubes 21, or bending of the outer tube 7 virtually average out due to the cascading.
Thus, ozone generators with ceramic dielectric and small widths can be economically produced for the first time.
Obviously, numerous modifications and variations of the present invention are possible in the light of the above teachings. It is therefore to be understood that within the scope of the appended claims, the invention may be practised otherwise than as specifically described herein.
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In the ozone generator, the inner electrodes which have been continuous until now, are subdivided into individual electrically series-connected segments (7) which are mechanically decoupled from one another. In this manner, ozoniers of almost arbitrary length can be implemented with gap widths of around 0.5 mm.
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BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to scraper attachments for tractors and the like and more particularly to scraper attachments which are under precise control by the tractor operator, and do not permit "wandering" of the blade from side-to-side, nor permit transverse tilting of the blade, except in response to controls on the tractor manipulated by the operator.
2. Description of the Prior Art
Tractor-mounted scrapers are well known in the prior art. The tractor-mounted scrapers of the prior art have in general, however, had their blades flexibly mounted, as by means of combinations of knuckle-joints, univeral/joints, and/or independently-pivoted arms, so that their blades responded to meeting resistance by tilting, wandering to one side, or riding up over the resisting matter. These prior art tractor-mounted scrapers, with their blades thus mounted, not only failed to take optimally deep cuts, limited only by the stalling of the tractor power plants, but were also characterized by wandering or imprecise tracking of their blades, in the sense that their blades failed to follow the path of their tractors themselves with the requisite precision.
Further, the downward forces on the blades of the tractor-mounted scrapers of the prior art were provided entirely by the weight of the blades themselves, and the weight of their support assemblies. This lack of downward force on the blades of tractor-mounted scrapers of the prior art was in substantial part responsible for the tendencies of these prior art devices to take insufficiently deep cuts, i.e., cuts of depth considerably less than that which would result in stalling of the tractor.
SUMMARY OF THE INVENTION
Accordingly, it is an object of the present invention to provide a tractor-mounted scraper the blade of which will track the path of the tractor with considerably greater precision than that characterizing the devices of the prior art.
Another object of the present invention is to provide a tractor-mounted scraper which will not tilt in response to the meeting of obstacles, or ride over such obstacles, but rather will bring the full force of the tractor power plant to bear in attempting to remove the obstacle, to the point of stalling the tractor power plant.
A further object of the present invention is to provide a tractor-mounted scraper in which the full weight of one end of the tractor can be brought to bear on the scraper blade and its associated assembly, in order to prevent the blade from riding over obstacles.
A still further object of the present invention is to provide a tractor-mounted scraper having side walls which coact with scraper blade to entrap earth removed by the scraper blade so that it can be drawn to one end of the cut being made with the scraper.
An additional object of the present invention is to provide a tractor-mounted scraper the blade of which tilts transversely with respect to the tractor only in response to forces impressed by power-operated means under control of the tractor operator, and not in response to the meeting of an obstacle.
Other objects of the present invention will in part be obvious, and will in part appear hereinafter.
The present invention, accordingly, comprises the apparatus embodying the features of construction, combinations of elements, and arrangements of parts exemplified in the following detailed disclosure, and the scope of the present invention will be indicated in the appended claims.
In accordance with a principal feature of the present invention a tractor-mounted scraper comprises a "box" including two side plates interconnected by a transverse beam, which beam is so mounted on the end of the tractor as to be constrained to remain parallel to the axis of the mounting pivots affixed to the end of the tractor, and the blade is mounted transversely between said side plates.
In accordance with another principal feature of the present invention, a hydraulic cylinder is provided for pressing down on the beam-side plate assembly, which hydraulic cylinder can selectively (1) raise that assembly and the blade from the ground, (2) force said assembly downward about the pivot means at the end of the tractor so far that the end of the tractor is supported solely by the blade and the assembly, and (3) permit the blade and assembly to rest upon the ground, bearing the weight of the blade and its associated assembly, but not bearing any part of the weight of the tractor.
In accordance with a further aspect of the present invention, such a scraper attachment is provided with power-operated tilting means for tilting the beam and the blade transversely with respect to the tractor, but at the same time the beam is mounted to the tractor in such a manner that it can tilt only in response to the power-operated tilting means, and not in response to the meeting of obstacles by the blade.
In accordance with a still further aspect of the present invention, hydraulic means are provided for tilting the blade about a transverse axis extending from one side plate to the other, whereby either one of two scraping edges of the blade are presented for scraping action.
In accordance with another aspect of the present invention the side plates cooperate with the blade to entrap a large portion of the earth removed by scraping, so that it can be drawn by the scraper to one end of the cut made by the scraper, or to both ends of the cut made by the scraper.
For a fuller understanding of the nature and objects of the present invention, reference should be had to the following detailed description, taken in conjunction with the drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a perspective view of a tractor-mounted scraper embodying certain features of the present invention, partly in phantom;
FIG. 2 is an enlarged fragmentary vertical sectional view taken on line 2--2 of FIG. 1;
FIG. 3 is a plan view of the tractor-mounted scraper of FIGS. 1 and 2;
FIG. 4 is a vertical sectional view taken on line 4--4 of FIG. 2; and
FIG. 5 is a fragmentary exploded view in perspective of the box beam of a tractor-mounted scraper embodying the present invention, and the means whereby it is tiltably mounted on the parallel arms by which the box assembly is pivotably affixed to one end of the tractor.
DESCRIPTION OF THE PREFERRED EMBODIMENT
Referring now to the drawing, there is shown in FIG. 1 a scraper embodying the present invention. The scraper of FIG. 1 comprises a scraper blade supporting and positioning assembly 8 mounted on a tractor 10. In order to fully carry out the principles of the present invention, tractor 10 should be a four wheel drive tractor, i.e., a tractor having all four of its wheels powered, so that the wheels remote from assembly 8, which are arbitrarily called the "front wheels" therein, are capable of propelling the scraper, i.e., tractor 10 and assembly 8, over the ground even when the rear wheels (nearest assembly 8) are raised out of contact with the ground by means of a hydraulic cylinder 42, as hereinafter explained, or should be equipped with treads of conventional type.
Tractor 10 is also provided with a compressor (not shown) of the conventional type, and driver-operable hydraulic control means, whereby hydraulic fluid under pressure is controllably supplied to hydraulic cylinders 42, 72, and 82, of assembly 8 in order to carry out the operational principles of the present invention in the manner described hereinafter.
Both tractor 10 and its associated hydraulic power system and controls may be of well-known types, or may be assembled from conventional elements without exercise of invention, and thus are not described or shown herein.
Assembly 8 comprises a frame 12, sometimes called the "box" herein.
Box 12 comprises a beam 14. A pair of side plates 16, 18 are affixed to the opposite ends of beam 14, as by welding.
Beam 14 is pivotably mounted on a plate 20 by means of a pivot pin 22. Thus, by means of plate 20 and pivot pin 22, box 12 is pivotably mounted for pivoting about an axis which is parallel to the upper edges of side plates 16, 18 and is located slightly therebelow.
As best seen by comparing FIGS. 2 and 3, assembly 8 is mounted on tractor 10 by means of an arm 24, which is itself comprised of two side members 26 and 28. Going to FIG. 5, it will be seen that the ends of side members 26 and 28 of arm 24 remote from tractor 10 are respectively attached to the assembly comprising plate 20 by means, for instance, of weld beads 30 and 31, and thereby constrained to remain parallel to each other at all times. It will also be seen that plate 20 is constrained to remain parallel to axis of the pivot pins by which arms 26 and 28 are pivotably mounted on tractor 10.
The ends of the side members 26, 28 or arm 24 which are nearest to tractor 10 are individually, pivotably affixed to the end of tractor 10 which is arbitrarily called the rear end thereof by means of lugs 34, 35 and pivot pins 36, 37. Lugs 34 and 35 may, for instance, be affixed to the rear end of tractor 10 by welding. Pivot pins 36 and 37 are provided with retaining means selected from among the types well known to those having ordinary skill in the art, whereby they are retained in registering holes in the lugs 35 and 36 and the ends of side members 26 and 28.
As best seen in FIG. 5, a pair of lugs 38, 39 are affixed to the face of the assembly including plate 20 which lies nearest tractor 10 by means of arc welding, for instance. A pivot pin 40 (FIGS. 2 and 3) passes through and is retained in lugs 38 and 39. A block 41 contains a passage with close-fittingly receives pivot pin 40, and thus block 41 is pivotably mounted on pin 40. As seen in FIG. 2, a hydraulic cylinder 42 is provided in the usual manner, with a piston rod 43, and the end of piston rod 43 is attached to block 41.
Going to FIG. 1, it will be seen that the end of cylinder 42 opposite piston rod 43 is provided with an ear 44 in the conventional manner.
As also seen in FIG. 1, a pair of lugs 45, 46 are affixed to the end of tractor 10, as by welding. A pivot pin 47 passes through suitable bores in lugs 44, 45, 46, and thus the upper end of cylinder 42 is pivotably affixed to the rear end of tractor 10.
In accordance with the principles of the present invention, cylinder 42 is supplied with operating fluid under pressure, from the above-mentioned compressor mounted on tractor 10, by means of hydraulic hoses 48, 49 of the well-known kind.
Cylinder 42 and its associated compressor and controls may be of the double-action type, wherein working fluid under pressure can be injected into cylinder 42 either above or below the piston attached to piston rod 43, and the opposite side of the piston simultaneously vented to a sump, whereby both the upward and downward strokes of piston 42 are power strokes.
As will now be evident to those having ordinary skill in the art who have studied this specification thus far, and the accompanying drawings, piston rod 43 can, under control of the driver sitting on the seat tractor 10, be drawn further into cylinder 42 than is shown in FIG. 2, and thus box 12 can be raised from the ground.
Conversely, and in accordance with a principal feature of the present invention, piston rod 43 can, under control of the driver sitting on the seat of tractor 10, be forcibly extended considerably further out of cylinder 42 than is shown in FIG. 2, and thereby the scraper blade 50 which is mounted in box 12 can be forced against the ground behind tractor 10, thus picking the rear wheels of tractor 10 off the ground, and bringing the full weight of the scraper, i.e., tractor 10 and assembly 8, to bear on scraper blade 50 and the front wheels of tractor 10. As pointed out hereinabove, tractor 10 must be powered through its front wheels, and must be sufficiently powerful to propel the scraper over the ground when the rear wheels of the tractor are raised from the ground, and the full weight of the tractor is borne by the front wheels of the tractor and the scraper blade 50.
In accordance with another feature of the present invention, the driver-operated hydraulic controls which are mounted on tractor 10 to enable the driver to control the working fluid pressure in cylinder 42 may be put in a "neutral" position, wherein both the space above the piston and the space below the piston in cylinder 42 are interconnected to the sump of the hydraulic system mounted on tractor 10. Thus, when the hydraulic controls mounted on the tractor for controlling lifting cylinder 42 are put in "neutral" position, cylinder 42 exerts neither upward or downward forces on box 12, and scraper blade 50 rests or drags on the ground, carrying the weight of the scraper blades supporting and positioning assembly 8, except cylinder 42, but not carrying the weight of tractor 10.
The mode of operation of the device of the invention just described is sometimes called the "floating mode;" whereas the earlier described mode of operation, with the scraper blade 50 bearing a substantial part of the weight of tractor 10, is sometimes called the "pressure mode" herein.
As best seen in FIG. 1, scraper blade 50 extends from side plate 16 to side plate 18 of box 12, and is largely contained within box 12.
Blade 50 comprises a major blade portion 52 (see FIG. 2), having a scraping edge 53, and a minor blade portion 54, having a scraping edge 55.
Blade portions 52 and 54 are joined by plates 58, 60, which are inserted between the lower ends of blade portions 52, 54, and affixed thereto, e.g., by suitable arc welding beads. Aligned holes are provided in plates 58 and 60 to close-fittingly receive a pivot rod 62. The outer ends of pivot rod 62 are received in bores in the two side plates 16, 18 of box 12. Thus, blade 50 is pivotably mounted in box 12, on an axis located near the bottom of box 12, and near the end of box 12 remote from tractor 10. It is to be understood that the mounting of blade 50 to be pivotable about an axis located near the lower corners of side plates 16 and 18 remote from tractor 10 is a principal feature of the present invention.
As best seen in FIG. 1, the upper edge of major blade 52 is provided with a pair of ears 64, 66. Ears 64, 66 are themselves provided with aligned transverse bores adapted to receive a pivot pin 68. Suitable retaining means (not shown) of the kind well known to those having ordinary skill in the art are provided for retaining pivot pin 68 in place in the abovesaid aligned bores in ears 64, 66, as shown in FIG. 3.
Going now to FIG. 3, and comparing it with FIG. 2, it will be seen that a block 70 is mounted on pivot pin 68 between ears 64 and 66. Block 70 is so mounted on pivot pin 68 as to be rotatable about the common axis of said aligned bores in ears 64 and 66. The end of piston rod 71 remote from its associated hydraulic cylinder 72 is affixed to block 70.
The end of hydraulic cylinder 72 remote from piston rod 71 is provided, in the well-known manner, with an ear 74, by means of which hydraulic cylinder 72 may be pivotably affixed to suitable mounting ears or the like.
As may best be seen by comparing FIGS. 1 and 3, a pair of ears 76, 78 are affixed to the upper edge of beam 14, and ear 74 of hydraulic cylinder 72 is disposed therebetween. Ears 74, 76, and 78 are provided with aligned bores adapted to receive a pivot pin 80, whereby cylinder 72 is pivotably affixed to beam 14.
Cylinder 72 is provided with a pair of hoses 72a, 72b (FIG. 2) whereby hydraulic fluid under pressure is supplied to cylinder 72 under the control of one of the driver-operable hydraulic control means mounted on tractor 10 as described hereinabove.
Thus, as may best be understood by reference to FIG. 2, blade 50 may be pivoted about pivot rod 62 by the operator of the device of the invention by manipulation of the corresponding hydraulic control means mounted on tractor 10, and may thus be selectively positioned over a range of angular positions about pivot rod 62. In one of these angular positions the upper part of major blade portion 52 is substantially perpendicular to the plane containing the upper edges of box walls 16 and 18, and the tips of both blade portions 52 and 54 project below the lower edges of box walls 16 and 18.
In one extreme angular position of blade 50, as pivoted about pivot rod 62 by means of hydraulic cylinder 72, the upper edge of major blade portion 52 is located well forward of the intermediate position just described (i.e., in which the upper edge of major blade portion 52 is substantially perpendicular to the plane containing the upper edges of box wall 16 and 18), i.e., more remote from tractor 10 than in said intermediate position.
In the other extreme position of blade 50, as pivoted about pivot rod 62 by means of hydraulic cylinder 72, the upper edge of major blade portion 52 is located well behind the position it occupies when blade 50 is in the abovesaid intermediate position, i.e., is located near or to tractor 10.
It is to be especially noted that in accordance with a principal feature of the present invention the lower edges of blade portions 52 and 54 both project approximately 11/2 inches below the plane containing the lower edges of box sides 16 and 18 when blade 50 is in the abovesaid intermediate position, and the upper edge of major blade portion 52 is substantially perpendicular to a plane containing the upper edges (remote from the ground) of box sides 16 and 18, blade 50 being a new blade.
Referring now to FIG. 4 and FIG. 5, there is shown a hydraulic cylinder 82 and the cooperating members whereby hydraulic cylinder 82 may be used by the operator of the scraper of the invention to tilt box 12 and the parts carried by it about the axis of pivot pin 22.
A pivot pin 84 is affixed to plate 20, in the manner shown in FIGS. 4 and 5. A block 86 is pivotably mounted on pin 84, being retained thereon by means well known to those having ordinary skill in the art (not shown).
As best seen in FIG. 4, the end of the piston rod 88 of hydraulic cylinder 82 remote from hydraulic cylinder 82 is affixed to block 84. In the usual manner, the end of hydraulic cylinder 82 opposite piston rod 88 is provided with an ear 90 having a bore for receiving a pivot pin of the well-known kind.
As best seen in FIG. 4, an inverted L-shaped member 92 is provided, the longer leg of which is affixed at its outer end to beam 14, as by arc welding.
The shorter leg of L-shaped member 92 is provided near its outer end with a bore adapted to receive a pivot pin 94, which also passes through a bore in ear 90 affixed to the upper end of hydraulic cylinder 82. Thereby hydraulic cylinder 82 is pivotably affixed to L-shaped member 92.
As best seen in FIG. 2, hydraulic cylinder 82 is provided with a pair of supply hoses 82, 82b, whereby hydraulic cylinder 82 is provided with hydraulic cylinder under pressure from a suitable reservoir and pump mounted on tractor 10, it being understood that in some cases it will be desirable to use a single hydraulic cylinder and pump as the source of working fluid under pressure for all three hydraulic cylinders, i.e., 42, 72, and 82.
The operation of hydraulic cylinder 82, like the operation of hydraulic cylinders 42 and 72, may be controlled by the driver of tractor 10 by means of manual control means provided at a conveniently accessible place on tractor 10.
Summarizing, it will be seen from the above that the driver of tractor 10, equipped with the scraper of the present invention, is provided with three readily accessible manual controls by which the driver can (1) raise box 12 and thus scraper blade 50 completely clear of the ground, (2) bring box 12 downward and thus bring scraper blade 50 into contact will the ground (3) exert sufficient downward force on box 12 and blade 50 so as to raise the wheels of tractor 10 adjacent box 12 off the ground, and thus to bring a substantial portion of the weight of tractor 10 to bear on blade 50, (4) manipulate blade 50 between the two extreme positions shown in FIG. 2, and (5) tilt box 12 and blade 50 about pivot pin 22.
In accordance with a principal feature of the present invention, then, the operator of the scraper of the invention can, by means of manual controls conveniently disposed upon tractor 10, bring the weight of the tractor to bear on blade 50.
In accordance with an additional feature of the present invention, the hydraulic control means which control the operation of hydraulic cylinder 42, and thus control the positioning of box 12 and blade 50, may be put in a "mutual" position, wherein hydraulic cylinder 42 neither lifts box 12 nor thrusts it toward the ground, and thus the downward force exerted upon blade 50 is that imposed by box 12, blade 50, and their associated assembly.
In this "neutral" position the spaces on the opposite sides of the piston in hydraulic cylinder 42 are valved directly to a sump, as will be recognized by those having ordinary skill in the art.
Thus, it is a particular feature of the present invention that the scraper of the present invention is characterized by both "floating action", in which mode of operation the weight of box 12, blade 50, and their associated assemblies provide the only force bringing the lower edges of blade 50 to bear upon the ground, and down-pressure action in which, in addition, a substantial part of the weight of the tractor is brought to bear on the lower edges of blade 50 in contact with the ground.
It is to be noted that while the abovedescribed pivoting action about pivot pin 22 of box 12 may have a total extent of, say, about 22°, other maximum pivoting or tilting angles about pivot pin 22 also fall within the scope of the present invention.
It will be seen from the above that the present invention, and the preferred embodiment shown and described herein, make possible a new method of scraper operation wherein a substantial portion of the weight of the tractor is brought to bear on the scraper blades, in addition to a method of operation which might be called "floating action", analagous in some ways to the operation of the scrapers of the prior art.
It will thus be seen that the objects set forth above, among those made apparent from the preceding description, are efficiently attained, and, since certain changes may be made in carrying out the above-described method of scraper operation and in the above scraper constructions without departing from the scope of the invention, it is intended that all matter contained in the above description and shown in the accompanying drawings shall be interpreted as illustrative and not in a limiting sense.
It is also to be understood that the following claims are intended to cover all of the generic and specific features of the invention herein described, and all statements of the scope of the invention which, as a matter of language, might be said to fall therebetween.
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A tractor-mounted scraper is disclosed in which the scraper blade has two scraping edges and is mounted in a box assembly having two side plates, the blade being mounted on pivots located near the lower edges of the side plates and near the outer edges of the side plates, remote from the tractor. The box assembly is mounted on one end of the tractor, on pivoted arms which are maintained parallel to each other. A power-operated tilting head is mounted rigidly on the parallel arms, and the side plates are rigidly mounted on the moving part of the tilting head by means of a transverse beam, so that the blade neither wanders from side-to-side with respect to the longitudinal axis of the tractor, nor is permitted to tilt with respect to the axis of the pivots by which the attachment is mounted to the tractor, except as permitted by the power-operated tilting head. A hydraulic cylinder is provided for (a) raising the blade and side plates out of contact with the ground, (b) pressing downwardly on the blade and side plate assembly so that the end of the tractor nearest the attachment is supported solely by the blade, and (c) permitting the blade to rest upon the ground, bearing the weight of the side plates, the beam, the tilting head, etc., but not bearing the weight of the tractor, when hydraulic cylinder is in its neutral, unpowered condition. A hydraulic cylinder is also provided for tilting the blade about its pivots, to lower one or the other of blade's two scraping edges.
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TECHNICAL FIELD
[0001] The present invention relates to a method for the treatment of septic shock by administering levosimendan, or (-)-[[4-(1,4,5,6-tetrahydro-4-methyl-6-oxo-3-pyridazinyl)phenyl]hydrazono]propanedinitrile (I), or pharmaceutically acceptable salts thereof, to a patient in need of such treatment.
BACKGROUND OF THE INVENTION
[0002] Levosimendan, which is the (-)-enantiomer of [[4-(1,4,5,6-tetrahydro-4-methyl-6-oxo-3-pyridazinyl)phenyl]hydrazono]propanedinitrile, and the method for its preparation is described in EP 565546 B1. Levosimendan is potent in the treatment of heart failure and has significant calcium dependent binding to troponin. Levosimendan is represented by the formula:
[0003] The hemodynamic effects of levosimendan in man are described in Sundberg, S. et al., Am. J. Cardiol., 1995; 75: 1061-1066 and in Lilleberg, J. et al., J. Cardiovasc. Pharmacol., 26(Suppl.1), S63-S69, 1995. Pharmacokinetics of levosimendan in man after i.v. and oral dosing is described in Sandell, E.-P. et al., J. Cardiovasc. Pharmacol., 26(Suppl.1), S57-S62, 1995. The use of levosimendan in the treatment of myocardial ischemia is described in WO 93/21921. The use of levosimendan in the treatment of pulmonary hypertension is described in WO 99/66912. Clinical studies have confirmed the beneficial effects of levosimendan in heart failure patients.
[0004] Septic shock (also known as sepsis) is the leading cause of morbidity and mortality in the intensive care units. Despite increased knowledge about the pathophysiology underlying the clinical symptoms mortality remains high and has not decreased substantially over the last decades.
[0005] There are several causes of septic shock including bacterial, fungal and viral infections as well as non-invasive stimuli such as multiple trauma, severe burns, organ transplantations and pancreatitis. The fatal outcome of septic shock has recently been linked to the systemic release of substantial amounts of various cytokines in the body.
[0006] Septic shock requires prompt treatment since the patient's condition often deteriorates rapidly. Symptoms of septic shock include fever, hypothermia, falling blood pressure, rapid breathing, rapid heartbeat, skin lesions and leakage of plasma proteins into the tissues, metabolic acidosis and elevated plasma lactate. Septic shock is particularly characterised by maldistribution of blood flow and disturbances in tissue oxygen in various organs of the body. Distribution of blood flow may become heterogenous with subsequent under- and overperfusion of various tissues. These disturbances have been noted both at the macro- as well as at the microcirculatory level. Septic patient usually die as a result of poor tissue perfusion and injury followed by multiple organ failure.
[0007] One of the organs in which the disturbances in nutritive flow is especially important is the gut. The importance of preserved of splanchnic blood flow in various shock conditions, including septic shock, has been largely emphasized in the literature. Reductions in splanchnic blood flow have been a suggested contributor to the development of multiple organ failure as well as maintenance of sepsis by translocation of gut derived bacteria over a hyperpermeable gut wall.
[0008] Current therapeutic strategies in sepsis include antibiotics, in certain cases surgical intervention, blood volume replacement as well as inotropic support to the failing circulation. However, the current therapy has not proven to be successful. Insufficient response to intropic drugs in terms of cardiac output is not uncommon. Also the distribution of blood flow to various organs may become negatively affected. For example, splanchnic blood flow is not increased in spite of increased cardiac output. Thus, an improved method for treating septic shock would be of great value.
SUMMARY OF THE INVENTION
[0009] It has now been found that in the porcine model of endotoxin shock levosimendan unexpectedly counteracts endotoxin-induced splanchnic hyperperfusion as well as endotoxin-induced decreases in cardiac output. These favourable effects suggest that levosimendan is particularly beneficial in the treatment of septic shock.
[0010] Therefore, the present invention provides the use of (-)-[[4-(1,4,5,6-tetra-hydro-4-methyl-6-oxo-3-pyridazinyl)phenyl]hydrazono]propanedinitrile or a pharmaceutically acceptable salt thereof in the manufacture of a medicament for the treatment septic shock.
[0011] The present invention also provides a method for the treatment of septic shock in a patient, said method comprising administering to a patient in need thereof an effective amount of (-)-[[4-(1,4,5,6-tetrahydro4-methyl-6-oxo-3-pyridazinyl)-phenyl]hydrazono]propanedinitrile or a pharmaceutically acceptable salt thereof.
BRIEF DESCRIPTION OF THE DRAWINGS
[0012] [0012]FIG. 1 shows the effect of levosimendan on the cardiac index in a porcine model of endotoxin shock compared to control.
[0013] [0013]FIG. 2 shows the effect of levosimendan on the portal blood flow index in a porcine model of endotoxin shock compared to control.
[0014] [0014]FIG. 3 shows the effect of levosimendan on the pulmonary vascular resistance index in a porcine model of endotoxin shock compared to control.
[0015] [0015]FIG. 4 shows the effect of levosimendan on the portal venous blood flow lactate in a porcine model of endotoxin shock compared to control.
DETAILED DESCRIPTION
[0016] The method of the invention comprises a step of administering to a subject an amount of levosimendan effective to reduce, inhibit or prevent symptoms of septic shock in a patient. In particular the method comprises administering to a patient an amount of levosimendan effective to counteract endotoxin-induced harmful effects on the peripheral circulation of a patient. The term “treatment of septic shock” is intended to cover therapeutic and/or prophylactic treatments. The administration of levosimendan can be enteral, e.g. oral or rectal, or parenteral, e.g. intravenous or transdermal.
[0017] The effective amount of levosimendan to be administered to a subject depends upon the condition to be treated, the route of administration, age, weight and the condition of the patient. In general levosimendan is administered orally to man in daily dose from about 0.1 to 20 mg, preferably from 0.2 to 15 mg, more preferably from 0.5 to 10 mg, given once a day or divided into several doses a day, depending on the age, body weight and condition of the patient. Levosimendan can be administered by intravenous infusion using the infusion rate typically from about 0.01 to 10 μg/kg/min, more typically from about 0.02 to 5 μg/kg/min. For the intravenous treatment of septic shock an intravenous bolus of 10-200 μg/kg followed by infusion of 0.2-3 μg/kg/min may be needed.
[0018] Levosimendan is formulated into dosage forms suitable for the treatment of septic shock using the principles known in the art. It is given to a patient as such or preferably in combination with suitable pharmaceutical excipients in the form of tablets, dragees, capsules, suppositories, emulsions, suspensions or solutions whereby the contents of the active compound in the formulation is from about 0.5 to 100% per weight. Choosing suitable ingredients for the composition is a routine for those of ordinary skill in the art. It is evident that suitable carriers, solvents, gel forming ingredients, dispersion forming ingredients, antioxidants, colours, sweeteners, wetting compounds, release controlling components and other ingredients normally used in this field of technology may be also used.
[0019] For oral administration in tablet form, suitable carriers and excipients include e.g. lactose, corn starch, magnesium stearate, calcium phosphate and talc. For oral administration in capsule form, useful carriers and excipients include e.g. lactose, corn starch, magnesium stearate and talc. For controlled release oral compositions release controlling components can be used. Typical release controlling components include hydrophilic gel forming polymers such as hydroxypropylmethyl cellulose, hydroxypropyl cellulose, carboxymethyl celluloses, alginic acid or a mixture thereof; vegetable fats and oils including vegetable solid oils such as hydrogenated soybean oil, hardened castor oil or castor seed oil (sold under trade name Cutina HR), cotton seed oil (sold under the trade names Sterotex or Lubritab) or a mixture thereof; fatty acid esters such as triglycerides of saturated fatty acids or their mixtures e.g. glyceryl tristearates, glyceryl tripalmitates, glyceryl trimyristates, glyceryl tribehenates (sold under the trade name Compritol) and glyceryl palmitostearic acid ester.
[0020] Tablets can be prepared by mixing the active ingredient with the carriers and excipients and compressing the powdery mixture into tablets. Capsules can be prepared by mixing the active ingredient with the carriers and excipients and placing the powdery mixture in capsules, e.g. hard gelatin capsules. Typically a tablet or a capsule comprises from about 0.1 to 10 mg, more typically 0.2 to 5 mg, of levosimendan.
[0021] Formulations suitable for intravenous administration such as injection or infusion formulation, comprise sterile isotonic solutions of levosimendan and vehicle, preferably aqueous solutions. Typically an intravenous infusion solution comprises from about 0.01 to 0.1 mg/ml of levosimendan.
[0022] Salts of levosimendan may be prepared by known methods. Pharmaceutically acceptable salts are useful as active medicaments, however, preferred salts are the salts with alkali or alkaline earth metals.
EXAMPLES
[0023] Pharmaceutical example.
Hard gelatin capsule size 3 Levosimendan 2.0 mg Lactose 198 mg
[0024] The pharmaceutical preparation in the form of a capsule was prepared by mixing levosimendan with lactose and placing the powdery mixture in hard gelatin capsule.
[0025] Experiments
[0026] 20 kg landrace pigs were anesthetized and catheterized. After baseline measurements 8 pigs received 200 μg/kg levosimendan as a 10 minute bolus followed by an infusion of 200 μg/kg/hour. 9 animals served as controls.
[0027] In the second phase of the experiment the animals were given an infusion of endotoxin (from E. Coli bacteria) 30 minutes after the start of the bolus dose of levosimendan. The endotoxin infusion was maintained for 3 hours and the levosimendan infusion was maintained throughout the experiment until 5 hours after onset of endoxemia. Comparison between the two groups was made with ANOVA.
[0028] The changes in the cardiac index, splanchnic (portal) blood flow index, portal venous blood lactate and pulmonary vascular resistance are shown in FIGS. 1 - 4 . In the Figures, (−0.5 h) means the start of levosimendan bolus and (0 h) the start of endotoxin infusion. The results show that levosimendan can significantly counteract endotoxin-induced circulatory disorders. All levosimendan treated animals survived whereas one animal in the control group died.
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Levosimendan, or (-)-[[4-(1,4,5,6-tetrahydro-4-methyl-6-oxo-3-pyridazinyl)phenyl]hydrazono]propanedinitrile, which has been previously suggested for the treatment of congestive heart failure is useful in the treatment of septic shock.
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BACKGROUND OF THE INVENTION
[0001] 1. (Field of the Invention)
[0002] The present invention relates to a seat assembly in general and, more particularly, to a retractable headrest assembly for an automobile seat assembly although not exclusively limited thereto.
[0003] 2. (Description of the Related Art)
[0004] In some countries over the world, seat assemblies in automotive vehicles are required by law to have a headrest for protecting one or more vehicle occupants. The headrest assembly generally in use is now available in two types, liftable and retractable types. While the liftable headrest is specifically designed to allow the position of the headrest to be adjustable to suit to the position of, for example, a vehicle driver, the currently available retractable headrest is of a structure employed in combination with a pivot or retracting mechanism by which the headrest can be pivoted forwards or rearwards between a use position and a retracted position in which the headrest is accommodated inside the seatback.
[0005] In this known retractable headrest assembly, the retracting mechanism makes use of a combination of at least one spring element with a damping device, or an electrically driven motor. In addition, installation of the known retractable headrest assembly requires a relatively large space enough to provide a hindrance to the field of view from a rear seat occupant and also to increase the weight and cost of the seat assembly as a whole.
SUMMARY OF THE INVENTION
[0006] Accordingly, the present invention has been devised to substantially eliminate the foregoing problems and inconveniences and is intended to provide a lightweight, inexpensive retractable headrest assembly employing an improved retracting mechanism effective to provide a relatively large field of view while neatly accommodated within the seatback.
[0007] In order to accomplish the foregoing and other objects and features of the present invention, there is provided a retractable headrest assembly for a seat, which includes a headrest assembly mounted on a top portion of a seatback for pivotal movement between use and retracted positions about a first axis; and a retracting mechanism for toggling the headrest assembly to either of the use and retracted positions. The retracting mechanism includes a first shaft member defining said first axis and coupled with a seatback frame, embedded in the seatback, and a biasing means for urging the headrest assembly rearwardly about the first axis.
[0008] In a preferred form of embodiment of the present invention, the retractable headrest assembly for use in a seatback includes a headrest having a frame structure embedded therein and having two spaced apart connecting portions. The seatback has a top portion formed with a recess configured to represent a shape substantially complemental to a shape of the headrest, so that when the headrest is in a retracted position, the headrest can be neatly accommodated within the recess. The headrest assembly may also include generally elongated connecting members each coupled at one end with a corresponding seatback frame embedded in the seatback so as to extend generally transverse to the associated seatback frame and axially aligned with each other to define a common axis and positioned on respective opposite sides of the recess, generally ring-shaped stop plates each rigidly secured to the respective connecting member so as to lie in a plane perpendicular to the connecting member, a bearing rod having its opposite ends coupled with the stop plates so as to extend parallel to, but be offset a distance from the common axis, and support plates pivotally mounted on the bearing rod and fixedly coupled with the connecting portions of the frame structure embedded in the headrest for movement together therewith. At least one biasing element is used and is connected between one of the support plates and one of the connecting member for retaining the headrest one of use and retracted positions about the bearing rod. This biasing element is operable to allow the headrest to be toggled to either of the use and retracted positions as the headrest being pivoted about the bearing rod move past a top dead center position defined on one side of the bearing rod opposite to the common axis.
BRIEF DESCRIPTION OF THE DRAWINGS
[0009] The present invention will become readily understood from the following description of preferred embodiments thereof made with reference to the accompanying drawings, in which like parts are designated by like reference numeral and in which:
[0010] [0010]FIG. 1 is a fragmentary perspective view of a seatback employing a retractable headrest assembly designed in accordance with the present invention, with a headrest held at a use position;
[0011] [0011]FIG. 2 is a view similar to FIG. 1, showing the headrest held at a retracted position;
[0012] [0012]FIG. 3 is an exploded view of the retracting mechanism shown in FIGS. 1 and 2;
[0013] [0013]FIG. 4 is a perspective view of the retracting mechanism showing the skeleton thereof when the headrest is held at the use position;
[0014] [0014]FIG. 5 is a view similar to FIG. 5, showing the skeleton of the headrest assembly when the headrest is held at the retracted position; and
[0015] [0015]FIG. 6 is a schematic side view of a portion of the retracting mechanism, showing an engagement between a stopper plate and a stopper bracket.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0016] This application is based on an application No. 2001-126 filed Jan. 4, 2001 in Japan, the content of which is herein expressly incorporated by reference in its entirety.
[0017] Referring first to FIGS. 1 and 2, there is shown a retractable headrest assembly R according to the present invention. The headrest assembly R is shown as used in an automobile seat assembly including a seatback S, but may be employed in any other seat such as, for example, a home reclining chair a lounger. As will be readily understood from the subsequent description, the retractable headrest assembly R according to the present invention does neither make use of an electrical installation nor any connection with an external actuating mechanism and, accordingly, the retractable headrest assembly R of the present invention can be employed in any type of seats or chairs that may be used where neither electric power nor an external drive source is available.
[0018] The retractable headrest assembly R embodying the present invention includes a headrest HR pivotable between a use position as shown in FIG. 1 and a retracted position as shown in FIG. 2 by means of the retracting mechanism generally identified by M. In FIGS. 1 and 2, the seatback S is shown to have its top portions formed with a recess 4 leaving a pair of shoulder supports Sa on respective sides thereof. As will become clear from the subsequent description, seatback support frames 2 connected at one end with, for example, seat cushion frames (not shown) or frame elements of any known seatback reclining adjustment (also not shown) extend to such an extent as to terminate within the shoulder supports Sa.
[0019] The headrest HR is shown to be of a generally triangular configuration and, hence, the recess 4 may have a correspondingly triangular configuration complemental to the shape of the headrest HR so that when the headrest HR is pivoted to the retracted position the headrest HR can be snugly and neatly accommodated within the recess 4 , although any other combination of shapes of the headrest HR and the recess 4 can be employed. It is, however, to be noted that the headrest assembly R embodying the present invention may be combined with any known headrest lift mechanism, but where no head rest lift mechanism is employed, the triangular shape of the headrest R such as shown is particularly advantageous in that when the headrest R is pivoted to the use position as shown in FIG. 1, a vertex portion of the headrest R can come to a position generally aligned with the head of a seat occupant.
[0020] Referring particularly to FIGS. 3 to 5 , respective top ends of the seatback support frames 2 may have headrest support bars 6 rigidly connected thereto, respectively, so as to extend further upwardly within the associated shoulder supports Sa. Each of the headrest support bars 6 has a transverse support rod 8 fixed at one end to the corresponding headrest support bar 6 so as to extend perpendicular thereto and also so as to face towards and be axially aligned with the transverse support rod 8 secured to the other of the headrest support bars 6 . It is to be noted that the headrest support bars 6 may be dispensed with, in which case the transverse support rods 8 are to be fixedly connected to the seatback support frames 2 so as to extend perpendicular thereto.
[0021] A generally L-shaped bracket 10 having a fixing arm and a bearing arm at right angles to the fixing arm is mounted on each of the headrest support rod 8 with the fixing arm secured thereto by means of a set bolt. A generally annular stopper plate 14 is secured to the bearing arm of each bracket 10 through an associated connecting pin 12 . The annular stopper plates 14 carried by the transverse support rods 8 in the manner described above are oriented in the same direction with their bores aligned with each other in a direction traversing the recess 4 . Although in the illustrated embodiment the transverse support rods 8 , and the connecting pins 12 separate therefrom are employed, each connecting pin 12 may be an integral part of the associated transverse rod 8 ana may hence be defined by a single rod member.
[0022] The retracting mechanism M also includes a pair of generally rectangular side plates 20 and a bearing rod 16 . Each of the rectangular side plates 20 has a bearing hole defined therein at a location adjacent one end thereof, and the bearing rod 16 has its opposite ends extending through the bearing holes in the side plates 20 and axially immovably received in the bores of the stopper plates 14 , respectively. A washer 18 may be interposed between an annular shoulder at each end portion of the bearing rod 16 and the adjacent side plate 20 . The bearing rod 16 has its longitudinal axis positioned offset a distance laterally from a common axis connecting between the connecting pins 12 by the reason which will become clear from the subsequent description.
[0023] In order to define the use and retracted positions of the headrest HR, a stopper piece 22 is fixedly mounted on, or otherwise welded to, one of opposite surfaces of each side plate 20 adjacent the corresponding annular stopper plate 14 . This stopper piece 22 is cooperable with the corresponding annular stopper plate 14 and, for this purpose, has a bottom face slidingly engaged with a portion of the outer peripheral edge of the annular stopper plate 14 substantially as best shown in FIG. 6. So far shown, a rubber piece 24 is bonded to the bottom face of each stopper piece 22 , which may not be always necessary.
[0024] The side plates 20 are connected together by means of a generally V-shaped upper headrest frame 26 having its opposite ends welded to respective upper ends thereof and a lower headrest frame 28 having its opposite ends received and fixed in position within respective holes each defined in the lower end of the associated side plate 20 so as to extend substantially parallel to the bearing rod 16 . The assembly including the side frames 20 and the upper and lower headrest frames 26 and 28 is pivotable about the bearing rod 16 between two positions corresponding to the use and retracted positions of the headrest HR. For enabling the headrest HR to be toggled between the use and retracted positions, biasing elements such as coil springs 32 are employed each having one end anchored to the adjacent connecting pin 12 and the other anchored to an associated anchor pin 30 . This anchor pin 30 is secured to each of the side plates 20 at a location on one side of the stopper piece 22 opposite to the bearing hole so as to protrude laterally towards the adjacent transverse support rod 6 .
[0025] It will readily be seen that since the longitudinal axis of the bearing rod 16 is offset laterally from the common axis aligned with the connecting pins 12 , the assembly including the side frames 20 and the upper and lower headrest frames 26 and 28 can be toggled to the use position or the retracted position by the action of the coil springs 32 while pivoting about the longitudinal axis of the bearing rod 16 .
[0026] More specifically, assuming that the headrest HR is in the use position as shown in FIGS. 1 and 4, the stopper pieces 22 are, having been pulled by the coil springs 32 , held in abutment with radially outward protrusion 14 a integral with the respective annular stopper plates 14 as best shown in FIG. 6 and, therefore, the headrest HR cannot go beyond the use position. When the headrest HR is pivoted counterclockwise about the bearing rod 16 against the coil springs 32 in readiness for the headrest HR to be accommodated neatly within the recess 4 by the application of an external pushing or pulling force acting in a forward direction confronting the position of the head of the seat occupant, and as the headrest HR passes over a top dead center position, the headrest HR can be quickly toggled over the top dead center position and then folded into the recess 4 by the action of the coil springs 32 . The dead center position referred to above is defined at a location on one side of the bearing rod 16 opposite to the common axis aligned with the connecting pins 12 , at which the coil springs 32 are axially outwardly expanded to accumulate respective energies necessary to toggle the headrest HR in the manner described above.
[0027] When the headrest HR is so pivoted to the retracted position as shown in FIGS. 2 and 5, the stopper pieces 22 are brought into engagement with radially outwardly protruding stops 14 b , as shown in FIG. 6, each integral with the corresponding stopper plate 14 , and are kept in that retracted position by the action of the coil springs 32 .
[0028] In practice, the assembly including the side frames 20 , the upper and lower headrest frames 26 and 28 , the bearing rod 16 , the coil springs 32 , and the brackets 10 is concealed within a casing (not shown) embedded in the headrest HR. The casing may includes casing halves of identical configuration made of a suitable synthetic resin. At least one of the casing halves may have a plurality of interior ribs 34 , some of which may be utilized for connection with fixture lugs 20 a , formed integrally with the side plates 20 so as to protrude transverse thereto, and fixture brackets 36 welded to the V-shaped headrest frame 26 . After such one of the casing halves have been connected to the assembly, the other of the casing halves may be welded, or otherwise bonded or screwed, to such one of the casing halves and the resultant casing is then embedded in a cushioning material to finish the headrest HR.
[0029] Although the present invention has been described in connection with the preferred embodiments thereof with reference to the accompanying drawings, it is to be noted that various changes and modifications are apparent to those skilled in the art. Such changes and modifications are to be understood as included within the scope of the present invention as defined by the appended claims, unless they depart therefrom.
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A retractable headrest assembly for a seat includes a headrest assembly mounted on a top portion of a seatback for pivotal movement between use and retracted positions about a first axis, and a retracting mechanism for toggling the headrest assembly to either of the use and retracted positions. The retracting mechanism includes a first shaft member defining the first axis and coupled with a seatback frame, embedded in the seatback, and a biasing element for urging the headrest assembly rearwardly about the first axis.
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BACKGROUND OF THE INVENTION
I. Field of the Invention
The present invention relates to waste drain pipes such as the types used with sinks, other plumbing fixtures and irrigation systems, and more particularly to sections of plumbing pipes which are designed to separate solids and other foreign bodies from the waste liquids flowing through the pipes.
II. Description of the Prior Art
The prior art includes many patent and other references which disclose plumbing devices of the type utilized for operably connecting sinks, washbasins and other such plumbing fixtures so as to prevent the flow of solid matter into the drainage system. Several of these devices are specifically designed to catch valuable items such as rings, contact lenses and so forth, which are frequently lost into the drainage system.
The prior art contains many forms of plumbing traps which employ removable strainers. The following patents are samples of those prior art references: U.S. Pat. Nos. 594,169; 3,466,901; 1,198,759; 1,903,366; 1,217,763; 2,693,734; 1,770,639; 3,747,771; 1,817,376; 3,788,485; 1,886,676; 4,032,455.
U.S. Pat. No. 3,466,901 issued to Reid discloses a generally T-shaped plumbing section which is used in conjunction with a pump in a laundry-type device. It should be noted that the Reid device does not include an access aperture which allows the operator to inspect and clean the partial strainer which is enclosed within the plumbing section. Furthermore, the Reid strainer does not effectively separate all of the solids from the fluids flowing adjacent thereto.
While many of these prior art devices are effective for their original design, they are nevertheless expensive to produce and are not directly applicable to modern plumbing fixtures and designs. These disadvantages are especially pronounced when cleaning the strainer is required. It is typically very difficult for the operator to obtain direct access to the strainer in order to remove hair, grease or other solids which foul the strainer, and in order to retrieve valuables such as rings or contact lenses from the strainer when lost into the drainage system.
The present invention is primarily designed in order to be inexpensively produced by plastic injection molding techniques. More specifically, it is envisioned that with many of the embodiments disclosed herein the strainer or screen may be integrally molded into the device in order to reduce costs and minimize assembly expenses.
BRIEF DESCRIPTION OF THE DRAWINGS
Other objects, features and advantages of the present invention will be apparant from a study of the written description and the drawings in which:
FIG. 1 illustrates a frontal cross-section elevation of a first preferred embodiment of the plumbing device in accordance with the teachings of the present invention.
FIG. 2 illustrates a frontal cross-section elevation of a second embodiment of the plumbing conduit in accordance with the teachings of the present invention.
FIG. 3 illustrates a frontal elevation of the strainer mesh of the present invention.
FIG. 4 illustrates a frontal perspective view of a third embodiment of the present invention which also employs a drain trap.
FIG. 5 illustrates a frontal cross-section view of the third embodiment as illustrated generally in FIG. 4.
FIG. 6 illustrates a frontal elevation of the strainer mesh as utilized in the third embodiment illustrated generally in FIGS. 4 and 5, and optionally in the second embodiment as illustrated in FIG. 2.
In these drawings, like reference characters refer to like parts throughout the several views of each of the embodiments of the present invention. However, variations and modifications may be effected without departing the spirit or scope of the concepts of the disclosure and the appended claims. It should also be observed that the elements and operation of the embodiments of the present invention have been illustrated in somewhat simplified form in each of these drawings and in the specification in order to eliminate unnecessary details which would be apparent to one skilled in this art.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
A frontal cross-section view of a first preferred embodiment of the plumbing coupler or fixture in accordance with the present invention is shown generally as 10 in FIG. 1. This plumbing coupler 10 includes a generally T-shaped body section 12 which defines adjacent the distended ends thereof an input portal 20, an output portal 30 and an access portal 40. The input portal 20 is generally circular in cross-section in order to form a close fit with an input pipe 28 into which the fluid and solids flow. The pipe 28 is coupled to the T-shaped body section 12 through an O-ring 24 which is pressed into firm engagement with the input pipe 28 by operation of a cap 22 which is coupled by a plurality of threads to the T-shaped body section 12.
In a similar fashion an output pipe 38 is coupled congruently within the output portal 30 and sealed therein by operation of an O-ring 34 which is compressed by operation of an output cap 32 which is coupled by a plurality of threads to the generally T-shaped body section 12.
The access portal 40 is generally closed by an access cap 42 which, together with an O-ring 44, is secured to the generally T-shaped body section 12 by a plurality of threads. The access cap 42 may be removed in order to provide direct access by the operator to an internal void 14 defined within the body section 12.
The section of the void 14 adjacent to the input portal 20 and the access portal 40 is separated from the section of the void 14 adjacent to the output portal 30 by a mesh-type strainer 50, which is also shown in a frontal view in FIG. 6. This strainer 50 includes a plurality of generally vertical members 52 and intersecting horizontal members 54 which are supported by a main circumferential frame 56. In FIG. 6 the mesh strainer 50 is illustrated as a separate unit which may be disconnected and separated from the body section 12, but in the preferred embodiment of the present invention the strainer 50 is molded integrally into the body 12 in order to eliminate costly machining and assembly expenses. The size of the apertures between the vertical members 52 and the horizontal members 54 is typically 0.3 inches square, but this dimension may be changed as required in accordance with the specific applications for which the device is required. While the present embodiment envisions molding body 12 and the strainer 50 from plastic, it may also be possible to form the strainer 50 from wire mesh, sheets of plastic with perforations or molded therein, etc.
With reference to FIG. 1, it should be noted that the strainer 50 is oriented in a generally vertical plane which is typically coincident with the circumference of the body section 12. In this manner the solid particles or other foreign bodies which are separated from the liquid by the operation of the strainer 50 will tend to be pulled downwardly by gravitational forces when the supporting forces derived from the flow of the liquid over the strainer 50 have subsided. In this manner the solid particles which are separated from the liquid will tend to fall into the lower part of the internal void 14 so as to collect generally within the access cap 42.
The collected solid materials or other contaminants may be removed from within the internal void 14 by unscrewing the access cap 42 from the end of the body section 12 adjacent to the access portal 40, and then rinsing out the internal section of the access cap 42. While the access cap 42 has been removed from the body section 12, the operator may easily clean other solid materials and contaminants from the front surface of the strainer 50 by merely inserting a cleaning device, such as a brush or similar instrument, into the void 14 and running the cleaning instrument over the strainer 50. For this reason it is desirable to locate the access portal 40 and the access cap 42 as close to the strainer 50 as practical so that the operator may use his hand or fingers for scraping clean the strainer 50.
An alternate or second embodiment of the present invention is illustrated generally in the cross-section view of FIG. 2. This embodiment is generally similar to the first embodiment illustrated in FIG. 1 except that the positions of the access portal, now referred to as 140, and the output portal, now referred to as 130, have been interchanged so as to provide a straight through flow of the liquid from the input pipe 28 to the output pipe 38. As illustrated in FIG. 2, a mesh strainer 150 has been placed within the internal void 114 within the body section 112 so that one end thereof will be elevated with respect to the horizontal. In this manner as the solid particles are separated from the fluid flowing through the strainer 50, the solid particles and other contaminants may be pulled by gravitational forces downwardly so as to come to rest generally adjacent to an access cap 142 which covers the access portal 140. A front elevation of the mesh strainer 150 is illustrated in FIG. 3 as being formed from a plurality of generally perpendicularly intersecting vertical and horizontal members as previously described with regard to FIG. 6. It will be observed that it may be necessary to construct the strainer 150 in an oval shape in order to assure that the effective area of the strainer 50 is generally coextensive with the area of flow of the fluid through the conduit 112.
It will be observed that the second embodiment may also be used in the horizontal mode, that is with the input pipe 28 and the output pipe 30 running generally horizontal, as long as the access portal 140 and the access cap 142 are located below the mesh strainer 150 for receiving the solid particulate matter and contaminants therein. In this orientation it would also be possible for the mesh strainer 150 to be mounted perpendicular to the flow of fluid at a point typically adjacent to the output portal 130, as long as the bottom edge of the strainer 150 would be adjacent to the access portal 140 for depositing the solid particulate matter adjacent thereto.
An alternate or third embodiment of the present invention is shown generally in FIGS. 4 and 5. This embodiment is basically similar to the embodiments illustrated in FIGS. 1 and 2 in that the main body section, now indicated as 60, retains its characteristic T-shape between the input pipe 28 and the output pipe 38. However, in this embodiment an extension of the input portal has been added and the size of the access portal and access cap have been enlarged.
More specifically, the body section 60 adjacent to an input portal 70 has been extended downwardly so as to communicate through an access portal 90 and into an access void or reservoir 56 defined within an access cap 92. A distended end 62 of the body section 60 opens into the reservoir 96 at a point substantially below the fluid level 66 within the body section 60 so as to function as a gas trap for preventing the flow of gases from the output pipe 30 through and into the input pipe 28. The fluid level 66 within the body section 60 will tend to stabilize at a level generally equal in vertical height to the lower end of the input pipe 38.
A mesh-type strainer 100 is located adjacent to an output portal 80 at a point generally along the extension of the circumferential body section 60. The mesh strainer 100 has an effective diameter which is generally coextensive with the effective diameter of the output pipe 38 and the output portal 80. The frontal view of the mesh strainer 100 is generally similar to the mesh strainer as illustrated in FIG. 6, and comprises a plurality of generally perpendicularly intersecting vertical and horizontal members which define liquid flow-through apertures therebetween. As with the other embodiments of this invention, the size of the apertures will be determined in accordance with the specific application of the present invention, but the apertures will be sized generally so as to prevent the passage of solid or particulate matter therethrough.
The flow of these solid particles is interrupted by the mesh strainer 100, and then the solid particles are generally pulled by gravitational forces downwardly and into the reservoir 96 defined within the access cap 92. In this manner the solid particulate matter may be removed from the trap and strainer of the plumbing fixture by merely unscrewing the access cap 92 and disconnecting it from the main body section 60. The solid materials and particles should be easily removable from within the reservoir 96 defined within the access cap 92.
As in the other embodiments, the strainer 100 is located adjacent to and generally above the access portal 90 and the access cap 92 so that gravitational forces may be utilized to draw the solid particles downwardly from the mesh strainer 100 after the pressure induced by the flow of fluid through the strainer 100 has subsided. While it is somewhat more difficult to clean hair and other long and stringy materials from the strainer 100, the separation between the distended end 62 of the body section 60 and the strainer 100 will still allow a brush or other cleaning article to be used for loosening and removing contaminants from the strainer 100. While the strainer 100 may be detachable from the body section 60, it may be possible and indeed preferable to mold the strainer 100 as an integral part of the body section 60.
The first and second embodiments of the plumbing fixtures in accordance with the present invention as illustrated in FIGS. 1 and 2 have been described primarily for use as couplings directly interposed along a section of drainage tubing. These embodiments may be utilized either with or without associated drainage traps as required. These embodiments may also be utilized for operatively coupling multiple fixtures such as sinks, etc., together so that one trap may be utilized for all of the devices. The third preferred embodiment as illustrated in FIG. 4 has been designed primarily to combine the safety of the strainer with the convenience of an integral gas trap. This embodiment may be utilized in a variety of different applications and should not be limited to conventional uses such as with respect to sinks, washbowls, drinking fountains, etc. These embodiments may also be used for the same or related purposes in well plumbing systems, irrigation systems or other similar applications.
In accordance with the provisions of the United States Patent Laws, preferred embodiments of the present invention have been described in detail. The principles of the present invention have been described in the best mode in which it is now contemplated that such principles may be applied. However, it should be understood that the construction shown and described in the attached specification and drawings are merely illustrative and that the invention is not limited thereto. Accordingly, alterations and modifications which readily suggest themselves to persons skilled in the art, without departing from the true spirit of the disclosure herein, are intended to be included in the scope of the following claims.
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A plumbing fixture with an integral strainer is provided for separating solids and other foreign bodies from a liquid flowing through a pipe. A generally T-shaped conduit section is provided having at least three portals including an input and an output portal for being operably interposed along the pipe for passing the fluid therethrough. The conduit also includes an access portal and a removable closure coupled thereto for allowing external access to within the conduit. A strainer is provided within the conduit and generally adjacent to the access portal for separating solids from the liquid flowing therethrough. The strainer is typically positioned above the access portal for allowing gravitational displacement of the solids toward the access portal after the liquid flow pressure has subsided.
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RELATED APPLICATIONS
[0001] This application is a continuation of International Application No. PCT/US03/01696, filed Jan. 21, 2003, entitled “SYSTEMS AND METHODS FOR ACKNOWLEDGMENT OF MULTI-CAST TRAFFIC,” invented by Shugong Xu, now published under International Publication No. WO 03/062955 A2; which claims the benefit of U.S. Provisional Patent Application No. 60/319,094, filed Jan. 22, 2002, entitled “METHODS AND SYSTEMS TO SUPPORT ACKNOWLEDGEMENT OF MULTI-CAST BASED ON BURST ACK,” invented by Shugong Xu and Srinivas Kandala.
BACKGROUND OF THE INVENTION
[0002] Networks may be used to efficiently transfer information between networked devices, however the variety of data now transmitted on networks requires differing protocols and methods to provide optimum efficiency and reliability. Many data networks support a number of data transfer schemes including, but not limited to unicast, broadcast and multi-cast transfer.
[0003] During unicast transfer, data is sent from a single source to a single recipient. If multiple recipients must receive the same information, the information must be sent once for each recipient. When there are many recipients of a unicast message, a network can easily become overloaded and congested.
[0004] A broadcast transfer scheme sends data from a single source to all recipients on a network at the same time. This scheme avoids multiple transmission of identical data, but all stations on the network receive the data whether they need it or not. Devices not intended to receive the information must receive it and discard it. Multicast transfer provides a limited form of broadcast in which a subset of the stations on the network agree to listen to a given multicast address. The set of participating stations is called a multicast group. To join a multicast group, a station must instruct its host interface to accept the group's multicast address. The advantage of multicasting lies in the ability to limit broadcast: every station in a multicast group can be reached with a single packet transmission, but stations that choose not to participate in a particular multicast group do not receive packets sent to the group.
[0005] Due to the difficulty of acknowledging the multicast transmission from the multicast group back to the multicast originator, current layer two multicast schemes, such as IEEE 802.11, do not provide for multicast acknowledgement. In an unreliable network, such as wireless LAN, there is a significant risk that some of the participating stations will not receive all of the multicast packets correctly. Without layer 2 multicast acknowledgment, the sender of the multicast packets cannot retransmit the lost packets without a significant delay.
[0006] For traditional applications, this is not a big problem since those applications can reply on the upper layer (e.g. Transport layer) to provide acknowledgment and retransmission to improve reliability. However, for time-sensitive, ordered data, such as digital Audio/Video (A/V) data, serious problems may arise. For digital video and audio transmission, network packets must be received in a specific order and often decoding information must be received before actual data packets can be decoded. These order requirements impose time constraints on packet reception that cannot be handled through upper layer acknowledgement techniques.
[0007] Thus, an acknowledgment scheme in Layer 2 for multicast is extremely desirable for those time-critical AV applications.
SUMMARY
[0008] Embodiments of the present invention comprise methods and systems for acknowledging the receipt of multicast network data within layer two of a network environment.
BRIEF DESCRIPTION OF THE DRAWINGS
[0009] FIG. 1 is a diagram showing a typical network configuration for some embodiments of the present invention.
[0010] FIG. 2 is a flowchart showing steps performed to acknowledge data transmission in some embodiments of the present invention.
[0011] FIG. 3 is a flowchart showing steps performed by some embodiments of the present invention for acknowledgement of data transmission.
[0012] FIG. 4 is a diagram showing a typical network configuration for some embodiments of the present invention comprising an acknowledgement sub-group.
[0013] FIG. 5 is a flowchart showing steps performed in some embodiments of the present invention comprising acknowledgement sub-groups.
[0014] FIG. 6 is a flowchart showing steps performed in some embodiments of the present invention comprising acknowledgement sub-groups wherein individual member acknowledgements are expected before further acknowledgement requests are transmitted.
DETAILED DESCRIPTION
[0015] Embodiments of the present invention may be implemented in conjunction with network environments that comply with the following standards as well as other environments. The following standards are hereby incorporated by reference:
[0016] ISO/IEC 8802-11 Information technology—Telecommunications and information exchange between systems—Local and metropolitan area networks-specific requirements-Part 11: Wireless LAN Medium Access Control (MAC) and Physical Layer (PHY) Specifications
[0017] ISO/IEC 8802-15 Information technology—Telecommunications and information exchange between systems—Local and metropolitan area networks-specific requirements-Part 15: Wireless Medium Access Control (MAC) and Physical Layer (PHY) specifications for Wireless Personal Area Networks
[0018] 802.11e-D4.0 Draft of 802.11e: Medium Access Control (MAC) Enhancements for Quality of Service (QoS), Nov 2002
[0019] Current implementations of networking technology do not acknowledge multicast data frame transmission within layer two (MAC layer) of the network environment. However, high-quality audiovisual (AV) applications in Wireless Local Area Networks (WLAN) demand a faster acknowledgement service that can operate within layer two of the network environment.
[0020] Embodiments of the present invention comprise acknowledgement methods and apparatus for multicast service in packet-based networks. Some embodiments of the present invention are particularly adaptable to implementations of IEEE 802.11(e) networks, which comprise a GroupACK (GA) feature (prior attempts at this feature were previously known as Burst ACK). However, other network configurations, such as IEEE 802.15(a) Ultra-Wide Band networks, some power-line networks and other network configurations may also be used to implement embodiments of the present invention.
[0021] Some embodiments of the present invention may be explained in reference to FIG. 1 , wherein a typical network environment 1 of embodiments of the present invention is shown. In these embodiments, a network source or server 2 may transmit information over a network 4 to multiple recipient stations 6 , 8 , 10 , 12 & 14 . A management entity 3 , which may be a part of source 2 , may be used to manage addresses and network functions. Each recipient station 6 , 8 , 10 , 12 & 14 has a Medium Access Control (MAC) layer unicast address 5 , 7 , 9 , 11 & 13 (U.ADD) as part of typical hardware and network configuration. When a multicast group is formed, a single multicast address 16 (M.ADD) is correlated by the individual group members 6 , 8 & 10 .
[0022] In this manner, a single multicast transmission can be directed to multiple station recipients without rebroadcasting to each recipient. However, when using demanding applications in unreliable, lossy networks, a quick and effective acknowledgement of the multicast transmission is useful. In many network configurations, a multicast sender 2 may not simply request acknowledgement thorough the layer two (MAC layer) multicast mechanism. This would cause all recipients to respond with an acknowledgement at the same time and all acknowledgements would not easily be received by the sender 2 in a timely manner.
[0023] After transmitting a quantity of information (i.e., one or more packets), embodiments of the present invention may send a separate Group Acknowledgement Request (GAR) to each MAC layer unicast address 5 , 7 & 9 of members of the multicast group 16 . Methods related to how the multicast sender 2 obtains and maintains these unicast addresses will be discussed in a later part of this document.
[0024] In response to the individual GARs, each station 6 , 8 & 10 in the multicast group 16 will respond with a Group Acknowledgement (GA) wherein each station 6 , 8 & 10 indicates which packets in the multicast transmission were received and which packets were lost. With this packet loss information, the source/server 2 may rebroadcast lost packets to the multicast group in time for demanding AV and multimedia applications.
[0025] Embodiments of the present invention may be further explained in reference to FIG. 2 , which designates several steps of embodiment methods. As explained above, the process may begin with a MAC layer multicast transmission 20 from a network source 2 . The multicast transmission is distributed to each member of the multicast group according to the particular network protocols and management methods. After a designated portion of the multicast transmission has been sent, the sender sends 22 an individual GAR to the MAC layer unicast addresses of each member of the multicast group.
[0026] Each member of the group responds 24 to the GAR with a GA, which acknowledges receipt of packets in the multicast transmission. When one or more of the GAs have been received, the sender may resend 26 any packets that were lost during the first multicast transmission. This process may be repeated until all data has been transmitted along with retransmission of any lost packets.
[0027] In some embodiments of the present invention, as illustrated in FIG. 3 , a sender 2 may send 70 one or more packets of data to a MAC layer multicast address. Following this transmission, the multicast sender 2 may send one GAR 72 to one member of the multicast group and then wait for the GA 74 from that member. After receiving the GA from a first member, the sender may request 76 and receive 78 acknowledgment from another member by sending a GAR to its unicast address. This process may be repeated 80 until the sender has requested acknowledgment from all the members. If the sender failed to receive an expected GA after sending out a GAR, the sender may choose to resend the GAR to this particular member immediately, or move on to the next member on the list for the acknowledgment process and get back to the failed one after other members have successfully responded to the GAR.
[0028] Once all members have acknowledged receipt of the data, the acknowledgements may be evaluated to determine which packets were not correctly received by at least one member 82 . These lost packets may be resent 84 to multicast address without any further delay.
[0029] The unicast addresses of the members in the multicast group may be sent to and maintained by the multicast sender 2 . The multicast sender may be informed of the unicast addresses of the intended participating stations through Layer 2 signaling, or through higher layer signaling. Address data may be maintained by the management entity of the sender station.
[0030] In some embodiments of the present invention, described in reference to FIG. 4 , sub-groups may be used to establish a quality of service within a multicast group. These embodiments comprise a network environment 31 in which a source or server 32 may transmit information over a network 34 to multiple recipient stations 36 , 38 , 40 , 42 & 44 . The management entity 33 , which is a part of source 32 , may be used to manage addresses and network functions. Each recipient station 36 , 38 , 40 , 42 & 44 has a Medium Access Control (MAC) layer unicast address 35 , 37 , 39 , 41 & 43 (U.ADD) as part of typical network configuration. When a multicast group is formed, a single multicast address 46 (M.ADD) is correlated by the individual group members 36 , 38 & 40 . In these embodiments, a subgroup 30 of the multicast group 46 may be maintained through a MAC layer acknowledgement service.
[0031] In these embodiments, a sender 32 may transmit one or more packets of data to a MAC layer multicast address 46 thereby attempting to deliver data to all recipients 36 , 38 and 40 within the multicast group 46 . Some members of multicast group 46 may require a reliable service that is higher than other members of the group. These members may become part of an acknowledgment or QOS sub-group for which MAC layer acknowledgement is implemented. In this case, once a sender 32 has sent one or more packets of data, sender 32 may send a Group Acknowledgement Request to the MAC layer unicast addresses 35 & 37 of each member of the acknowledgment sub-group 30 . Each acknowledgment sub-group member 36 & 38 may then respond to the GAR with a Group Acknowledgement indicating which packets have been received by each member 36 & 38 . A sender 32 may then determine whether packets have been lost and resend any lost packets to the multicast group 46 .
[0032] The steps performed by embodiments of the present invention using an acknowledgment sub-group for multicast may be explained in reference to FIG. 5 . In these embodiments, a sender transmits 60 one or more packets to a MAC layer multicast address. A sender may then send an individual Group Acknowledgement Request (GAR) 62 to the MAC layer unicast address of each member of an acknowledgment sub-group comprising one or more recipients of the initial multicast transmission. Each member of the acknowledgment sub-group may respond 64 to the GAR with a Group Acknowledgement (GA) indicating whether any packets have been lost. If packets have been lost, the sender 32 may retransmit 66 the lost packets to the members of the multicast group.
[0033] In some embodiments of the present invention, as described with reference to FIG. 6 , an acknowledgement or QOS sub-group may be established 90 at any point prior to data transmission. Data may then be sent to a MAC layer multicast address 92 . The multicast sender may then send an individual GAR to a first member 94 of the acknowledgment sub-group 30 and then wait for the GA 96 from that member. After receiving the GA from this first member, the sender may request 98 and receive 100 acknowledgment from another member on the list by sending a GAR to its unicast address. This process may be repeated 102 until the sender has requested and received acknowledgment from all members. If the sender fails to receive an expected GA after sending out a GAR, the sender may choose to resend the GAR to this particular member or move on to the next member on the list for the acknowledgment process and get back to the failed one after all other members on the acknowledgment sub-group list have successfully responded to the GAR.
[0034] Once a sufficient number of sub-group members have acknowledged, the acknowledgements may be evaluated 104 to determine which packets were not properly received by at least one station in the sub-group. These lost packets may be resent 106 to the sub-group without further delay.
[0035] The unicast addresses of the members in the acknowledgment sub-group of the multicast group may be obtained and maintained by the multicast sender. Sub-group addresses and other data may be communicated through Layer 2 signaling, or through higher layer signaling. This communication may be managed through the management entity of the sender station. In these embodiments, the sender will need to maintain a list of the unicast addresses for the acknowledgment sub-group. However, in these embodiments, the sender does not need to maintain the list of unicast addresses for the whole multicast group.
[0036] Some embodiments of the present invention may comprise sub-group management methods and systems. In these embodiments, a multicast member may inform a sender of its interest in joining an acknowledgement or QOS sub-group within a multicast group. This may be done through upper layer signaling or by other methods. In response to this request, the multicast sender may add the unicast address of the member to a sub-group list maintained by the sender.
[0037] Members of a sub-group may also be eliminated from the group under certain conditions. If a sub-group member fails to reply after a certain time period or certain number of tries, that member's unicast address may be removed from the sub-group list.
[0038] Other variations and embodiments of the invention will occur to those skilled in the art.
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Embodiments of the present invention comprise methods and systems for MAC layer acknowledgement of the receipt of network data in a multicast transfer environment. Some embodiments include methods wherein data is sent from a source to a MAC layer multicast address followed by separate acknowledgement requests, which are sent to each data recipient's MAC layer unicast address. Each recipient may then acknowledge receipt of the multicast data thereby allowing the source to resend any lost data. The MAC layer acknowledgement of these embodiments allows fast quality of service assurance compatible with demanding audio and video applications where higher level acknowledgement is not effective.
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PRIORITY
[0001] The present application is related to, and claims the priority benefit of, Great Britain Patent Application Serial No. GB1608390.9 (1608390.9), filed May 12, 2016, the contents of which are expressly incorporated herein by reference and in their entirety.
BACKGROUND
[0002] The present invention relates generally to a book and finds particular, although not exclusive, utility in a pop-up book.
[0003] The use of a light source to project an image onto a surface by illuminating a slide, transparency or plate is known. The article to be illuminated may also be solid in that light does not pass through. Rather, a shadow of the article may be cast onto the surface.
[0004] Books which include transparencies and which may be illuminated with a torch are known, for instance as described in US20090298381. However, the torch must be held in the hand meaning that if the person holding the torch also has to hold the book he has no free hands to turn the pages.
BRIEF SUMMARY
[0005] The present invention solves this problem by providing, in a first aspect, a book including a bracket for maintaining a light source at a predetermined position relative to the book such that, in use, the light source illuminates at least one article included in the book and casts its shadow, and/or projects an image after the light passes through it, onto an adjacent surface for viewing thereof.
[0006] In this respect the term “book” may include any article which includes one or more pages whether they be bound into the book or loose-leaf.
[0007] The light source may be a torch or a mobile phone. Other sources are contemplated.
[0008] The predetermined position may be relative to the distance from the at least one article.
[0009] The at least one article may include at least one of a translucent, transparent and removed portion. For instance, it may include an image of a zebra on a card where the white stripes of the zebra are cut-out, missing portions of the card.
[0010] The translucent portions may include coloured material.
[0011] The bracket may be movable relative to the book for stowing of the bracket when not in use and/or for adjusting the size of the cast shadow and/or projected image. For instance, the bracket may move away from and towards the book such that the distance from a light source associated with the bracket to the at least one article may be adjusted as required. If pushed all the way into the book the bracket may be stowed. Other ways of stowing the bracket are contemplated such as folding it across the book and removing it from the book, when not in use. In this regard, the bracket may be removably attachable to the book.
[0012] The movement of the bracket relative to the book may also be used to adjust the focus (sharpness) of the cast image.
[0013] The bracket may include a support for resting the light source thereon, in use. In this manner the light source may be placed on the support. The support may be a tray which and may possibly be flat or curved to accommodate a torch or mobile phone.
[0014] The bracket may include an attachment mechanism for releasably attaching the light source thereto. For instance, the attachment mechanism may include a sucker, a clamp or a strap. The sucker may be used to attach to one of the surfaces of a mobile phone. The clamp may be used to grip a torch. The strap may be used to hold the light source stationary relative to the book and/or it may be used to hold the light source onto the support.
[0015] The at least one article may be substantially two dimensional and may be arranged to pop-up from the book as the book is opened. For instance, the at least one article may be a pop-up page.
[0016] The bracket may be movable into and out of the book's spine, although other locations for attaching the bracket to the book are contemplated such as across one of the back covers.
[0017] The bracket may be arranged such that, in use, with the light source associated with the bracket the light beam is directed across the surface of a page in the book.
BRIEF DESCRIPTION OF THE DRAWINGS
[0018] The above and other characteristics, features and advantages of the present invention will become apparent from the following detailed description, taken in conjunction with the accompanying drawings, which illustrate, by way of example, the principles of the invention. This description is given for the sake of example only, without limiting the scope of the invention. The reference figures quoted below refer to the attached drawings.
[0019] FIG. 1 is a perspective view of a book including a bracket and mobile phone light source projecting an image onto a wall;
[0020] FIGS. 2 and 3 are plan views of the book in FIG. 1 in the closed position with the bracket retracted and extended;
[0021] FIG. 4 is a plan view of an alternative book which includes a clamp in a recess in the back cover;
[0022] FIG. 5 is a plan view of another alternative book which includes a shelf retractable into the spine of the book; and
[0023] FIG. 6 shows an end-on view of the shelf of FIG. 5 with a torch.
DETAILED DESCRIPTION
[0024] The present invention will be described with respect to certain drawings but the invention is not limited thereto but only by the claims. The drawings described are only schematic and are non-limiting. Each drawing may not include all of the features of the invention and therefore should not necessarily be considered to be an embodiment of the invention. In the drawings, the size of some of the elements may be exaggerated and not drawn to scale for illustrative purposes. The dimensions and the relative dimensions do not correspond to actual reductions to practice of the invention.
[0025] Furthermore, the terms first, second, third and the like in the description and in the claims, are used for distinguishing between similar elements and not necessarily for describing a sequence, either temporally, spatially, in ranking or in any other manner. It is to be understood that the terms so used are interchangeable under appropriate circumstances and that operation is capable in other sequences than described or illustrated herein.
[0026] Moreover, the terms top, bottom, over, under and the like in the description and the claims are used for descriptive purposes and not necessarily for describing relative positions. It is to be understood that the terms so used are interchangeable under appropriate circumstances and that operation is capable in other orientations than described or illustrated herein.
[0027] It is to be noticed that the term “comprising”, used in the claims, should not be interpreted as being restricted to the means listed thereafter; it does not exclude other elements or steps. It is thus to be interpreted as specifying the presence of the stated features, integers, steps or components as referred to, but does not preclude the presence or addition of one or more other features, integers, steps or components, or groups thereof. Thus, the scope of the expression “a device comprising means A and B” should not be limited to devices consisting only of components A and B. It means that with respect to the present invention, the only relevant components of the device are A and B.
[0028] Reference throughout this specification to “an embodiment” or “an aspect” means that a particular feature, structure or characteristic described in connection with the embodiment or aspect is included in at least one embodiment or aspect of the present invention. Thus, appearances of the phrases “in one embodiment”, “in an embodiment”, or “in an aspect” in various places throughout this specification are not necessarily all referring to the same embodiment or aspect, but may refer to different embodiments or aspects. Furthermore, the particular features, structures or characteristics of any embodiment or aspect of the invention may be combined in any suitable manner, as would be apparent to one of ordinary skill in the art from this disclosure, in one or more embodiments or aspects.
[0029] Similarly, it should be appreciated that in the description various features of the invention are sometimes grouped together in a single embodiment, figure, or description thereof for the purpose of streamlining the disclosure and aiding in the understanding of one or more of the various inventive aspects. This method of disclosure, however, is not to be interpreted as reflecting an intention that the claimed invention requires more features than are expressly recited in each claim. Moreover, the description of any individual drawing or aspect should not necessarily be considered to be an embodiment of the invention. Rather, as the following claims reflect, inventive aspects lie in fewer than all features of a single foregoing disclosed embodiment. Thus, the claims following the detailed description are hereby expressly incorporated into this detailed description, with each claim standing on its own as a separate embodiment of this invention.
[0030] Furthermore, while some embodiments described herein include some features included in other embodiments, combinations of features of different embodiments are meant to be within the scope of the invention, and form yet further embodiments, as will be understood by those skilled in the art. For example, in the following claims, any of the claimed embodiments can be used in any combination.
[0031] In the description provided herein, numerous specific details are set forth. However, it is understood that embodiments of the invention may be practised without these specific details. In other instances, well-known methods, structures and techniques have not been shown in detail in order not to obscure an understanding of this description.
[0032] In the discussion of the invention, unless stated to the contrary, the disclosure of alternative values for the upper or lower limit of the permitted range of a parameter, coupled with an indication that one of said values is more highly preferred than the other, is to be construed as an implied statement that each intermediate value of said parameter, lying between the more preferred and the less preferred of said alternatives, is itself preferred to said less preferred value and also to each value lying between said less preferred value and said intermediate value.
[0033] The use of the term “at least one” may mean only one in certain circumstances.
[0034] The principles of the invention will now be described by a detailed description of at least one drawing relating to exemplary features of the invention. It is clear that other arrangements can be configured according to the knowledge of persons skilled in the art without departing from the underlying concept or technical teaching of the invention, the invention being limited only by the terms of the appended claims.
[0035] In FIG. 1 a book 10 is shown in the open position with the page surfaces lying in a substantially horizontal plane. A pop-up slide 16 is shown extending upwardly and approximately perpendicularly away from the pages. The slide 16 includes cut-out portions 30 to form shapes such as a moon. A bracket 30 in the form of a rectilinear rod-like member extends from within the spine of the book in a plane parallel to the surface of the pages. A mobile phone 55 is attached to the end of the bracket 30 . The phone's flash is switched on providing a torch-like beam of light which is directed towards the pop-up slide 16 .
[0036] The book is held near a wall 40 such that the light projects an image 50 onto the wall after passing through and around the slide 16 . In this way the image on the slide is enlarged and illuminated.
[0037] The book 10 is held with one hand 22 and the light source is attached to the book so that the person's other hand is free turn the pages of the book as the story progresses. The shadow of the left and right hand pages of the book is indicated with reference “ 152 ” on the wall 40 .
[0038] The book may be a children's book.
[0039] With the light source attached relatively firmly to the book the book may be oriented in any direction such that the image is cast onto a wall, ceiling or floor. In other words, the image may be cast in a horizontal direction, or a vertical direction, or at any angle therebetween.
[0040] In FIG. 2 a schematic view of the book 10 is shown. The bracket 30 is shown in broken lines within the spine 20 of the book. A short portion 35 extends outwardly from the spine at the end of which is a sucker 60 . The sucker 60 may be used to attach the phone 55 to the bracket 30 . The sucker 60 may be removable when not required. It may fit into a recess (not shown) provided within the book.
[0041] The bracket may be pulled out as shown in FIGS. 1 and 3 .
[0042] In FIG. 4 an alternative book 12 is shown in the open position. The inside of the rear cover 15 is visible on the right hand side. It includes a recess 70 within which a clamp 75 may be located. The clamp 75 is attached to the rear over by a ball joint 80 . It comprises a first arm 90 attached the ball joint 80 and a second arm 100 attached perpendicularly to the distal end of the first arm 90 . At the distal end of the second arm a pincer is provided comprising two fingers 110 facing one way and an opposing finger 120 facing the opposite way. The fingers are curved inwardly so as to be able to grip a torch or other such light source between them. The fingers may be sprung, or resiliently biased so that they may be opened to fit in a torch but will then grip the torch. A torch 130 is shown in broken lines to indicate how this may be achieved.
[0043] Another ball joint may be provided at the junction of the first 90 and second 100 arms to allow adjustment of the direction of the light source and to allow the clamp 75 to be stowed in the recess 70 when not required.
[0044] Either or both of the arms 90 , 100 may be telescopic to adjust the distance between the light source and the slide (not shown).
[0045] Another alternative book 14 is shown in FIG. 5 . In this case the bracket 140 again fits inside the spine 20 and is extensible from, and retractable into, the spine 20 . However, rather than a sucker being provided at the distal end two flaps 150 are movable away from the bracket to form an approximate “V” shape to act as shelf into which a torch may be placed.
[0046] FIG. 6 shows an end-on view of the bracket 140 which has a rectangular cross-section. The two flaps 150 extend from either side of the bracket 140 but may be folded over the bracket when not required to allow the bracket to be stowed inside the spine.
[0047] A torch 130 is shown in broken lines indicating how it may be held by the shelf created by the bracket 140 and flaps 150 .
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A book 10 including a bracket 30 for maintaining a light source 55 at a predetermined position such that, in use, the light source illuminates at least one article 16 included in the book and casts its shadow, and/or projects an image 50 after the light passes through it, onto an adjacent surface 40 for viewing thereof.
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[0001] The present invention relates to a spring device and more particularly to a spring device of the type used in automatic transmissions for motor vehicles.
INCORPORATION BY REFERENCE
[0002] Automatic transmissions for vehicles often include a plurality of coil springs that are adapted to apply a biasing force against clutch plates that control the engagement of various gears in the transmission. These coil springs are assembled in a ring shaped device comprising two annular plates having a multiplicity of circumferentially spaced, parallel compression coil springs mounted therebetween. Such a ring shaped spring device is disclosed in Orlowski U.S. Pat. No. 5,306,086, which is incorporated by reference herein as the basic background to which the present invention is directed. A ring shaped spring device is also disclosed in pending application Ser. No. 10/078,465 filed on Feb. 2, 2002 which is incorporated by reference herein as the basic background to which the present invention is directed.
BACKGROUND OF INVENTION
[0003] In the ring shaped spring device disclosed in Orlowski, there is a pair of spaced apart first and second annular support plates defining the ring shape of the spring device. A plurality of circumferentially spaced parallely oriented coil springs are disposed between the annular plates so that vertical movement of one plate toward the other compresses the springs. To interconnect the plates, an integral hook is formed in one plate and a loop is integrally formed in the other plate. The hook and loop are designed so that the device can be assembled by merely locating the various coil springs and then pressing one plate toward the other. The hook snaps over the loop to lock the plates together, with the coil springs partially compressed. However, when assembled in a transmission, the ring shaped spring device is compressed further so that the hook actually disengages the loop. Consequently, during repetitive operation of the spring assembly over many years, the individual coil springs can become canted in a manner to reduce the spring constant and cause damage and/or unintended biasing forces. By compressing the spring device for shifting the gears of the automatic transmission, distortion of the coil springs in the annular direction is magnified. Consequently, the prior ring shaped spring device, as shown in Orlowski only employs the concept of integral interconnecting elements and does not address the problem of controlling the annular movement of the spaced plates during long term operation of the spring device. Orlowski also must remove four of his coil springs to provide space for integral hooks used to maintain the plates relative to one another. As a result, the force produced by the Orlowski spring device is not maximized and is not balanced. The spring assembly in copending application Ser. No. 10/078,465 is a different mechanism to overcome the deficiency of Orlowski regarding circumferential shifting. But, this design uses spaces which should accept coil springs.
THE INVENTION
[0004] The present invention relates to a ring-shaped spring device as shown in Orlowski wherein there are a plurality of locking assemblies located at circumferentially spaced positions around the ring that are each within one of the coil spring's center passage. In this respect each of these lock assemblies includes a first element extending from one of the plates toward the other plate, a second element extending in the opposite direction from the other plate to form a generally sliding contact between the first and second elements as the spaced plates move vertically to compress and release the coil springs. The first and second elements are sized and shaped to fit within the center passage of the coil spring. This configuration maximizes the force produced by the ring shaped spring device and balances the circumferentially extending spring action.
[0005] In accordance with another aspect of the present invention, the first and second elements or tabs include a guiding mechanism to restrict annular movement at the plates relative to one another. The first tab having a guide slot with a given width and which extends in a direction perpendicular to the plates. The second tab having a hook shaped guide member which extends through the guide slot to restrict the vertical movement between the two plates. The width of the hook corresponds with the width of the slot which provides the guiding mechanism between the two plates. The structure assembly procedure and operation of the present invention is different than the ring shaped spring device in Orlowski. These added features further result in the advantage of being capable of maintaining the proper annular orientation between the spaced plates during long term operation of the spring device in an automatic transmission.
[0006] Still another aspect of the present invention, the guide slot has an end remote from the plate from which the second tab extends. The distance of this end from the plate maintains the coil springs in a compressed or prestressed condition when the device is assembled.
[0007] Yet another aspect of the present invention, by providing a tab which is sized to fit within the center passage of a coil spring, one of the annular support plates can be omitted. In its place are disk shaped pressure plates for each coil spring which reduces weight. Each of the disk plates includes a locking tab surface that maintains the disk plate and spring relative to the remaining annular plate.
[0008] Even yet another aspect of the present invention, there are an even number of locking assemblies around the circumference of the annular plates. One group of locking assemblies has the first tab extending from the first plate and the second group has the first tab extending from the second plate. By using two groups of locking assemblies, the tabs of a plate alternate between a tab with the guide slot and a tab with the hook. The tabs may be integrally formed in the guide plates as in Orlowski. In the one embodiment, four locking assemblies are used wherein the integral tabs at the twelve o'clock position and six o'clock position have one construction and the tabs at the three o'clock position and nine o'clock position have the opposite configuration. By merely indexing the plates 90°, identical plates can be used in constructing the ring shaped spring device.
[0009] Yet a further aspect of the present invention relates to utilizing molded tab components which incorporate one-way barbs or locking tabs to maintain the plates relative to one another. In this respect, one of the annular plates includes a plurality of spaced receptacles corresponding to the position of the coil springs. The receptacles are sized so that the coil springs fit about the receptacle. The other annular ring includes posts which also correspond to the position and number of coil springs. The receptacle is shaped to receive the post and includes one-way or locking barbs such that once the post enters the receptacle, it can not be removed.
[0010] Another aspect of the present invention involves spring tabs to locate the coil springs around the annular plates. These spring tabs are lanced from the edge of the annular plates and are bent downwardly at circumferentially spaced locations around the plates. The tabs are bent downwardly from a point generally at the midpoint of the plates, whereby the coil springs are located by the tabs in or near the center of the annular plates. This configuration allows the spring tabs to be produced by a simple punch press operation that first lances and then bends the tabs relative to the plate. This operation is much simpler than the complex bending operation required in Orlowski.
[0011] An object of the present invention is the provision of an improved ring-shaped spring device having two annular plates used to capture and locate circumferentially spaced coil springs, wherein the spring device guides the movement of the annular plates as the springs are compressed and/or released and solving the deficiencies of Orlowski U.S. Pat. No. 5,306,086.
[0012] Another object of the present invention is the provision of a spring device which utilizes locking assemblies that fit within the center passage of one of the coil springs so as to maximize the number of springs that can be utilized and balancing the spring action around the assembly.
[0013] Yet a further object of the present invention is the provision of a ring-shaped spring device wherein spaced annular plates are held together by lock assemblies having members that limit the movement between the plates to a generally vertical sliding movement as the plates move vertically to compress and/or release the coil springs, so the plates are fixed in a circumferential direction.
[0014] Even yet a further object of the present invention is the provision of replacing one annular ring with independent disk shaped pressure plates corresponding to each coil spring.
[0015] Another aspect of the present invention is the provision of utilizing molded components having one-way or locking barbs that can be easily snap-fitted together.
[0016] Even yet another object of the present invention is the provision of eliminating one annular ring by utilizing coil spring which can interengage with the other annular ring.
[0017] These and other objects and advantages will become apparent from the following description taken together with the accompanying drawings.
BRIEF DESCRIPTION OF DRAWINGS
[0018] [0018]FIG. 1 is a top plan view of the ring shaped spring device constructed in accordance with an embodiment of the present invention;
[0019] [0019]FIG. 2 is an enlarged cross-sectional view taken generally along line 2 - 2 of FIG. 1;
[0020] [0020]FIG. 2A is an enlarged cross-sectional view taken generally along line 2 - 2 of FIG. 1 , however, the top hook tab is formed from material near the inner rim of top annular ring;
[0021] [0021]FIG. 3 is a cross-sectional view taken generally along line 3 - 3 of FIG. 2;
[0022] [0022]FIG. 3A is a cross-sectional view taken generally along line 3 A- 3 A of FIG. 2A;
[0023] [0023]FIG. 4 is an enlarged exploded partial view of the spring device shown in FIG. 1;
[0024] [0024]FIG. 5 is an enlarged cross-sectional view of another embodiment of a ring shaped spring device according to the present invention;
[0025] [0025]FIG. 6 is a cross-sectional view taken generally along line 6 - 6 of FIG. 5;
[0026] [0026]FIG. 7 is a top plan view showing another embodiment of a ring shaped spring device according to the present invention;
[0027] [0027]FIG. 8 is an enlarged cross-sectional view taken generally along line 8 - 8 of FIG. 7;
[0028] [0028]FIG. 9 is an enlarged cross-sectional view taken generally along line 9 - 9 of FIG. 7;
[0029] [0029]FIG. 10 is an enlarged exploded partial perspective view of the ring-shaped device shown in FIG. 7;
[0030] [0030]FIG. 11 is a top plan view of yet another embodiment of a ring shaped spring device according to the present invention;
[0031] [0031]FIG. 12 is an enlarged cross-sectional view taken generally along line 12 - 12 of FIG. 11;
[0032] [0032]FIG. 13 is an enlarged cross-sectional view taken generally along line 13 - 13 of FIG. 11;
[0033] [0033]FIG. 14 is an enlarged cross-sectional view taken generally along line 14 - 14 of FIG. 11;
[0034] [0034]FIG. 15 is an enlarged cross-sectional view taken generally along line 15 - 15 of FIG. 11 ;
[0035] [0035]FIG. 16 is an enlarged exploded partial perspective view of the spring device shown in FIG. 11;
[0036] [0036]FIG. 17 is a top plan view of even yet another embodiment of a spring shaped spring device according to the present invention;
[0037] [0037]FIG. 18 is an enlarge cross-sectional view taken generally along line 18 - 18 of FIG. 17;
[0038] [0038]FIG. 19 is a cross-sectional view taken generally along line 19 - 19 of FIG. 18;
[0039] [0039]FIG. 20 is an exploded partial perspective view of the spring device shown in FIG. 17;
[0040] [0040]FIG. 21 is a top plan view of still yet a further embodiment of a ring shaped spring device according to the present invention;
[0041] [0041]FIG. 22 is an enlarged cross-sectional view taken generally along line 22 - 22 of FIG. 21; and,
[0042] [0042]FIG. 23 is an exploded partial perspective view of the spring device shown in FIG. 21.
DESCRIPTION OF PREFERRED EMBODIMENTS
[0043] Referring now to the drawings, wherein the showings are for the purpose of illustrating preferred embodiments of the invention only and not for the purpose of limiting same, FIGS. 1, 2, 3 and 4 show a ring shaped spring device 8 having annular spaced-apart plates 10 , 12 with outer rims 14 , 16 , respectively, and inner edges 15 , 17 . Plates 10 , 12 are coaxial to axis 18 and include spring tabs 20 of plate 10 and spring tabs 22 of plate 12 . The tabs, sometimes called “elements”, are lanced from a center portion of its respective plate and are bent to locate at circumferentially spaced positions a number of coil springs 30 . The spring tabs 20 , 22 have spaced distal edges 20 a , 22 a facing one another and have a length such that there is a gap between edges 20 a , 22 a when device 8 as a whole is in a free state. Edges 20 a , 22 a engage one another to limit the vertical movement of plates 10 , 12 toward one another. The widths W of the spring tabs are just slightly smaller than the diameters of passages 32 of springs 30 . Any number of tabs and springs can be circumferentially spaced around plates 10 , 12 . In a preferred embodiment, twenty-four springs are employed and are equally spaced around plates 10 , 12 . The tabs or elements extend through the springs so there is no circumferential gap in the circular array of coil springs.
[0044] Four lock assemblies 40 , 42 , 44 and 46 are utilized to maintain plates 10 , 12 relative to one another and are positioned within center passages 32 A, 32 B, 32 C and 32 D of coil springs 30 A, 30 B, 30 C and 30 D respectively. By positioning the lock assemblies within the coil springs, four additional coil springs can be utilized thereby increasing the possible overall spring force of spring device 8 without changing the design of coil springs 30 . All lock assemblies 40 , 42 , 44 and 46 are essentially the same, however, the orientation of the assemblies is alternated one lock assembly to the next which allows plates 10 , 12 to be identical. In this respect, while each lock assembly is structurally the same, lock assemblies 40 , 44 are oriented in one direction and lock assemblies 42 , 46 are oriented in the opposite direction. Plates 10 , 12 are merely positioned facing each other and are rotated 90° relative to one another about axis 18 to properly align lock assemblies 40 , 42 , 44 and 46 . The advantage of this concept is that by using identical plates, manufacturing and inventory costs can be reduced.
[0045] Since all lock assemblies 40 , 42 , 44 and 46 are structurally the same, only lock assembly 40 will be described in detail and this description applies to the other lock assemblies 42 , 44 and 46 . However, as stated above, assemblies 42 , 46 are oriented differently. Lock assembly 40 includes hook tabs 50 , 52 which are provided on the opposite plates 10 , 12 . Tabs 50 , 52 are created by forming a lanced portion of plates 10 , 12 , respectively, wherein tabes 50 , 52 are still attached to plates 10 , 12 , at bases edges 54 , 56 respectively. Turning to tab 50 , it is lanced from an outer portion of plate 10 such that there is a gap in plate 10 from base edge 54 which extends radially outwardly to rim 14 . Tab 50 is bent at base edge 54 at a 90 degree angle from plate 10 toward plate 12 and includes a base portion 66 , an extension 68 and a distal end 58 . Tab 50 further includes a hook 62 on distal end 58 which is opened toward outer rim 14 . Tab 52 is lanced from an inner portion of plate 12 such that there is a gap in ring 12 from base edge 56 which extends radially inwardly to edge 17 . Tab 52 is bent at base edge 56 at a 90 degree angle from plate 12 towards plate 10 and includes base portion 70 , an extension 72 and a distal end 60 . Tab 52 further includes a hook 64 on distal end 60 which is opened toward inner edge 17 . When plates 10 , 12 are move vertically toward one another, hooks 62 , 64 pass over each other and then prevent the plates 10 , 12 from being separated vertically. As a result, plates 10 , 12 can move vertically relative to one another, however, hooks 62 , 64 prevent separation of the plates. The length of tabs 50 , 52 determine the free-state height of device 8 as a whole and maintain the springs in a prestressed condition. In this respect coil springs 30 have a free-state spring height which is different than the overall free-state height of device 8 . The free-state spring height is achieved when coil springs 30 are unstressed and allowed to extend to a maximum spring height (not shown). The gap between plates 10 , 12 is less than the free-state height for coil springs 30 when hooks 62 , 64 are interengaging with one another. Accordingly, spring 30 is exerting a force against plates 10 , 12 even when the overall spring device 8 is in its unstressed or free-state condition. When an external force is applied to spring device 8 , plates 10 , 12 move vertically downwardly toward one another and hooks 62 , 64 disengage. As discussed above, the downward vertical motion is limited by edges 20 a , 22 a of spring tabs 20 , 22 respectively.
[0046] In the following discussions concerning other embodiments, the components of the spring device which remain the same, as discussed above, will include the same reference numbers as above.
[0047] Referring to FIGS. 2A and 3A, Lock assembly 40 a is shown which works the same was as lock assembly 40 except it includes hook tabs 52 and 50 a . While tab 52 is the same as describe above, tab 50 a is lanced from an inner portion of plate 10 a such that there is a gap in ring 10 a from base edge 54 a which extends radially inwardly to edge 15 . Tab 50 a is bent at base at a 90 degree angle from plate 10 a toward plate 12 . Tab 50 a is bent at base edge 54 a and includes a distal end 58 a with a hook 62 a which is opened toward outer rim 14 just like hook 62 . The only difference being that tab 50 a is formed from an inner portion of plate 10 a while tab 50 is formed from the outer portion. In similar fashion as assembly 40 , when plates 10 a , 12 are move vertically toward one another, hooks 62 a , 64 pass over each other and then prevent the plates 10 a , 12 from being separated vertically.
[0048] Referring to FIGS. 5 and 6, a ring shaped spring device 100 is shown which is essentially the same as device 8 above except for a modification to the locking assemblies. More particularly, spring device 100 includes annular spaced-apart plates 10 , 102 with outer rims 14 , 104 , respectively. Plates 10 , 102 are coaxial to axis 18 and include spring tabs 20 (not shown) of plate 10 and spring tabs 22 (not shown) of plate 102 which are configured the same as above and therefore will not be discussed in detail. Any number of tabs and springs can be circumferentially spaced around plates 10 , 102 . In a preferred embodiment, twenty-four springs are employed and are equally spaced around plates 10 , 102 .
[0049] Four lock assemblies 110 , 112 , 114 and 116 (only 110 is shown) are utilized to maintain plates 10 , 102 relative to one another. As with device 8 , assemblies 110 , 112 , 114 and 116 are structurally the same except that they are oriented differently to allow plates 11 , 102 to be identical. Therefore only assembly 110 will be described in detail and this description applies to the other lock assemblies 112 , 114 and 116 . Assembly 110 is positioned within center passage 32 A of coil spring 30 A and includes hook tab 50 , described above, and slot tab 122 . Slot tab 122 is formed from an inner portion of plate 102 and extends from a base edge 124 to a distal end 126 . Tab 122 extends at a 90° angle from plate 102 toward plate 10 and has a maximum width 128 allowing it to fit within center passage 32 A. Extending vertically in tab 122 is an elongated slot 130 having a width 132 , a length 134 and a slot edge 136 near distal end 126 . Side edges 138 , 140 are essentially parallel to one another and extend from either side of slot edge 136 toward plate 102 . Tab hook 62 along with extension 68 have essentially a common width which is slightly smaller than slot width 132 such that hook 62 can extend through slot 130 . Accordingly, when plates 10 , 102 are assembled, hook 62 first engages slot tab 122 and then enters slot 130 . Once in slot 130 , the engagement between hook 62 and slot edge 136 prevents separation of plates 10 , 102 . In addition, the length of tab 50 and slot 130 determine the free-state height of device 100 as a whole and maintains springs 30 in a prestressed condition. Movement of plates 10 and 102 relative to one another about axis 18 is controlled by the engagement between hook 62 and slot edges 138 , 140 . In this respect, hook 62 has hook edges 142 , 144 and rotation is prevented in one direction by the engagement between slot edge 138 and hook edge 142 and in the other direction by the engagement between hook edge 144 and slot edge 140 .
[0050] Referring now to FIGS. 7-10, a ring shaped spring device 200 is shown which includes only one annular plate 202 . Plate 202 includes an outer rim 204 and an inner edge 205 . Plate 202 further includes spring tabs 206 which are lanced from an inner portion of plate 202 wherein tabs 206 are still attached to plate 202 at base edges 207 . In this respect, tabs 206 are formed by an inner portion of plate 202 such that there is a gap in plate 202 from base edge 207 which extends radially inwardly to edge 205 . Tabs 206 are bent at a 90 degree angle at base edge 207 from plate 202 . The widths W of the spring tabs are smaller than the diameters of the passages 208 of springs 210 . Any number of tabs and springs can be circumferentially spaced around plate 202 . In a preferred embodiment, twenty-four springs are employed and they are equally spaced around plate 202 .
[0051] Each spring tab 206 includes a vertically extending slot 212 having a top edge 214 , a bottom edge 216 and parallel side edges 218 and 220 . Each spring 210 , is made from a single wire 228 and includes a bottom edge 230 which rests on plate 202 and a top edge 232 spaced from bottom edge 230 . Spring 210 further includes extension 234 which is a continuation of wire 228 and which extends downwardly into center passage 208 . At the end of extension 234 is a hook 238 shaped and sized to enter slot 212 . Spring 210 is assembled to plate 202 by urging spring 210 over tab 206 and partially compressing spring 210 until hook 238 enters slot 212 . Once hook 238 enters slot 212 it maintains spring 210 relative to plate 202 in a prestressed condition with spring bottom 230 engaging plate 202 . As spring 210 is compressed by the transmission, hook 238 rides in slot 212 between top and bottom edges 214 , 216 respectively.
[0052] Referring now to FIGS. 11-16, yet even another embodiment is shown. Shown is a ring shaped spring device 300 having annular spaced apart plates 302 , 304 with outer rims 306 , 308 , and inner edges 307 , 309 , respectively. Device 300 includes spring tabs 310 for plate 302 and spring tabs 312 for plate 304 which are each lanced from an inner portion of plates 302 , 304 , respectively, wherein tabs 310 are attached to plate 302 at bases edges 314 and tabs 312 are attached to plate 304 at base edges 316 . In this respect, tabs 310 are formed from an inner portion of the plates between base edges 314 , 316 and inner edges 307 , 309 respectively. Tabs 310 , 312 are bent at a 90 degree angle at base edges 314 , 316 . The widths W of the spring tabs are smaller than the diameters of passages 32 of springs 30 . Any number of tabs and springs can be circumferentially spaced around plates 302 , 304 . In a preferred embodiment, twenty-four springs are employed and are equally spaced around plates 302 , 304 . Spring tabs 310 , 312 have spaced distal edges 317 , 318 facing one another and have a length such that there is a gap between edges 317 and 318 when device 300 as a whole is in a free state. Edges 317 , 318 engage one another to limit the vertical movement of plates 302 , 304 toward one another.
[0053] Four lock assemblies 320 , 322 , 324 and 326 are positioned about plates 302 , 304 . While four such assemblies are shown, as with the other embodiments, a different number of assemblies could be utilized. As with previous embodiments, assemblies 320 , 322 , 324 and 326 are structurally the same except that they could be oriented differently to allow plates 302 , 304 to be identical. Therefore only assembly 320 will be described in detail and this description applies to the other lock assemblies 322 , 324 and 326 . Referring with particular reference to FIGS. 14, 15 and 16 , lock assembly 320 includes a hook tab 350 and a notch tab 352 . Tabs 350 , 352 are created by forming a lanced portion of plates 302 , 304 , respectively, wherein tabes 350 , 352 are still attached to plates 302 , 304 at bases edges 354 , 356 respectively. Turning to tab 350 , it is lanced from an inner portion of plate 302 such that there is a gap in plate 302 from base edge 354 to inner edge 307 . Tab 350 is bent at base edge 354 ninety degrees from plate 302 toward plate 304 and includes a base portion 358 , an extension 360 and a distal end 362 . Extension 360 has a width which is approximately half the width of base portion 358 and further, extension 360 extends from one side of base portion 358 thereby making hook tab 350 L-shaped. Tab 350 further includes a hook 364 on distal end 362 which is opened toward inner edge 307 . Tab 352 is lanced from an inner portion of plate 304 such that there is a gap in ring 304 from base edge 356 to edge 309 . Tab 352 is bent at base edge 356 ninety degrees from plate 304 toward plate 302 and is essentially C-shaped having outer side edges 366 , 368 which extend from plate 304 towards distal end 370 of tab 352 . Side edge 368 includes a notch 372 having parallel notch edges 374 , 376 that are joined by vertical notch edge 378 . The length of notch edges 374 , 376 corresponds with the width of hook 364 . With particular reference to FIG. 15, by utilizing L-shaped hook tab 350 and C-shaped notch tab 352 , assembly 320 can fit within spring cavity 32 and can be assembled without forcing hook 364 to deform in order to pass over its engagement point on notch tab 352 . In this respect, while within cavity 32 , hook 364 can be manipulated to pass next to edge 368 and then to be positioned within notch 372 . As hook 364 is being manipulated into notch 372 , spring 30 is partially compressed. Once in notch 372 , spring 30 forces plates 302 and 304 away from one another until hook 364 engages edge 374 .
[0054] Referring now to FIGS. 17-20, a ring shaped spring device 400 is shown which includes annular spaced apart plates 402 , 404 with outer rims 406 , 408 and inner edges 407 , 409 , respectively. Spring device 400 is shown to include twenty-four lock assemblies 410 , however, it should be noted that less than twenty-four lock assemblies could be used and less than twenty-four coil springs 30 could be used. However, it is preferred that all twenty-four springs 30 are used in connection with twenty-four lock assemblies 410 . Lock assemblies 410 are all identical and each includes a receptacle 412 and a post 414 . Receptacle 412 is cylindrical with a base end 420 secured to plate 404 and which extends toward plate 402 . Receptacle 412 has a distal end 422 spaced from end 420 that includes an opening 424 to an inner portion 428 . Receptacle 412 further includes several barbs 426 that extend downwardly into inner portion 428 . Post 414 includes a base 430 connected to plate 402 and extends toward plate 404 . In addition, post 414 includes a tapered lead 432 which is shaped to urge barbs 426 outwardly and allow a portion of post 414 to enter inner portion 428 . Post 414 further include locking groove 434 having a cylindrical portion 436 and a frustum conical portion 438 adjacent to cylindrical portion 436 . As a result, once tapered lead 432 urges barbs 426 outwardly and allows the end of post 414 to enter inner portion 428 , barbs 426 spring into locking groove 434 thereby retaining post 414 relative to receptacle 412 . Cylindrical portion 436 provides for the compression of spring 30 by allowing post 414 to move downwardly into inner portion 428 . However, barbs 426 do not allow post 414 completely pull out of inner portion 428 . Furthermore, the vertical dimensions of post 414 and receptacle 412 are such that when barbs 426 engage edge 440 , springs 30 remain in a prestressed condition. In addition, the engagement between the post and the receptacle prevent rotational movement of plate 402 relative to plate 404 about axis 18 .
[0055] Referring to FIGS. 21-23, a ring shaped spring device 500 is shown which includes only a single annular plate 404 as described above. Spring device 500 further includes twenty-four receptacles 412 which are the same as described above with respect to spring device 400 . However, device 500 includes twenty four independent post assemblies 508 . While each post assembly 508 includes posts 414 as described above, each post assembly 508 is joined to a post disk 510 that has a diameter greater than the outer diameter of springs 30 . This results in each post assembly 508 moving independent of one another. The functional relationship between post 414 of assemblies 508 and receptacle 412 is also the same as described above with respect to spring device 400 and therefore will not be described in detail.
[0056] While considerable emphasis has been placed on the preferred embodiments of the invention illustrated and described herein, it will be appreciated that other embodiments can be made and that many changes can be made in the preferred embodiments without departing from the principles of the invention. Accordingly, it is to be distinctly understood that the foregoing descriptive matter is to be interpreted merely as illustrative of the invention and not as a limitation.
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A spring device comprising at least one annular support plate defining a ring with a central axis; a plurality of circumferentially spaced, parallel oriented coil springs disposed about the at least one annular plate; and, a plurality of lock assemblies spaced about the plate. Each of the lock assemblies being in position within a spring cavity of one of the coil springs to allow additional springs to be provided on the spring device. In addition, the lock assemblies are dimensioned so that the coil spring is retained in a prestressed condition.
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CROSS-REFERENCE TO RELATED APPLICATION
[0001] Not applicable.
STATEMENT REGARDING FEDERALLY SPONSORED RESEARCH OR DEVELOPMENT
[0002] Not applicable.
[0003] Reference to a “Computer Listing Appendix submitted on a Compact Disc”
[0004] Not Applicable.
BACKGROUND OF THE INVENTION
[0005] (1) Field of the Invention
[0006] The invention relates to a method for automatically processing multiple used oil filters used for internal combustion engines for disposal, in particular for disposal in which essentially all of the residual oil is removed making the crushed canister and internal element a non-hazardous material and making the connector base plate available for recycling as scrap steel.
[0007] (2) Description of Related Art
[0008] Many state governments have classified used automotive and truck oil filters with substantial amounts of retained oil as a hazardous waste material causing a high disposal cost. A number of states have statutes that provide for special hazardous waste sites for landfill of these materials with substantial charges for their use. There is also a potential generator liability where filters have been disposed of without removing essentially all the retained oil.
[0009] Methods have been devised for removing residual oil from used filters and for removing the base plate. However, the more common method in general use for removing the oil involves crushing the filter axially with the base plate intact. Most filters are constructed with a check valve in conjunction with the base plate preventing free flow of oil out of the filter assembly during axial crushing thus leaving a substantial amount of oil. The methods devised for removing the base plate lack the simplicity and/or ruggedness needed for an economical automatic system.
[0010] The ideal location for processing used oil filters is at the service facility that removes the filter from the vehicle, in particular if the filter can be processed while it is still warm. Service facilities normally deal with more than one size of filter. This multiple size processing requirement coupled with the numerous small business locations require an economical rugged system with adaptive size processing capability.
[0011] Automatic operation is needed for uniformity of processing and for labor savings. Automatic operation also facilitates the processing of warm filters as they are removed from the vehicle, as minimal operator input is required to initiate the process.
[0012] U.S. Pat. No. 5,274,906 provides for shearing off the base plate and then crushing the canister and filter element normal to the filter axis. The mechanism as claimed in '906 is not suitable for adapting to automatic operation, particularly where it is desired for the processed filter components to have a minimum amount of residual oil or where it is desired to separate the base plate from the canister and filter element. '906 deposits the sheared connector plate and crushed canister assembly into a common receptacle where oil from subsequent cycles will drain onto previously processed filter components. It has been found that when severing filter connector plates, small pieces of the internal construction of filters are generated and it is believed that shearing plate 43 in '906 will generate shaving like pieces which will collect and fill shear plate receiving slot 58 requiring on going maintenance and thus limit the utility of apparatus described.
SUMMARY OF THE INVENTION
[0013] The invention provides a method for automatically processing multiple used oil filters used for internal combustion engines for disposal, in particular for disposal in which essentially all of the residual oil is removed making the crushed canister and internal element a non-hazardous material and making the connector base plate available for recycling as scrap steel.
[0014] Therefore, the present invention provides a method and apparatus for processing used oil filters for recycling where the connector plates are severed from the canister and where the canister and filter elements are crusher squeezing out waste oil. A processing or crushing zone with one stationary wall and one opposite and parallel movable wall is provided on guide-ways and with both walls having one edge in a common plane.
[0015] Thus, the present invention provides an apparatus for processing multiple used oil filters for an engine using oil for lubrication by shearing a connector plate of each filter from a canister and then crushing the canister which comprises (a) a fixed wall in a frame against which a used oil filter is positioned in a crushing zone with the connector plate below the canister; (b) a movable wall mounted on the frame which is movable by a driving means to engage the filter in the crushing zone to crush the filter, and which is retracted by the driving means from the crushing zone; (c) blade means mounted adjacent to the movable wall or adjacent to the fixed wall so as to shear the connector plate from the canister as the movable wall crushes the canister against the fixed wall; (d) a floor mounted on the frame for the removal of the used oil the sheared connector plate and the crushed canister from the apparatus; and (e) a feed chute with an escapement means for individually and automatically feeding the oil filters to the crushing zone based upon the position of the movable wall wherein the retaining means holds a preceding oil filter of the multiple filters away from the crushing zone until the used oil, the crushed canister and the sheared connection plate have been removed from the crushing zone of the apparatus.
[0016] The present invention further provides a process for automatically processing used oil filters of the type used in an engine which comprises (a) individually crushing the filters fed by a multiple filter feed means of an apparatus with an escapement for metering one filter at a time into a crushing zone; (b) removing a filter connector base plate from a canister of the filter in the crushing zone by a guillotine like shearing action; (c) compressing the canister of the filter with an internal filter element to a crushing pressure thereby extracting residual oil from the canister and filter element; and (d) discharging the connector plate and crushed canister filter element from the apparatus.
[0017] Further still, the present invention provides an apparatus for automatically processing used oil filters of the type used in an engine comprising (a) a multiple filter feed means with an escapement for metering one filter at a time into a zone with a blade means, which removes a connector plate from a canister of the filter by a guillotine like shearing action, compression means for compressing the canister and filter element at a crushing pressure thereby extracting residual oil from the filter element, door means for selectively discharging the crushed canister, filter element and the connector plate from the apparatus.
[0018] Further still, the present invention provides an apparatus for processing multiple used oil filters for an engine using oil for lubrication by shearing a connector plate of each filter from a canister and then crushing the canister which comprises (a) a fixed wall in a frame against which a used oil filter is positioned in a crushing zone with the filter axis parallel to the fixed wall; (b) a movable wall mounted on guideways of the frame which is movable by a driving means to engage the filter in the crushing zone to crush the filter, and which is retracted by the driving means from the crushing zone; (c) blade means mounted on the driving means adjacent to the movable wall and adjacent to the fixed wall so as to shear the connector plate from the canister as the movable wall crushes the canister against the fixed wall; (d) a retractable floor in said crushing zone mounted on the frame which retracts for the removal of the used oil, the sheared connector plate and the crushed canister from the apparatus; and (e) a feed chute with an escapement means for individually and automatically feeding the oil filters to the crushing zone based upon the position of the movable wall, wherein the retaining means holds a preceding oil filter of the multiple filters away from the crushing zone until the used oil, the crushed canister and the sheared connector plate have been removed from the crushing zone.
[0019] Further still, the present invention provides in an apparatus for processing oil filters for an engine using oil for lubrication by shearing a connector plate from a canister with a blade means which shears the connector plate and wherein the canister is crushed between a movable wall driven by a driving means and a fixed wall, the improvement which comprises an oil pump actuated by the driving means to remove the oil from a container for delivery to a storage tank, the improvement which comprises the blade means fixed to the driving means and a spring-loaded collapsible wall which engages the canister while the blade means cuts the connector plate and then the movable wall crushes the canister.
[0020] Significant features of the present invention are: (1) a retractable floor is preferably provided under the crushing zone having a horizontal surface in a first position, a retracted sloping surface in a second position and third position that is away from under the crushing zone and with said positions being in sequence with movements and positions of said movable wall. The retractable floor in the second position preferably forms a sloping surface to direct sheared off filter connector plates to a first selected location and the retractable floor in the third position is away from under said processing zone allowing processed filter canister assemblies to fall to an inclined surface directing them to a second select location.
[0021] (2) An escapement is provided for escaping one filter at a time into said processing zone. A Filter loading chute for feeding filters to be processed to said escapement.
[0022] (3) A driving mechanism is provided for driving the movable wall towards and away from said stationary wall, preferably having a spring-loaded attachment to the movable wall and having the spring-loaded attachment collapsing to solid upon the moving wall meeting predetermined resistance as the driving mechanism advances towards the stationary wall.
[0023] (4) A shearing blade is preferably attached to the driving mechanism and positioned so the shearing plane is normal and adjacent to the walls common edge and with a shearing edge leading relative to advance motion of the driving mechanism, positioned so that the shearing edge is masked by the spring-loaded movable wall when the movable wall is not meeting resistance but is extended as driving mechanism advances and movable wall meets resistance and because of the filter where upon the movable wall spring-loading collapses, shearing edge extends into and through the processing zone creating a shearing action as said blade passes said common edge of the stationary wall. A discharge means is provided for discharging processed filter components.
[0024] (5) A waste oil sump is provided for the recovered oil.
[0025] (6) The process is preferably controlled by a master control system and the process cycle is automatic.
[0026] (7) The filter axis in the processing zone is preferably vertical with the base plate down.
[0027] (8) Preferably, a pump to pump collected waste oil to a remote location is provided on the apparatus where the pump is preferably a piston type and action is slaved off said driving mechanism motion.
[0028] (9) Preferably the discharge means have paths for receiving severed base plates from a first select location and crushed filter canisters from a second select location cradles with draining provisions for holding them until a significant point in the subsequent process cycle before discharging them through diverting channels directing sheared off filter base plates to one external collection point and processed filter canisters to a second external collection point.
[0029] (10) The movable wall and the stationary wall are preferably essentially parallel to each other but one or both having a shallow concave shape in the surface running parallel to and centered with the axis of a filter in the processing zone.
[0030] (11) The driving mechanism preferably uses a hydraulic cylinder for the driving force and the shearing blade has a shearing edge which is a recessed vee shape.
[0031] (12) Preferably, the feed chute is positioned on the centerline of the crushing zone.
[0032] (13) The used filters are preferably escaped one at a time and reoriented from the feed chute slope into a vertical position on a shutter like mechanism over the crushing zone.
[0033] (14) Preferably, a shutter mechanism is operated by the action of the movable wall driving means and timed to feed the used filter into the crushing zone after the preceding crushed canister and connector plate are removed from the zone.
OBJECTS
[0034] It is the object of this invention to provide a process and apparatus for automatically processing used oil filters where the filters are placed in a feed chute having capacity for several filters and from which filters are escaped one at a time and fed into a crushing zone where the filter is supported by a an openable floor, where the filter is first clamped by an advancing of a movable wall driven by a hydraulic cylinder means positioning and holding the filter against a parallel fixed wall and where the driving means contains a shearing blade positioned to shear off a filter connector plate as the driving means with a spring-loaded attachment to the movable wall continues to advance collapsing the spring-loaded attachment exposing the blade to the filter. The shearing action continues and when the spring loading has fully collapsed, and the movable wall is solidly driven by the driving means crushing the filter canister to a crushing pressure against the stationary wall extracting the oil from the filter element and canister and where the used oil is collected in a container mounted to the apparatus.
[0035] An another objective of the invention is directing the severed connector plate in one direction away from oil draining and directing the crushed filter canister in another direction to facilitate segregation of the connector plate as scrap steel.
[0036] Another objective of the invention is an openable floor in the crushing zone to first open forming an incline plane to direct the discharged severed connector plates in one direction and on further opening having means for crushed canisters to go in another direction.
[0037] A further objective of the invention is to hold the squeeze force on the filter canister assembly for a finite period of time to facilitate more complete draining.
[0038] Still another objective of the invention is a discharge action at the start of a subsequent cycle that discharges the previously crushed filter canister and connector plate from the apparatus to separate positions for select disposal/recycle of each with the discharge action completed in a sufficiently short time so as not to drain oil from the dumping apparatus into receiving containers.
[0039] It is yet another objective of the invention to provide a pumping means for pumping the used oil from the apparatus collection container to a remote used oil storage.
[0040] These and other objects of the present invention will become increasingly apparent with reference to the following drawings and preferred embodiments.
DESCRIPTION OF THE DRAWINGS
[0041] [0041]FIG. 1 is a side view of the main apparatus components of this invention showing the primary structure and moving mechanisms, including a filter feed chute, filter escapement for feeding one filter at a time into a crushing zone, a movable wall driven by a hydraulic cylinder driving means, a fixed wall, an openable floor for supporting filter in the crushing zone, a piston type pump for pumping collected used oil, an enlarged view of the shearing blade with recessed vee shearing edges and a partial view of the apparatus supporting structure.
[0042] [0042]FIG. 2 is a top view including the hydraulic cylinder driving means in the advanced position, spring-loaded movable wall with a concave surface in contact with a crushed filter canister, the escapement shuttle in position to receive a filter from the feed chute, the escapement shuttle actuating mechanism, the used oil pump cylinder and hydraulic cylinder driving means position indicating switches.
[0043] [0043]FIG. 3 is similar to FIG. 2 except it shows the hydraulic cylinder driving means retracted and the escapement shuttle in position to escape a filter into the crushing zone.
[0044] [0044]FIG. 4 is an side view of the side opposite FIG. 1 showing detail of the pivoting supporting mechanism for the retractable (openable) floor for supporting a filter in the crushing zone and showing the path of a filter being escaped into the crushing zone.
[0045] [0045]FIG. 5 is similar to FIG. 4 but showing the hydraulic cylinder driving means nearing the full advance position and showing the filter connector plate nearly sheared off with the retractable floor positioned so as not to interfere with the shearing of the filter connector plate.
[0046] [0046]FIG. 6 is a left end projection view of FIG. 5 showing the filter support floor in the retracted downward sloping first position, used oil draining from the crushed canister and the final shearing of the connector plate and it being directed in one direction.
[0047] [0047]FIG. 7 is a view similar to FIG. 5 except the driving means is partially returned, the filter support floor is opened swung on a vertical axis providing clearance for a crushed filter canister to drop free onto a fixed sloping surface directing it in another direction.
[0048] [0048]FIG. 8 shows a mechanism for receiving a crushed filter canister from the sloping surface shown in FIG. 7 and retaining it until the start of a subsequent cycle where it is discharged by the initial advance movement of the driving means via linkage.
[0049] [0049]FIG. 9 is a schematic of the control functions which provide for automatic operation of the process.
[0050] [0050]FIG. 10 illustrates a modification to the slide bar for actuating the escapement providing spring over travel if the escapement was not free to travel its full stroke because of a fault.
[0051] [0051]FIG. 11 illustrates an improvement to the escapement means with a door incorporated on the shuttle that opens when the escapement means is adjacent to the crushing zone.
[0052] [0052]FIG. 12 is a top view illustrating the actuating means for escapement means improvement of FIG. 11.
[0053] [0053]FIG. 13A shows a means for centering filters in the crushing zone but prior to crushing and shearing of the connector plate comprising; fingers moving in equal distance from each side coming against a filter centering it.
[0054] [0054]FIG. 13B illustrates filter centering, fingers retracted so as not to interfere with escaping a filter into the crushing zone.
[0055] [0055]FIG. 13C illustrates filter centering fingers fully retracted so as not to interfere with the movable wall in the advance position.
[0056] [0056]FIG. 14A illustrates an alternate filter escapement means comprising; a feed chute aligned centrally with the crushing zone and a cradle at the lower end of the feed chute adjacent to the crushing zone hinged so as to tip-up a filter on the cradle to an axis vertical position.
[0057] [0057]FIG. 14B the alternate escapement means illustrating the cradle in the vertical tipped-up position actuated by the advance motion of the driving means depositing the filter being fed on a horizontal plate above the crushing zone with the plate attached to the driving means so that the horizontal plate is pulled out from under the tipped-up filter, as the driving means retracts, releasing the filter into the crushing zone.
[0058] [0058]FIG. 14C is a top view of the alternate escapement means.
[0059] [0059]FIG. 15 is a side view of an alternate embodiment of this invention with a moving wall solidly connected to a hydraulic cylinder driving means and an opposite wall with a spring-loaded attachment to a fixed end frame element which has a shear blade attached.
DETAILED DESCRIPTION OF THE INVENTION
[0060] All patents, patent applications, government publications, government regulations, and literature references cited in this specification are hereby incorporated herein by reference in their entirety. In case of conflict, the present description, including definitions, will control.
[0061] Reference is made to FIG. 1 illustrating hydraulic cylinder 10 mounted to a frame comprising guideways 13 and fixed wall 11 with the frame attached to floor support 47 through brackets 27 . Hydraulic cylinder 10 powers driving means 7 mounted on guideways 13 and movable wall 8 is mounted to the driving means through a spring-loaded coupling.
[0062] In FIG. 1, driving means 7 mounted on guideways 13 is returned and driving means spring-loaded attachment to movable wall 8 is fully extended. In FIG. 1 but more easily seen in FIG. 3, escapement shuttle 4 is adjacent to and in alignment with a crushing zone, formed by a fixed wall 11 , the opposite facing spring-loaded wall 8 and central to the two guideways 13 . Retractable openable floor 6 forms the bottom of the crushing zone and supports filter 3 in position 3 A in the crushing zone with the filter axis parallel to the fixed wall.
[0063] The operating cycle starts with escaping a filter into the crushing zone which begins, as seen in FIG. 2, with movable wall 8 driven to its advanced position by the driving means 7 , during the previous cycle, with bearing 24 having traveled along slide bar 23 contacting collar 25 fixed to bar 23 driving bar 23 attached to lever 16 . Lever 16 and parallel levers 17 are rotated to where shuttle cradle 4 carried by parallel levers 17 is adjacent with feed chute 1 and where filter 3 moved by gravity has enter escapement shuttle 4 . Filter 3 was previously restricted from sliding down feed chute 1 by shield 15 attached to shuttle 4 when shuttle 4 was out of position to receive filter 3 . After a driving means 7 advanced dwell period, during which time, additional used oil can drain from crushed filter canister 18 , hydraulic cylinder 10 retracts driving means 7 .
[0064] In FIG. 5 it can be seen that as driving means 7 retracts, cam 28 attached to driving means 7 , with notch 29 , engages pin 32 on floor 6 . As driving means 7 continues to retract, cam notch 29 bears on retractable floor pin 32 causing openable floor 6 to rotate about vertical pivot mounting 33 as can be seen in FIG. 7. This rotating action of openable floor 6 swings it on an arc creating an opening under the crushing zone and crushed filter canister 18 . During this same increment of driving means 7 retracting, spring-loaded movable wall 8 extends stripping crushed filter canister 18 off shear blade 9 .
[0065] Further retraction of driving means 7 and with spring-loaded movable wall 8 fully extended, crushed canister 18 is released falling by gravity onto sloping surface 43 . Draining used oil 41 follows the curved lip 42 of surface 43 directing the flow of used oil 41 downwards into collection container 39 while inertia of moving crushed canister 18 A carries it in one direction to location 44 where it enters a discharge means (not shown) leading to an external location.
[0066] During the final increment of retraction of driving means 7 , as seen in FIG. 3, sliding bearing 24 driven by ram 7 contacts collar 26 on slide bar 23 pulling bar 23 which in turn causes levers 16 and 17 to rotate counter-clockwise. Levers 17 move escapement shuttle 4 with filter 3 from a position adjacent to feed chute 1 to a position adjacent to the crushing zone. Filter 3 carried along by shuttle 4 is supported by sloping platform 19 during the later part of the transverse movement. Filter 3 is restricted from sliding axially along sloping surface 19 and out of shuttle 4 by feed chute end stop plate 5 , which is at the end of and normal to feed chute 1 , until essentially the completion of the shuttle transverse movement. End plate 5 extends towards the crushing zone (center of the machine) but ends so as to allow filter 3 in shuttle 4 , when adjacent to the crushing zone, to slide off sloping surface 19 into the crushing zone as depicted by filter 3 B. Filters in feed chute 1 are kept from advancing in feed chute 1 when shuttle 4 is not in alignment with feed chute 1 by shield plate 15 attached to shuttle 4 . With filter 3 escaped into position 3 A in the crushing zone, driving means 7 advances driven by hydraulic cylinder 10 bringing movable wall 8 into firm contact with filter in position 3 A. Driving means 7 also advances shearing blade 9 , with a recessed vee shaped cutting edge as illustrated in FIG. 1, into engagement with filter in position 3 A at essentially the top surface of filter 3 A connector plate.
[0067] As shearing blade 9 engages filter 3 A, spring-loaded movable wall 8 securely holds filter 3 A against fixed wall 11 . Further advancement of driving means 7 causes the collapse of spring-loaded attachment to movable wall 8 , crushing canister 18 and severing connector plate 38 by shearing action between blade 9 and fixed wall edge 14 . During this period of driving means 7 advance, cam bar 28 , attached to driving means 7 , as seen in FIG. 4 and FIG. 5, ramp 30 has engaged pin 32 attached to filter support floor 6 . Spring 36 holds pin 32 on floor 6 in contact with cam 28 . Pin 32 is camed downwards, by ramp 30 , causing floor 6 , as seen in FIG. 5 and FIG. 6, to rotate about horizontal pivot mounting 34 to a downward sloping angle as seen in FIG. 6.
[0068] The sloping attitude of floor 6 has two functions; first is to provide clearance for severing of filter connector plate 38 which is forced downwards as it is sheared by blade 9 ; the second function is to form an incline plane for severed connector plate 38 A to slide on in another direction to location 40 . The end of floor 6 has a curved edge, as seen in FIG. 6, which directs draining used oil 41 downwards. Inertia carries severed connector plate 38 A to location 40 where it enters a discharge means (not shown) leading to an external location.
[0069] Driving means 7 completes its advance motion crushing filter canister 18 squeezing used oil from canister 18 . It has been found when crushing filter canisters normal to their axis to extract used oil, flat wall surfaces apply more pressure to the central axis portion of the canister than to areas farthest from the filter axis. A shallow concave surface in one or both of the wall surfaces, in contact with the canister while crushing, more evenly distributes the pressure on the canister for more complete used oil extraction. This concave wall surface is illustrated in FIG. 2.
[0070] As driving means 7 completes its advance stroke, bearing 24 moved by driving means 7 motion contacts collar 25 fixed on slide bar 23 connected to lever 16 causing clockwise rotation of lever 16 and parallel levers 17 positioning shuttle 4 adjacent to feed chute 1 moving shield 15 away from contact with filters manually placed in feed chute 1 . Filters, in feed chute 1 , are now free to slide one filter increment down feed chute 1 placing the lead filter in shuttle 4 . The foregoing description of operation covers one complete cycle which will repeat automatically providing at the appropriate point of the automatic cycle, a filter to be processed is sensed in feed chute 1 by the logic controller in FIG. 9 through filter sensing switch 37 in FIG. 5.
[0071] [0071]FIG. 9 schematic illustrates the relationship between the various control components and the operation of the used oil pump. The process automatic cycle is monitored and controlled by a programmable logic controller depicted in schematic block 58 . Electrical power is fed by a power cord to an electrical magnetic contactor, also depicted in block 58 , which is energized by manual input through operator interface 59 . The contactor in turn energizes the logic controller and the hydraulic pump drive motor 63 . Hydraulic pump 64 supplies hydraulic pressure to the solenoid operated 4-way directional valve 62 . The logic controller receives input signals at significant positions in the process cycle from drive means hydraulic cylinder 10 position indicating switches 20 and 21 . When an automatic cycle is initiated through the operator interface, the logic controller in the appropriate sequence energizes one of directional valves 62 solenoids directing hydraulic pressure to the blind end of drive means hydraulic cylinder 10 causing it to advance releasing “cylinder returned” sensing switch 20 . As drive means 7 completes its forward stroke, the “cylinder advanced” sensing switch 21 is actuated. After a squeeze dwell period, the logic controller energizes the opposite solenoid on the directional valve 62 which in turn ports hydraulic pressure to the rod end of the drive means cylinder 10 causing it to retract. When hydraulic cylinder 10 drive means advances, it also extends the used oil pump cylinder 12 piston rod connected through a mechanical coupling. The used oil pump cylinder 12 draws oil from the used oil container 39 through check valve 65 . As cylinder 10 returns, retracting pump cylinder 12 piston rod, used oil is pumped out through second check valve 66 to a remote used oil storage tank.
[0072] Exception to the automatic cycle described above occurs if there is not a filter in feed chute 1 at the moment the logic controller monitors filter present switch 37 . If a filter is not present, the automatic cycle is interrupted until a filter is placed in feed chute 1 and is sensed by switch 37 .
[0073] An option, to the above process and apparatus, is illustrated in FIG. 8 for receiving crushed filter canister 18 A from location 44 and holding crushed canister 18 A before it is discharged from the apparatus until the start of advance motion of driving means 7 in the subsequent cycle. This provides a holding time for residual used oil on crushed canister 18 A to drain off. Discharge cradle 55 has provisions, not illustrated, for draining. As driving means 7 starts advancing, pawl 50 , attached to driving means 7 through pawl 50 pivot point on bracket 49 , engages pin 56 on bell crank 46 rotating bell crank clockwise. Bell crank 46 pulls on link 51 through a pivoting connection. Link 51 pulling on arm 53 attached to cradle 55 pivot shaft 54 rotates cradle 55 essentially 90 degrees, to attitude illustrated by the cradle 55 in position 55 A, where crushed canister 18 A is discharged by gravity. Immediately after cradle 55 reaches its full clockwise rotation position, it begins its return to its initial position as pawl 50 travels “over center” allowing tension spring 57 to return bell crank 46 back to stop 48 . Cradle 55 discharge cycle is completed in the first portion of driving means 7 forward stroke. Pawl 50 hangs free ( 50 B) during the remaining driving means 7 forward stroke. On driving means 7 return stroke, pawl 50 is reset as it rides up over pin 56 . This optional function can be modified to also include severed filter connector plates received from location 40 . Another feature of cradle 55 discharge cycle is the relative short time period the cradle is in the discharge position to where it could drip used oil in an unwanted place.
[0074] In practice, because of used oil viscosity, no oil drains off during the short period the cradle is in position 55 A. The above optional discharge cradle 55 cycle can be arranged with two diverting channels so as to discharge a crushed filter canister in one position and a severed connector plate to another position.
[0075] Another option to the above process and apparatus is adding door 4 A to shuttle 4 , illustrated in FIG. 11, to assist in directing filter 3 B into the crushing zone. With this added feature, linkage actuating the shuttle transverse motion is modified, as illustrated in FIG. 12, to open shuttle door 4 A subsequent to shuttle 4 completing its traverse motion to a position adjacent to the crushing zone. Shuttle 4 traverse motion is interrupted by it coming in contact with stop 19 A at which point driving means 7 still has a short distance to travel on its return stroke. As driving means 7 completes its return stroke, bar 23 pulls on bell crank 16 arm rotating bell crank 16 counter-clockwise. Bell crank 16 is on the same axis as one parallel lever 17 but is not rotationally connected. Bell crank 16 drives link 16 A transferring motion to bell crank 16 B which is on the same axis as another parallel lever 17 but has no angular drive connection to it. Traverse motion of shuttle 4 , for this option, is driven through link 4 D connecting bell crank 16 B arm with shuttle door 4 B attached by hinge 4 C which is held closed by spring 4 E. The increment of return motion of driving means 7 , after shuttle 4 has come to rest against stop 19 A, continues the transfer of motion to link 4 D which pulls on door 4 A, overcoming spring 4 E opening Door 4 D to position 4 B. This is illustrated in FIG. 11.
[0076] Opening shuttle door to position 4 B releases filter 3 and deflects filter 3 B into an axis vertical attitude as it is driven by gravity into the crushing zone. On driving means 7 forward stroke, the above apparatus motions are reversed returning shuttle 4 to its position adjacent to feed chute 1 .
[0077] Still another option to the above apparatus is spring overtravel protection added to shuttle 4 transverse drive slide bar 23 , illustrated in FIG. 10. The normal forward motion of driving means 7 is limited by the thickness of a crushed canister in the crushing zone as driving means 7 stalls against the crushed canister. In event there is not a filter in the crushing zone, driving means 7 overtravels driving the escapement linkage of FIG. 2 and FIG. 3 into an overtravel position which could cause damage. Also, if escapement motions were restricted by a misaligned filter or some other malfunction, linkage driving escapement motions could be damaged. To prevent such damage, escapement drive link slide bar 23 can be modified as illustrated in FIG. 10.
[0078] In normal operation, as driving means 7 advances, bearing 24 slides free on shouldered sleeve 24 A until bearing 24 contacts collar 25 fixed to bar 23 . Further motion of bearing 24 drives bar 23 actuating the escapement means but if shuttle 4 is restricted from moving a normal amount, for example, spring 23 C will compress allowing bar 23 to continue to travel sliding through bushing 23 D avoiding damage.
[0079] On driving means 7 return stroke, if there is a restriction to an escapement motion, bearing 24 can continue to travel causing shouldered sleeve 24 A to slide on bar 23 compressing spring 23 B and preventing damage. springs 23 B and 23 C are preloaded providing normally required driving forces without there deflection.
[0080] A further option to the above process and apparatus is a means for centering filters in the crushing zone is illustrated in FIGS. 13A, 13B and 13 C. A filter resting on floor 6 (refer to FIG. 1) in the crushing zone, is centered as driving means begins its forward stroke advancing movable wall 8 . During the first increment of movable wall 8 advance stroke but before a filter in position 3 A is griped by movable wall 8 , centering fingers 67 , under tension of spring 67 B, are released by ramps on cam bars 68 , as illustrated in FIG. 13A, to move towards each other, rotating around pivot pins 67 C, as rollers 67 A mounted on the lower side of center fingers 67 ride down the ramps on cam bar 68 , centering filter 3 A. As movable wall 8 continues to advances, centering finger rollers 67 A are engaged by perpendicular cam bar ramps 68 B which swing fingers 67 outwards to clear advancing movable wall 8 . This is illustrated in FIG. 13C. When a filter to be processed is escaped into the crushing zone, centering fingers 67 are held retracted, so not to interfere with feeding of filters, by surface 68 A of cam bars 68 . This illustrated in FIG. 13B.
[0081] An alternate system for escaping filters one at a time into the crushing zone is illustrated in FIGS. 14A, 14B and 14 C. Feed chute 1 is located centrally to the crushing zone an seen in FIG. 14B. In FIG. 14A, filter 3 is held by tip-up cradle 80 and is retained from sliding further by fixed end plate 5 that is supported by bracket 72 which is fastened to fixed wall 11 with bolts 75 . FIG. 14A shows the filer escapement apparatus with driving means 7 fully retracted. When the tip-up cradle is in the retracted or load position as illustrated in FIG. 14A the cradle presses down on leaf spring excluder 78 that is fastened to feed chute 1 by rivets 79 . In this position filters can slide down the feed chute into cradle 80 and the lead filter is stopped by end plate 5 . Deck plate 74 is fastened to driving means 7 by fasteners 81 and extends toward the crushing zone flush with the face of movable wall 8 . Deck plate 74 extends aft away from the crushing zone to providing a mounting for actuator arm 76 .
[0082] When driving means 7 advances, deck plate 74 also moves along over the top of the crushing zone acting as a shutter like device. As movable wall 8 spring loading collapses crushing canister 18 , deck plate 74 covers the crushing zone providing a support for the next filter. When driving means 7 advances, actuator arm 76 starts pushing bar 23 through free travel region 24 A. This free travel region delays action of lever arm 70 until deck plate 74 has covered the crushing zone. After bar 23 passes free travel region 24 A and has pushed through bearing 24 , to where bar collar 25 engages bearing 24 , lever arm 70 rotates cradle 80 , around pivot point 71 . Filter 3 in cradle 80 is raised clear of end plate 5 and when filter 3 is vertical the connector plate on filter 3 slips off of the top or end plate 5 , dropping to and resting on deck plate 74 over the crushing zone as illustrated in FIG. 14C by filter 3 in position 3 B. Filter 3 B now sitting on deck plate 74 falls into the crushing zone when deck plate 74 is retracted along with driving means 7 .
[0083] When deck plate 74 retracts, space opens between fixed wall 11 , stationary stabilizer wall 73 and deck plate 74 and when deck plate 74 is even with movable wall 8 , filter 3 B, restrained from moving with deck plate 74 by the backside of end plate 5 , drops into the crushing zone. FIG. 14C, illustrates, as cradle 80 lifts, leaf spring excluder 78 raises to stop next filter 2 in feed chute 1 from advancing until cradle 80 has returned to its load position, pushing excluder 78 clear of feed chute 1 pathway.
[0084] An alternate embodiment of this invention is illustrated in FIG. 15 for automatically escaping a single used oil filter from a multiple filter feed chute into a crushing zone where the filter connector plate is sheared from the filter canister, where the canister and filter element are crushed extracting retained used oil and where the sheared connector plate and crushed canister are selectively discharged from the crushing zone. In automatic operation, filter 3 is escaped from feed chute 1 and during the final increment of retraction of movable wall 7 A, filter 3 is driven, by gravity, into a crushing zone intermediate to movable wall 7 A and spring-loaded wall 8 B attached to fixed frame element 11 A, resting on crushing zone floor 6 .
[0085] With filter 3 in the crushing zone, hydraulic cylinder 10 driving means advances driving movable wall 7 A towards filter 3 A forcing it against spring-loaded wall 8 B collapsing its spring loading exposing shear blade to filter 3 A with the cutting blade essentially just above the canister connector plate severing the connector from the canister. On contact of the movable wall 7 A with filter 3 A, holding it solidly against spring loaded wall 8 B, floor 6 retracts downwards driven by cam 28 as can be seen in FIGS. 4 and 5.
[0086] Continued advancement of wall 7 A, completely collapses wall 8 B spring loading, shears the connector plate from filter 3 A canister and crushes the canister to a pressure extracting the used oil. Sheared connector plate 38 , as illustrated in FIG. 6 falls away, sliding on now sloping floor 6 to location 40 . After a dwell period in which movable wall 7 A maintains a crushing pressure on the canister for more complete draining, driving means 10 retracts, completely opening floor 6 , under the crushing zone by means of cam 28 , notch 29 engaging pin 32 on floor 6 and rotating floor 6 on its vertical axis 33 as cam 28 mounted to movable wall retracts. As movable wall 7 A continues retracting, wall 8 B spring loading extends striping crushed canister 18 off blade 9 . Further retraction releases crushed canister 18 where it falls to sloping surface 43 then slides to location 44 . The opening of floor 6 and the discharge of crushed canister 18 are as illustrated in FIG. 7. Other functions, not here described, of this alternate embodiment remain essentially as described in the primary embodiment above.
[0087] While the present invention is described herein with reference to illustrated embodiments, it should be understood that the invention is not limited hereto. Those having ordinary skill in the art and access to the teachings herein will recognize additional modifications and embodiments within the scope thereof. Therefore, the present invention is limited only by the claims attached herein.
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The invention provides a method for automatically processing multiple used oil filters ( 3, 34 ) used for internal combustion engines for disposal, in particular for disposal in which essentially all of the residual oil is removed making the crushed canister ( 18, 18 A) and internal element a non-hazardous material and making the connector base plate ( 38 A) available for recycling as scrap steel.
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FIELD OF THE INVENTION
The present invention relates to silver halide color photographic materials and, more precisely, to those with an improved colorability and an improved color image fastness to light.
BACKGROUND OF THE INVENTION
It is well known that the color development of silver halide color photographic materials is followed by a coupling reaction between an oxidized aromatic primary amine type color developing agent and a coupler contained in the material to form an indophenol, indaniline, indamine, azomethine, phenoxazine, phenazine or the like dye to thereby form a color image in the material. 5-Pyrazolone, cyanoacetophenone, indazolone, pyrazolobenzimidazole or pyrazolotriazole type couplers may be used for the formation of magenta color images.
Almost all the magenta color image forming couplers which have heretofore been studied and have been widely practically used are 5-pyrazolone type couplers. Although the dyes formed from the 5-pyrazolone type couplers have high fastness to heat and light, it is also known that these have an undesirable yellow component due to side-absorption of light at a wavelength of 430 nm or so, which causes color staining in the formed dyes.
Some magenta color image forming coupler skeletons with a reduced yellow component have heretofore been proposed, including, for example, pyrazolobenzimidazole skeletons as described in British Pat. No. 1,047,612; indazolone skeletons as described in U.S. Pat. No. 3,770,447; or 1H-pyrazolo[5,1-c][1,2,4]triazole skeletons as described in U.S. Pat. No. 3,725,067. Further, some other skeletons have recently been proposed, including, for example, 1H-imidazo[1,2-b]pyrazole skeletons as described in European Pat. No. 119,741; 1H-pyrazolo[1,5-b][1,2,4]triazole skeletons as described in European Pat. No. 119,960; 1H-pyrazolo[1,5-d]tetrazole skeletons as described in Research Disclosure, No. 24220 (June, 1984); and 1H-pyrazolo[1,5-b]pyrazole skeletons as described in Research Disclosure, No. 24230 (June, 1984).
In particular, the magenta dyes formed from 1H-pyrazolo[5,1-c][1,2,4]triazole type couplers as described in U.S. Pat. No. 3,725,067, British Pat. Nos. 1,252,418 and 1,334,515; 1H-imdazo[1,2-b]pyrazole type couplers as described in European Pat. No. 119,741; 1H-pyrazolo[1,5-b][1,2,4]triazole type couplers as described in European Pat. No. 119,860; 1H-pyrazolo[1,5-d]tetrazole type couplers as described in Research Disclosure, No. 24220 (June, 1984); and 1H-pyrazolo[1,5-b]pyrazole type couplers as described in Research Disclosure, No. 24230 (June, 1984), among the above-mentioned dyes, have excellent absorption characteristics with no side-absorption in the visible range, in a solvent such as ethyl acetate or dibutyl phthalate.
However, these couplers are still disadvantageous in that the colorability is low and the color images formed therefrom have an insufficient light fastness. In order to improve the colorability, the introduction of a sulfonamidophenylenesulfonyl group into the pyrazoloazole ring-containing molecules, such as described in Japanese Patent Application (OPI) No. 177557/84 (the term "OPI" as used herein refers to a "published unexamined Japanese patent application"), is somewhat effective, but this is still insufficient for use in color photographic materials, especially in those for prints.
Pyrazoloazole couplers whose pyrazoloazole nucleus contains a branched alkyl group at the 2-, 3- or 6-position thereof and a sulfonamidophenylenesulfonyl group at the 2-, 3- or 6-position thereof show improved fastness of color images to light but have problems that fog during development processing increases to some extent and yield of ring formation is low.
SUMMARY OF THE INVENTION
Accordingly, a first object of the present invention is to provide silver halide color photographic materials with improved color image fastness to light by the incorporation therein of a pyrazoloazole type magenta coupler which may form an azomethine dye with improved color reproducibility and a high light fastness.
A second object of the present invention is to provide silver halide color photographic materials with excellent colorability with less fog formation during development processing.
In order to attain the above-mentioned objects, the present invention provides a silver halide color photographic material which comprises at least one silver halide emulsion layer provided on a support and which is characterized by the incorporation of a pyrazoloazole type coupler of the following general formula (I) into at least one of the silver halide emulsion layer(s) or the adjacent layer(s) thereto: ##STR4## wherein Za and Zb each may represent ##STR5## R 1 and R 2 each may represent a hydrogen atom or a substituent; X represents a hydrogen atom or a group capable of being removed upon a coupling reaction with an oxidized form of an aromatic primary amine type developing agent; when Za═Zb is a carbon-carbon double bond, this may be a part of the aromatic ring in the formula; with the proviso that at least one of R 1 an R 2 is a group represented by general formulae (II) or (III): ##STR6## wherein R 3 represents a hydrogen atom or a substituted or unsubstituted alkyl group; R 4 represents a hydrogen atom or a substituent; R 5 represents a halogen atom, a substituted or unsubstituted alkoxy, aryloxy, amino, alkylthio or arylthio group; Ar represents an aryl group; Y represents an alkylene group or an arylene group; l' is an integer of 0 or 1; n is an integer of 0 or 1; and m is an integer of 1 to 3; and that when R 1 represents an alkyl group or Y represents an alkylene group, the alkyl or alkylene group is a group of which the carbon atom directly bonded to the pyrazoloazole nucleus is a primary carbon.
DETAILED DESCRIPTION OF THE INVENTION
The term "primary carbon" as used herein means that the carbon atom has two or three hydrogen atoms bonded thereto.
Preferred compounds among the pyrazoloazole type magenta couplers of general formula (I) are those represented by the following general formulae (IV), (V), (VI), (VII) or (VIII): ##STR7##
In the above general formulae (IV) through (VIII), R 1 and X have the same meanings as those with respect to general formula (I); R 21 and R 22 have the same meanings as R 2 in general formula (I); and l is an integer of 1 to 4.
The substituents in the pyrazoloazole type couplers of general formulae (IV) through (VIII) are explained in detail hereinafter.
More specifically, R 1 , R 21 and R 22 each represents a hydrogen atom, a halogen atom (such as a chlorine atom, a bromine atom or a fluorine atom), a substituted or unsubstituted alkyl group (such as a methyl group, an ethyl group, a trifluoromethyl group, a dodecyl group, a 3-(2,4-di-tert-amylphenoxy)propyl group, an allyl group, a 2-dodecyloxyethyl group, a cyclopentyl group or a benzyl group), an aryl group (such as a phenyl group, a 4-t-butylphenyl group, a 2,4-di-t-amylphenyl group or a 4-tetradecanamidophenyl group), a heterocyclic group, preferably 5- to 7-membered and containing N, O or S as hetero atom(s) (such as a 2-furyl group, a 2-thienyl group, a 2-pyrimidinyl group or a 2-benzothiazolyl group), a cyano group, a hydroxyl group, a substituted or unsubstituted alkoxy group (such as a methoxy group, an ethoxy group, an i-propoxy group, a 2-methoxyethoxy group, a 2-dodecyloxyethoxy group or a 2-methanesulfonylethoxy group), an aryloxy group (such as a phenoxy group, a 2-methylphenoxy group or a 4-t-butylphenoxy group), a heterocyclic oxy group, preferably having a 5- to 7-membered heterocyclic ring containing N, O or S as hetero atom(s) (such as a 2-benzimidazolyloxy group), an acyloxy group (such as an acetoxy group or a hexadecanoyloxy group), a carbamoyloxy group (such as an N-phenylcarbamoyloxy group or an N-ethylcarbamoyloxy group), a silyloxy group (such as a trimethylsilyloxy group), a sulfonyloxy group (such as a dodecylsulfonyloxy group), an acylamino group (such as an acetamido group, a benzamido group, a tetradecanamido group, an α-(2,4-di-t-amylphenoxy)butyramido group, a γ-(3-t-butyl-4-hydroxyphenoxy)butyramido group or an α-[4-(4-hydroxyphenylsulfonyl)phenoxy]decanamido group), an anilino group (such as a phenylamino group, a 2-chloroanilino group, a 2-chloro-5-tetradecanamidoanilino group, a 2-chloro-5-dodecyloxycarbonylanilino group, an N-acetylanilino group or a 2-chloro-5-[α-(3-t-butyl-4-hydroxyphenoxy)dodecanamido]anilino group), an amino group (such as an ethylamino group, a dimethylamino group or a methyloctylamino group), a ureido group (such as a phenylureido group, a methylureido group, an N,N-dimethylureido group or an N,N-dibutylureido group), an imido group (such as an N-succinimido group, a 3-benzylhydantoinyl group or a 4-(2-ethylhexanoylamino)phthalimido group), a sulfamoylamino group (such as an N,N-dipropylsulfamoylamino group or an N-methyl-N-decylsulfamoylamino group), a substituted or unsubstituted alkylthio group (such as a methylthio group, an octylthio group, a tetradecylthio group, a 2-phenoxyethylthio group, a 3-phenoxypropylthio group or a 3-(4-t-butylphenoxy)propylthio group), an arylthio group (such as a phenylthio group, a 2-butoxy-5-t-octylphenylthio group, a 3-pentadecylphenylthio group, a 2-carboxyphenylthio group or a 4-tetradecanamidophenylthio group), a heterocyclic thio group, preferably having a 5- to 7-membered heterocyclic ring containing N, O or S as hetero atom(s) (such as a 2-benzothiazolylthio group), a substituted or unsubstituted alkoxycarbonylamino group (such as a methoxycarbonylamino group or a tetradecyloxycarbonylamino group), a aryloxycarbonylamino group (such as a phenoxycarbonylamino group or a 2,4-di-tert-butylphenoxycarbonylamino group), a sulfonamido group (such as a methanesulfonamido group, a hexadecanesulfonamido group, a benzenesulfonamido group, a p-toluenesulfonamido group, an octadecanesulfonamido group or a 2-methoxy-5-t-butylbenzenesulfonamido group), a carboxyl group, a carbamoyl group (such as an N-ethylcarbamoyl group, an N,N-dibutylcarbamoyl group, an N-(2-dodecyloxyethyl)carbamoyl group, an N-methyl-N-dodecylcarbamoyl group or an N-[3-(2,4-di-tert-amylphenoxy)propyl]carbamoyl group), an acyl group (such as an acetyl group, a (2,4-di-tert-amylphenoxy)acetyl group or a benzoyl group), a sulfamoyl group (such as an N-ethylsulfamoyl group, an N,N-dipropylsulfamoyl group, an N-( 2-dodecyloxyethyl)sulfamoyl group, an N-ethyl-N-dodecylsulfamoyl group or an N,N-diethylsulfamoyl group), a sulfonyl group (such as a methanesulfonyl group, an octanesulfonyl group, a benzenesulfonyl group or a toluenesulfonyl group), a sulfinyl group (such as an octanesulfinyl group, a dodecylsulfinyl group or a phenylsulfinyl group), a substituted or unsubstituted alkoxycarbonyl group (such as a methoxycarbonyl group, a butyloxycarbonyl group, a dodecyloxycarbonyl group or an octadecyloxycarbonyl group) or an aryloxycarbonyl group (such as a phenyloxycarbonyl group or a 3-pentadecylphenyloxycarbonyl group).
In general formulae (IV), (V), (VI), (VII) and (VIII), X represents a hydrogen atom, a halogen atom (such as a chlorine atom, a bromine atom or an iodine atom), a carboxyl group, a group bonded via an oxygen atom (such as an acetoxy group, a propanoyloxy group, a benzoyloxy group, a 2,4-dichlorobenzoyloxy group, an ethoxyoxaloyloxy group, a pyruvinyloxy group, a cinnamoyloxy group, a phenoxy group, a 4-cyanophenoxy group, a 4-methanesulfonamidophenoxy group, a 4-methanesulfonylphenoxy group, an α-naphthoxy group, a 3-pentadecylphenoxy group, a benzyloxycarbonyloxy group, an ethoxy group, a 2-cyanoethoxy group, a benzyloxy group, a 2-phenethyloxy group, a 2-phenoxyethoxy group, a 5-phenyltetrazolyloxy group or a 2-benzothiazolyloxy group), a group bonded via a nitrogen atom (such as a benzenesulfonamido group, an N-ethyltoluenesulfonamido group, a heptafluorobutanamido group, a 2,3,4,5,6-pentafluorobenzamido group, an octanesulfonamido group, a p-cyanophenylureido group, an N,N-diethylsulfamoylamino group, a 1-piperidyl group, a 5,5-dimethyl-2,4-dioxo-3-oxazolidinyl group, a 1-benzylethoxy-3-hydantoinyl group, a 2N-1,1-dioxo-3(2H)-oxo-1,2-benzisothiazolyl group, a 2-oxo-1,2-dihydro-1-pyridinyl group, an imidazolyl group, a pyrazolyl group, a 4-chloro-1-pyrazolyl group, a 3,5-diethyl-1,2,4-triazol-1-yl group, a 3-chloro-1,2,4-triazol-1-yl group, a 5- or 6-bromobenzotriazol-1-yl group, a 5-methyl-1,2,3,4-triazol-1-yl group, a benzimidazolyl group, a 3-benzyl-1-hydantoinyl group, a 1-benzyl-5-hexadecyloxy-3-hydantoinyl group or a 5-methyl-1-tetrazolyl group), an arylazo group (such as a 4-methoxyphenylazo group, a 4-pivaloylaminophenylazo group, a 2-naphthylazo group or a 3-methyl-4-hydroxyphenylazo group), a group bonded via a sulfur atom (such as a phenylthio group, a 2-carboxyphenylthio group, a 2-butoxy-5-t-octylphenylthio group, a 4-methanesulfonylphenylthio group, a 4-octanesulfonamidophenylthio group, a 2-butoxyphenylthio group, a 2-(2-hexanesulfonylethyl)-5-tert-octylphenylthio group, a benzylthio group, a 2-cyanoethylthio group, a 1-ethoxycarbonyltridecylthio group, a 5-phenyl-2,3,4,5-tetrazolylthio group, a 2-benzothiazolylthio group, a 2-dodecylthio-5-thiophenylthio group or a 2-phenyl-3-dodecyl-1,2,4-triazolyl-5-thio group).
Compounds represented by general formulae (IV), (V) and (VI) are especially preferred among the compounds of general formulae (IV) through (VIII). The compounds represented by general formula (VI) are most preferred.
The substituents as represented by general formulae (II) and (III) are explained in detail hereafter. The substituents of general formulae (II) or (III) may be the same as R 1 , R 21 or R 22 in the aforesaid general formulae (IV) through (VIII), or otherwise, may be a group bonded to the appropriate atom of R 1 , R 21 and R 22 .
In general formulae (II) and (III), R 3 represents a hydrogen atom or a substituted or unsubstituted alkyl group (such as a methyl group, an ethyl group, an n-hexyl group, a 2-ethylhexyl group, a 2-dodecyloxyethyl group, a benzyl group or a 2-methanesulfonylethyl group); R 4 represents a hydrogen atom or the same substituents as R 1 , R 21 or R 22 , defined above; Ar represents, for example, a substituted or unsubstituted phenyl group or naphthyl group, and more precisely, a phenyl group, an α- or β-naphthyl group, a 2-chlorophenyl group, a 4-tert-octylphenyl group, a 4-dodecyloxyphenyl group, a 2,4-didodecyloxyphenyl group, a 2-chloro-5-tetradecanamidophenyl group, a 2-octyloxy-5-tert-octylphenyl group, a 3,5-didodecylsulfamoylphenyl group, a 3,5-bis(2-ethylhexyloxycarbonyl)phenyl group, a 2,5-dioctyloxyphenyl group or a 4-dodecylphenyl group; R 5 represents a halogen atom (such as a fluorine atom, a chlorine atom or a bromine atom), a substituted or unsubstituted alkoxy group (in which the alkyl residue may be linear, branched or cyclic, or may be a saturated alkyl residue or an unsaturated alkyl residue) (such as a methoxy group, a butoxy group, a hexyloxy group, an octyloxy group, an allyloxy group, a 2-dodecylthioethoxy group, a 2-propionoxy group, a 2-methoxyethoxy group or a 2-(N,N-diethylamino)ethoxy group), an aryloxy group (such as a phenoxy group, a 2-methoxyphenoxy group, a 4-tert-butylphenoxy group or a 2-phenylphenoxy group), an amino group (such as an unsubstituted amino group, an N,N-dimethylamino group, an N-methyl-N-butylamino group, a pyrrolidinyl group, a morpholino group, an N-methylanilino group, a 2-chloroanilino group, a 2-methoxy-5-methylanilino group, an N,N-dibutylamino group or an N,N-bis(2-propyloxyethyl)amino group), a substituted or unsubstituted alkylthio group (in which the alkyl residue may be linear, branched or cyclic) (such as a dodecyl group, a 2-butoxyethylthio group, a 2-(N,N-diethyl)aminoethylthio group or a 2-[2-(2-ethoxy)ethoxy]ethylthio group) or an arylthio group (such as a phenylthio group, a 2-butoxyphenylthio group, a 4-tert-octylphenylthio group or a 2-butoxy-5-tert-octylphenylthio group).
Among the substituents represented by general formulae (II) and (III), those where R 3 is hydrogen are most preferred.
Among the compounds represented by general formulae (I), (II) and (III), those where at least one of R 1 and Y represents an alkyl group or an alkylene group are particularly preferred.
Examples of the couplers of the present invention are shown hereafter; however, the couplers of the present invention are not limited in scope by the following specific examples thereof: ##STR8##
Some examples are described herein to illustrate the synthesis of the couplers of the present invention. Couplers in accordance with the present invention, other than the ones illustrated below, may also be synthesized in an analogous manner.
SYNTHESIS EXAMPLE
Synthesis of Coupler No. (1) Shown Above ##STR9##
2-(2-Aminoethyl)-7-chloro-6-methylpyrazolo[1,5-b][1,2,4]triazole dihydrochloride (A) (20 g) was dissolved in 100 ml of dimethylacetamide. The resulting solution was cooled with an ice water bath, and then 34 ml of triethylamine was added thereto and stirred for 10 minutes. To this solution was dropwise added a solution of 51.4 of 5-(5-t-octyl-2-octyloxybenzenesulfonamido)-2-octyloxybenzenesulfonyl chloride (B) as dissolved in acetonitrile (100 ml) in the course of 30 minutes. This resulting solution was stirred for 30 minutes and then the reaction mixture was poured into 400 ml of water and thereafter extracted with 200 ml of ethyl acetate. The organic layer was washed twice with 150 ml of salt solution and then dried with anhydrous magnesium sulfate. The ethyl acetate solution was concentrated to dryness and the residue was then dissolved in 50 ml of ethyl acetate under heat. 300 ml of n-hexane was added to the resulting solution for crystallization to obtain 45.6 g of Coupler No. (1). Yield: 72%. m.p.: 106°-107° C.
The silver halide color photographic materials of the present invention can be prepared in a conventional manner using in addition to the pyrazoloazole coupler represented by general formula (I) various conventional additives and elements as described below.
______________________________________Additive/Element/Method Reference______________________________________(1) Color image stabilizing U.S. Pat. No. 4,540,654,agent col. 41, lines 6-47(2) Method of adding Ibid., col. 42, lines 41couplers to col. 43, line 28(3) Color fog preventing Ibid., col. 43, lines 40-51agent(4) Ultraviolet ray absorb- Ibid., col. 43, lines 52 toing agent col. 44, line 6(5) A water-soluble dye as Ibid., col. 44, lines 7-21a filter dye or for thepurpose of preventingirradiation or othervarious purposes(6) A spectral sensitizing Ibid., col. 44, line 22 todye col. 45, line 16(7) A color developing Ibid., col. 45, lines 17-42solution and a colordeveloping agent(8) Other additives to color Ibid., col. 45, lines 43-59developer(9) Bleach (blix) process Ibid., col. 45, line 60 toand a bleaching agent col. 46, line 11(10) A bleaching accelerator Ibid., col. 46, lines 12-17(11) Halogen composition of Ibid., col. 46, lines 23-26silver halide emulsion(12) Grain size distribution Ibid., col. 46, lines 32-36and crystal form of (Grain size distribution issilver halide preferably 0.15 or less in terms of a variation coeffi- cient.)(13) Method for producing Ibid., col. 46, line 37 tosilver halide emulsion col. 47, line 6(14) Additives for grain Ibid., col. 47, lines 7-11formation and/orphysical ripening ofsilver halide emulsion(15) Chemical sensitization Ibid., col. 47, lines 26-34(16) A surface active agent Ibid., col. 47, line 35 to col. 48, line 5(17) A yellow coupler U.S. Pat. No. 4,607,002 2-Equivalent couplers repre- sented by general formula (II) as described in col. 9, line 25 to col. 10, line 64, corresponding 4-equivalent couplers and polymer couplers derived therefrom. Specific examples of the couplers represented by general formula (II), Y-1 to Y-25 are described in col. 11 to col. 15, line 12.(18) A cyan coupler U.S. Pat. No. 4,607,002 2-Equivalent couplers repre- sented by general formulae (III) and/or (IV) as described in col. 15, line 15 to col. 16, line 40, corresponding 4-equivalent couplers and polymer couplers derived therefrom. Specific examples of the couplers represented by general formula (III), C-(I)-1 to -12, are described in col. 16, line 41 to col. 18, line 35, and those of the couplers represented by general formula (IV), C-(II)-1 to10, are described in cols. 17-20. Other useful cyan couplers include those represented by general formula (I) described in col. 1, line 55 to col. 3, line 43 of U.S. Pat. No. 4,327,173. Specific examples thereof, Couplers (1) to (28) are described in col. 3, line 50 to col. 6, line 34. Further, useful cyan couplers include those represented by general formulae [I], [II], [III] or [IV] as described in col. 2, line 1 to col. 4, line 52 of U.S. Pat. No. 4,430,423. Specific examples thereof, Compounds (1) to (17), are described in col. 5, line 10 to col. 7, line 10.U.S. Pat. Nos. 4,540,654, 4,607,002, 4,327,173 and4,430,423 are incorporated herein by reference.______________________________________
As for the support constituting the light-sensitive material of the present invention, there can be used plastic film, plastic laminated paper, baryta paper, synthetic paper, etc. Also, reflective supports can be used which comprise a substrate provided with, for example, a thin metal film or a layer filled with metal powders so that the surface thereof can have a mirror-surface reflectivity or second degree reflectivity.
The silver halide color photographic material of the present invention contains the pyrazoloazole coupler represented by general formula (I) preferably in an amount of from about 0.003 to about 0.3 mol per mol of silver halide in the green-sensitive emulsion layer.
The pyrazoloazole coupler represented by general formula (I) can be added to one or more silver halide emulsion layers or light-insensitive hydrophilic colloid layer(s) adjacent thereto containing gelatin as a major binder component.
The present invention will be explained in greater detail by reference to the following examples, which, however, are not intended to be interpreted as limiting the scope of the present invention in any manner. Unless otherwise indicated, all parts, percents, ratios and the like are by weight.
EXAMPLE 1
Tricresyl phosphate (8.8 mg), 8.6 ml of tris(2-ethylhexyl)phosphate and 25 ml of ethyl acetate were added to 8.8 g of Coupler No. (4) and dissolved under heat, and the resulting solution was added to 100 ml of an aqueous solution containing 10 g of gelatin and 1.0 g of sodium dodecylbenzenesulfonate and rapidly stirred to obtain a finely emulsified dispersion of Coupler No. (4). All of this emulsified dispersion was added to 100 g of a silver chlorobromide emulsion (Br content: 50 mol%, Ag content: 6.5 g), and 10 ml of 2% sodium 2,4-dihydroxy-6-chloro-s-triazine, as a hardener, as added thereto. The resulting solution was coated on a paper support, which had been laminated with polyethylene on both surfaces, the coated silver amount being 200 mg/m 2 . A gelatin layer was superposed on the thus coated emulsion layer to obtain Sample (A).
In the same manner as Sample (A) but differing in that the same molar amount of Coupler Nos. (1), (11), (14) or (25) was used instead of Coupler No. (4) in Sample (A) and that the ratio of the coupler (g)/high boiling point organic solvent (mg) was changed to 1/2, other Samples (B), (C), (D) and (E) were obtained, respectively.
Further, Comparative Samples (F), (G) and (H) were formed, where the following Comparative Couplers (a), (b) and (c) were used, respectively. ##STR10##
These samples were exposed to a red light through a continuous wedge and then developed in accordance with the following process:
______________________________________Processing Step Temperature (°C.) Time______________________________________Development 33 3 min 30 secBleaching Fixation 33 1 min 30 secRinsing 28-35 3 min______________________________________
The composition of each processing solution as used in the above steps was as follows:
Developer:
______________________________________Diethylenetriaminepentaacetic Acid 1.0 gBenzyl Alcohol 15 mlDiethylene Glycol 10 mlNa.sub.2 SO.sub.3 2.0 gKBr 0.5 gHydroxylamine Sulfate 3.0 g4-Amino-3-methyl-N--ethyl-N--[β-(methane- 5.0 gsulfonamido)ethyl]-p-phenylenediamineSulfateNa.sub.2 CO.sub.3 (monohydrate) 30 gFluorescent Whitening Agent (4,4'- 1.0 gdiaminostilbene type)Water to make 1 literpH 10.1______________________________________
Bleaching Fixation Solution:
______________________________________Ammonium Thiosulfate (70 wt % aq. soln.) 150 mlNa.sub.2 SO.sub.3 15 gNH.sub.4 [Fe(EDTA)] 55 gEDTA.2Na 4 gWater to make 1 literpH 6.9______________________________________
The magenta color image thus formed in each sample was sharp and had a high chroma. The photographic characteristics of the color image of each sample was measured. Further, the samples were exposed to light with a Xenon Discoloration Tester (100,000 luxes) for 6 days to observe the degree of the discoloration of each sample. After the discoloration test, the density in the part which had had a density of 1.0 before the test was measured. For the measurement of the density, Macbeth Densitometer RD-514 was used. The results are given in the following Table 1.
TABLE 1__________________________________________________________________________ Light Discoloration Test Photographic Characteristics (initial density: 1.0)Sample Maximum (Xe discoloration tester,No. Coupler Sensitivity* Gradation Density 6 days) Note__________________________________________________________________________A Coupler No. (4) 100 2.82 2.55 0.84 Present InventionB Coupler No. (1) 98 2.79 2.53 0.80 Present InventionC Coupler No. (11) 101 2.83 2.57 0.83 Present InventionD Coupler No. (14) 102 2.82 2.62 0.80 Present InventionE Coupler No. (25) 97 2.71 2.38 0.68 Present InventionF Comparative 85 2.45 2.26 0.68 Comparative Sample Coupler (a)G Comparative 81 2.36 2.21 0.63 Comparative Sample Coupler (b)H Comparative 79 2.10 1.95 0.48 Comparative Sample Coupler (c)__________________________________________________________________________ Note: *This represents the relative value of the reciprocal of the exposure to obtain a density of (fog + 0.5). (The sensitivity of Sample (A) was selected as 100.)
The results shown in Table 1 prove that the couplers having a sulfonamidophenylenesulfonamido group in accordance with the present invention have excellent photographic characteristics. In particular, the results of the light discoloration test prove that the couplers of the present invention having the substituent R 5 in the o-position of the benzenesulfonamido group, which is the nearest position to the skeleton of the coupler, have unexpectedly superior photographic characteristics, especially a higher color image fastness to light. Regarding the pyrazoloazole skeleton of the couplers, the above results show that the 1H-pyrazolo[1,5-b][1,2,4]triazole type couplers (i.e., Coupler Nos (4), (1), (11) and (14) are relatively superior to the 1H-pyrazolo[5,1-c][1,2,4]triazole type coupler, e.g., Coupler No. (25), with respect to photographic characteristics and color image fastness.
EXAMPLE 2
The following first layer (layer closest to the support) to seventh layer (outermost layer) were coated on a paper support having been laminated with polyethylene on both surfaces, as shown in the following Table 2, to obtain Color Photographic Material Samples (I), (J), (K) and (L).
The coating solution for the first layer was prepared as follows:
115 g of the yellow coupler (as shown in Table 2) was dissolved in a mixture solution comprising 100 ml of dibutyl phthalate (DBP) and 200 ml of ethyl acetate, and the resulting solution was emulsified and dispersed in 800 g of a 10% gelatin aqueous solution containing 80 ml of a 1% sodium dodecylbenzenesulfonate aqueous solution. Next, this emulsified dispersion thus prepared was blended with 1,450 g of a blue-sensitive silver chlorobromide emulsion (Br content: 80%, Ag content: 66.7 g) to obtain the coating solution for the first layer. The other coating solutions for the other layers were prepared in the same manner. Sodium 2,4-dichloro-6-hydroxy-s-triazine was used as a hardener in each layer.
The following spectral sensitizer was used in each layer:
Blue-Sensitive Emulsion Layer:
Sodium 3,3'-di(γ-sulfopropyl)selenacyanine (2×10 -4 mol per mol of silver halide)
Green-Sensitive Emulsion Layer:
Sodium 3,3'-di(γ-sulfopropyl)-5,5'-diphenyl-9-ethyloxacarbocyanine (2.5×10 -4 mol per mol of silver halide)
Red-Sensitive Emulsion Layer:
Sodium 3,3'-di(γ-sulfopropyl)-9-methylthiadicarbocyanine (2.5×10 -4 mol per mol of silver halide)
The following dye was used as an anti-irradiation dye in each emulsion layer:
Green-Sensitive Emulsion Layer: ##STR11##
Red-Sensitive Emulsion Layer: ##STR12##
TABLE 2______________________________________Seventh Layer: Protective LayerGelatin 1,500 mg/m.sup.2Sixth Layer: UV Absorbent LayerUV absorbent (*f) 180 mg/m.sup.2UV absorbent solvent (TNP) 80 mg/m.sup.2Gelatin 500 mg/m.sup.2Fifth Layer: Red-Sensitive LayerSilver chlorobromide emulsion Ag 250 mg/m.sup.2(silver bromide: 50 mol %)Cyan coupler (*d/*e) 180 mg/220 mg/m.sup.2UV absorbent (*g) 200 mg/m.sup.2Cyan coupler solvent (TNP/DBP) 200 mg/200 mg/m.sup.2Gelatin 1,000 mg/m.sup.2Fourth Layer: UV Absorbent LayerUV absorbent (*f) 60 mg/m.sup.2UV absorbent solvent (TNP) 200 mg/m.sup.2Gelatin 1,200 mg/m.sup.2Third Layer: Green-Sensitive LayerSilver chlorobromide emulsion Ag 200 mg/m.sup.2(silver bromide: 70 mol %)Magenta coupler (see Table 3 fordescription and amount)Discoloration inhibitor 200 mg/m.sup.2Magenta coupler solvent (seeTable 3 for description and amount)Gelatin 1,300 mg/m.sup.2Second Layer: Color Stain Inhibitory LayerGelatin 1,200 mg/m.sup.2First Layer: Blue-Sensitive LayerSilver chlorobromide emulsion 400 mg/m.sup.2(silver bromide: 80 mol %)Yellow coupler (*a) 690 mg/m.sup.2Color stain inhibitor (*b) 690 mg/m.sup.2Yellow coupler solvent (DBP) 1,000 mg/m.sup.2Gelatin 1,500 mg/m.sup.2SupportPaper support as laminated withpolyethylene on both surfaces______________________________________
In the above Table 2, TNP means trinonyl phosphate; DBP means dibutyl phthalate; TCP means tricresyl phosphate; TOP means tris(2-ethylhexyl)phosphate; and the compounds (*a) through (*g) have the following structural formulae:
(*a) Yellow Coupler: ##STR13##
(*b) Discoloration Inhibitor: ##STR14##
(*c) Discoloration Inhibitor: ##STR15##
(*d) Cyan Coupler: ##STR16##
(*e) Cyan Coupler: ##STR17##
(*f) UV Absorbent: ##STR18##
(*g) UV Absorbent: ##STR19##
TABLE 3______________________________________Sample Magenta Coupler Magenta CouplerNo. (mg/m.sup.2) Solvent (mg/m.sup.2) Note______________________________________I Coupler (1) (370) TCP/TOP Present (370/370) InventionJ Coupler (4) (380) TCP/TOP Present (380/380) InventionK Coupler (11) (450) TCP/TOP Present (450/459) InventionL Comparative TCP/TOP Comparative Coupler (a) (320) (320/320) Sample______________________________________
These samples were exposed to a green light through a continuous wedge and then developed in the same manner as in Example 1.
The photographic characteristics of each of the thus processed samples were measured. Next, the samples were exposed to light with a fluorescent light discoloration tester (15,000 luxes) for 8 weeks, and the magneta color density of each sample in the part which had had an initial density of 1.0 was measured. The results are given in the following Table 4.
TABLE 4__________________________________________________________________________ Light Discoloration Test Photographic (initial density: 1.0) Characteristics (fluorescent lightSample Maximum discoloration tester,No. Coupler Gradation Density 8 weeks) Note__________________________________________________________________________I Coupler (1) 2.57 2.20 0.83 Present InventionJ Coupler (4) 2.62 2.25 0.88 Present InventionK Coupler (11) 2.63 2.26 0.87 Present InventionL Comparative 2.25 1.98 0.69 Comparative Sample Coupler (a)__________________________________________________________________________
The surprisingly superior effects which are obtained when color photographic materials employing magenta couplers in accordance with the present invention are apparent from the above experiments. In particular, the results shown in Table 1 and Table 4 prove that photographic materials incorporating couplers of the present invention are superior in the photographic characteristics and colorability as well as in light fastness of the color images formed therefrom.
While the invention has been described in detail and with reference to specific embodiments thereof, it will be apparent to one skilled in the art that various changes and modifications can be made therein without departing from the spirit and scope thereof.
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Silver halide color photographic materials are described, which comprise at least one silver halide emulsion layer coated on a support and which are characterized by the incorporation of a pyrazoloazole type coupler of the following general formula (I) into the silver halide emulsion layer(s) or the adjacent layer(s) thereto: ##STR1## wherein Za and Zb each may represent ##STR2## R 1 and R 2 each may represent a hydrogen atom or a substituent; X represents a hydrogen atom or a group capable of being removed upon a coupling reaction with an oxidized form of an aromatic primary amine type developing agent; when Za═Zb is a carbon-carbon double bond, this may be a part of the aromatic ring in the formula: with the proviso that at least one of R 1 and R 2 is a group represented by general formulae (II) or (III): ##STR3## wherein R 3 represents a hydrogen atom or a substituted or unsubstituted alkyl group; R 4 represents a hydrogen atom or a substituent; R 5 represents a halogen atom, a substituted or unsubstituted alkoxy, aryloxy, amino, alkylthio or arylthio group; Ar represents an aryl group; Y represents an alkylene group or an arylene group; l' is an integer of 0 or 1; n is an integer of 0 or 1; and m is an integer of 1 to 3; and that when R 1 represents an alkyl group or Y represents an alkylene group, the alkyl or alkylene group is a group of which the carbon atom directly bonded to the pyrazoloazole nucleus is a primary carbon.
The pyrazoloazole type magenta couplers of general formula (I) may form azomethine dyes with improved color reproducibility and high light fastness. The present silver halide color photographic materials containing the coupler of general formula (I) have excellent colorability and excellent light fastness.
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CROSS-REFERENCE TO RELATED APPLICATIONS
This application is the U.S. National Phase of International Patent Application No. PCT/EP2013/061514 filed on 4 Jun. 2013, which claims benefit of European Patent Application No. 12171024.8 filed on 6 Jun. 2012, the contents of which are incorporated herein by reference in their entireties.
TECHNICAL FIELD
The present invention relates to a bioreactor according to the preamble of independent claim 1 and to a mounting rack for mounting a plurality of bioreactors of this kind. Such bioreactors include a scaffold chamber, a first tube, a second tube and a first valve with a scaffold adapter, a tube adapter and a medium adapter, wherein the tube adapter of the first valve is connected to the first tube and the scaffold adapter of the first valve is connected to the scaffold chamber; the first valve is arrangeable in an operation position in which the scaffold adapter of the first valve is in fluid connection with the tube adapter of the first valve and the medium adapter of the first valve is fluid sealed to the tube adapter of the first valve; and the first valve is arrangeable in a medium change position in which the medium adapter of the first valve is in fluid connection with the tube adapter of the first valve and the scaffold adapter of the first valve is fluid sealed to the tube adapter of the first valve, can be used for preferably three-dimensional cell culturing, particularly tissue or tissue-like cell culturing such as bone tissue cell culturing.
BACKGROUND ART
In recent years, scientific evidence proving the inadequacy of monolayer cell cultures have triggered the development of techniques that allow culturing of cells in a three-dimensional (3D) environment. These techniques include the use of suitable porous biomaterials, i.e. scaffolds, that can be seeded with cells but can also include cell clusters, tissue or tissue like structures, biopsies and similar.
As a consequence, tools have been made available to respond to specific needs inherent to these techniques. Among these tools, bioreactors provide a controlled chemo-physical environment suitable for the culturing of cells in 3D. In particular, perfusion bioreactors have proven to be effective in overcoming typical limitations of static cultures. Such limitations include lack of a uniform cell seeding through the scaffold, limited mass transport, i.e. nutrient delivery and waste removal, particularly in a central part of the scaffold.
For example, in the article “Uniform tissues engineered by seeding and culturing cells in 3D scaffolds under perfusion at defined oxygen tension” of Wendt D. et al. from the Departments of Surgery and of Research of the University Hospital Basel, Switzerland, published in Biorheology, 43, 481-488, 2006, a bioreactor for 3D cell culturing is shown. This bioreactor comprises a first tube and a second tube each being connected to a scaffold chamber via a three way valve. The first tube is made of Teflon and provided with a cell suspension. The second tube comprises a portion made of Teflon and a flexible portion. The first tube and the flexible portion of the second tube are connected to a pump allowing to circulate the cell suspension through the scaffold chamber in which a porous scaffold is arranged. The three way valves are additionally connected to the pump and a medium storage. The valves are further arranged to be in medium change position in which the first and second tubes are in fluid connection with the medium storage and an operation position in which the first and second tubes are connected to the scaffold chamber.
However, such bioreactors are usually comparably cumbersome to set up and to operate such that mistakes impairing cell culturing can occur. For example, when setting up such a bioreactor numerous components of various vendors have to be manually assembled wherein these components frequently do not properly fit together. Further, such bioreactors are typically made of comparably expensive recyclable components that are used for multiple cycles which bears the risk of accumulation of undesired substances. Still further, the three way valves used within such bioreactors usually have to be operated by rotating an actuator in various proper rotational positions. Operation of these three way valves often is confusing and can easily induce mistakes when being handled particularly by inexperienced users.
Therefore, there is a need for a bioreactor and system allowing for a convenient operation and handling within cell culturing.
SUMMARY
According to the invention this need is settled by a bioreactor as it is defined by the features of independent claim 1 , and by a rack as it is defined herein below. Preferred embodiments are subject of the dependent claims.
In particular, the gist of the invention is: A bioreactor for preferably three-dimensional cell culturing includes a scaffold chamber, a first tube, a second tube and a first valve with a scaffold adapter, a tube adapter and a medium adapter. The tube adapter of the first valve is connected to the first tube and the scaffold adapter of the first valve is connected to the scaffold chamber. The first valve is arrangeable in an operation position in which the scaffold adapter of the first valve is in fluid connection with the tube adapter of the first valve and the medium adapter of the first valve is fluid sealed to the tube adapter of the first valve. The first valve further is arrangeable in a medium change position in which the medium adapter of the first valve is in fluid connection with the tube adapter of the first valve and the scaffold adapter of the first valve is fluid sealed to the tube adapter of the first valve. Thereby, the first valve has a housing with a longitudinal female portion ending in an opening and a longitudinal actuator being arranged through the opening of the female portion of the housing such that the actuator is arranged partially inside the housing and partially outside the housing, wherein the actuator of the first valve is axially moveable relative to the housing of the first valve between a first position in which the first valve is in the operation position and a second position in which the first valve is in the medium change position.
The bioreactor can particularly be a perfusion bioreactor suitable for bone or cartilage tissue culturing. The term “adapter” as used in the context of the invention relates to any possible connection of two units or of two portions of one single unit. In particular, an adapter can be a connector of a first unit allowing for mounting and dismounting a corresponding connector of a second unit. Or, an adapter can also be the connecting portion of a single unit such as a tubular portion connecting two portions of one unit or a passage connecting two portions of one unit. Particularly, the scaffold adapter of the first valve can be fixedly mounted to the scaffold chamber, wherein the scaffold adapter and at least a part of the scaffold chamber can be made as one piece. The first and the second tube can be made of silicone such that they are slightly permeable, particularly for oxygen and/or for carbon dioxide. The first valve can be made of polycarbonate and/or acrylonitrile butadiene styrene (ABS), e.g. such that it is not autoclavable in order to avoid reuse, if desired. The actuator can be essentially circular cylindrical or essentially polygonal cylindrical. The term “axially” with regard to the actuator relates to a direction along a longitudinal axis of the actuator.
By providing the actuator in the first valve which is applied by axial movements, operation of the bioreactor can be comparably simple and safe. In particular, such arrangement allows for a comparably easy identification of the position of the first valve, i.e., e.g., if the valve is in the medium change position or in the operation position. Furthermore, it also allows for exactly adjusting the position of the actuator such that also positions in between the medium change position and the operation position can be conveniently identified and applied, if necessary.
Preferably, the bioreactor further includes a second valve with a scaffold adapter, a tube adapter and a medium adapter, wherein the tube adapter of the second valve is connected to the second tube and the scaffold adapter of the second valve is connected to the scaffold chamber; the second valve is arrangeable in an operation position in which the scaffold adapter of the second valve is in fluid connection with the tube adapter of the second valve and the medium adapter of the second valve is fluid sealed to the tube adapter of the second valve; the second valve is arrangeable in a medium change position in which the medium adapter of the second valve is in fluid connection with the tube adapter of the second valve and the scaffold adapter of the second valve is fluid sealed to the tube adapter of the second valve; the second valve has a housing with a longitudinal female portion ending in an opening and a longitudinal actuator being arranged through the opening of the female portion of the housing such that the actuator is arranged partially inside the housing and partially outside the housing; and the actuator of the second valve is axially moveable relative to the housing of the second valve between a first position in which the second valve is in the operation position and a second position in which the second valve is in the medium change position.
As the first valve mentioned above, also the second valve can be made of polycarbonate and/or ABS and its actuator can be essentially circular cylindrical or essentially polygonal cylindrical. Providing the second valve within the bioreactor allows for a particular efficient operation. Thereby, the second valve including the actuator being applicable by axial movements in correspondence with the first valve allows for operating the bioreactor in a comparably simple and safe manner. In particular, such arrangement also allows for a comparably easy identification of the position of the second valve, i.e., e.g., if the valve is in the medium change position or in the operation position. Furthermore, it also allows for exactly adjusting the position of the actuator such that also positions in between the medium change position and the operation position can be conveniently identified and applied, if necessary.
Thereby, each of the first valve and the second valve preferably is arranged such that the tube adapter is essentially opposed to the scaffold adapter wherein the actuator has a through bore connecting the tube adaptor and the scaffold adaptor in the operation position of the respective valve. In this context, the term “respective valve” with regard to the actuator relates to the valve of which the actuator forms a part. For example, the first valve is the respective valve of the actuator of the first valve. As mentioned above, in the operation position of the respective valve the actuator is in the first position. The through bore can have a circular profile and can be a straight through bore. Such an arrangement of the valves can allow for a comparably easy implementation of the bioreactor.
The actuator of each of the first valve and the second valve preferably has an inner duct connecting the medium adaptor and the tube adaptor in the medium change position of the respective valve. As mentioned above, in the medium change position of the respective valve the actuator is in the second position. Thereby, the inner duct of the actuator of each of the first valve and the second valve preferably has an essentially axial portion and an essentially radial portion. Such an arrangement of the valves can allow for a comparably easy and precisely operatable implementation of the bioreactor.
Preferably, the actuator of each of the first valve and the second valve has a flange portion. The flange portion can particularly be arranged in a distal end region of the corresponding actuator. It can also radially project above the rest of the actuator. Such a flange portion allows for an efficient operation of the valves. For example, a user of the bioreactor can conveniently manually move the actuators of the first and second valves via the respective flange portion.
Preferably, the housing of each of the first valve and the second valve has a guidance interacting with the actuator such that the actuator is solely axially moveable within a predefined range. Like this, the risk of faulty operation of the valves can be reduced. Also the valves can be provided in a comparable stable arrangement and a stroke of the actuator can be defined. Thereby, the guidance preferably comprises a groove and the actuator an arm wherein the arm of the actuator engages the groove of the housing of the respective valve. Beyond others, such a groove allows for example determining the stroke of the actuator via its length. In order to provide sufficient stability, the housing can particularly comprise two grooves and the actuator to corresponding arms.
Preferably, the scaffold chamber includes a casing wherein the casing of the scaffold chamber has a first part with a first bayonet mount structure and a second part with a second bayonet mount structure, wherein the casing is arrangeable in an open position in which the first part and the second part are disassemblable and in a closed position in which the first bayonet mount structure of the first part and the second bayonet mount structure of the second part are engaging. Such a casing which can be opened allows for conveniently accessing a scaffold in the scaffold chamber.
Thereby, the scaffold chamber preferably includes a scaffold holder wherein the scaffold holder is removable from the casing in the open position of the casing and the scaffold holder is enclosable inside the casing in the closed position of the casing. The scaffold holder can have an essentially cylindrical shape with an essentially cylindrical opening axially extending through the scaffold holder. The opening can be narrowed into the direction of one of the axial ends of the scaffold holder. This can, e.g., be provided by a bottom or top plate having a through bore of a smaller dimension than the opening of the scaffold holder. In particular, the scaffold holder can be essentially cup shaped with a through bore at its closed end for allowing accessing a scaffold being arranged inside the scaffold holder. Thereby, the scaffold can be positioned inside the scaffold holder by arranging it in the opening of the scaffold holder. At its outer surface, the scaffold holder can be provided with one or more recesses circumferentially extending around the scaffold holder. Each of the one or more recesses can be arranged for accommodating a sealing ring such that the scaffold holder can be arranged in the casing in a sealed manner. The outer surface of the scaffold holder can further be provided with gripping surfaces which allow an efficient handling of the scaffold holder. The scaffold holder allows for holding the scaffold in a preferred manner such that a convenient and efficient handling is possible as well as an efficient operation of the bioreactor.
The scaffold chamber further preferably includes blocking adapters being arrangeable in the scaffold holder to embed the scaffold. Advantageously there are two blocking adapter which can be made of silicone. The blocking adapters can be essentially ring shaped wherein the interior opening can be provided with a step for accommodating the scaffold. The blocking adapters can particularly be shaped to be tightly arranged in a scaffold holder as mentioned above. One of the axial end sides of each of the blocking adapters can be colored for allowing convenient correct insertion into the scaffold holder. Blocking adapters as described herein allow for a safe and soft fixation of the scaffold in a predefined position within the bioreactor.
Preferably, the medium adapter of the actuator of each of the first valve and the second valve comprises a male locking thread. The male thread can be a luer-lock thread and particularly a double luer-lock thread. Such a male locking thread allows for conveniently and safely mounting a tubular medium structure to the bioreactor.
Another aspect of the present disclosure relates to a rack for mounting a plurality of bioreactors as described above. The rack includes a frame with a plurality of mounting structures wherein each mounting structure comprises a tube holder arranged to hold a first tube of one of the plurality of bioreactors and a second tube of the one of the plurality of bioreactors, and a guiding arch arranged to turn the first tube or the second tube of the one of the plurality of bioreactors. The tube holder of each mounting structure can be arranged to hold the first tube of one of the plurality of bioreactors at an end region opposite to a scaffold chamber of the one of the plurality of bioreactors and the second tube of the one of the plurality of bioreactors at an end region opposite to the scaffold chamber of the one of the plurality of bioreactors. The guiding arch allows to arrange the first and second tubes such that their end regions opposite to the scaffold chamber are heading into the direction of the corresponding tube holder. In particular, the guiding arch can be arranged to turn the first tube or the second tube about 180° such that it is arranged to U-turn the first tube or the second tube.
The rack allows for correct positioning of the bioreactors and particularly of the flexible parts thereof such that their proper functioning can be achieved. It can provide stability during operation and in an incubator for cell culturing. It also can provide comparably good visibility and comparably easy access all bioreactors mounted in the rack. It further allows for an efficient organisation of the bioreactors and particularly of tubes going from a pump to the single bioreactors. It also makes a compact and safe arrangement and comparable easy transportation possible. In summary, with such a rack a particularly comfortable and efficient correct handling of plural bioreactors requiring comparably little space can be provided.
Preferably, each of the tube holders of the plurality of mounting structures includes a plate with two clamping portions arranged to clamp the first tube and the second tube of one of the plurality of bioreactors. Such clamping portions allow for a comparably simple implementation of the tube holders. For example, the tube holders can be shaped as two essentially rectangular plates with a U-shaped recess at each longitudinal end as the clamping portions.
Preferably, the rack includes a base wherein the frame is turnably mounted on the base such that the frame is turnable about an essentially vertical axis when the rack is positioned on the base. Such a turnable rack allows for conveniently accessing each of the bioreactors mounted in the rack.
Preferably, the rack includes an operating handle which can allow for a convenient and efficient handling of the rack. Preferably, each of the plurality of mounting structures or a group mounting structures of the plurality of mounting structures is arranged as a removable unit. Such removable units can further improve handling of the bioreactors within the rack.
These and other aspects of the invention will be apparent from and elucidated with reference to the embodiment(s) described hereinafter.
BRIEF DESCRIPTION OF THE DRAWINGS
The bioreactor and the rack according to the invention are described in more detail herein below by way of exemplary embodiments and with reference to the attached drawings, in which:
FIG. 1 shows a side view of an embodiment of a bioreactor according to the invention;
FIG. 2 shows perspective view of the bioreactor of FIG. 1 ;
FIG. 3 shows an exploded side view of the valves, the scaffold chamber and parts inside the scaffold chamber of the bioreactor of FIG. 1 ;
FIG. 4 shows an exploded perspective view of the valves, the scaffold chamber and the parts inside the scaffold chamber of the bioreactor of FIG. 1 ;
FIG. 5 shows an exploded cross-sectional side view of the valves in a operation position, the scaffold chamber and the parts inside the scaffold chamber of the bioreactor of FIG. 1 ;
FIG. 6 shows an exploded cross-sectional side view of the valves in a medium change position, the scaffold chamber and the parts inside the scaffold chamber of the bioreactor of FIG. 1 ; and
FIG. 7 shows a perspective view of an embodiment of a rack intended for mounting and handling a plurality of bioreactors according to the invention.
DETAILED DESCRIPTION
In the following description certain terms are used for reasons of convenience and are not to be interpreted as limiting. The terms “right”, “left”, “horizontal”, “vertical”, “up”, “down”, “under” and “above” refer to directions in the figures. The terminology includes the explicitly mentioned terms as well as their derivations and terms with a similar meaning. Furthermore, if, in order to clarify the drawings, a figure contains reference signs which are not explained in the directly associated part of the description, then it is referred to previous description sections.
In FIG. 1 and FIG. 2 an embodiment of a bioreactor 1 according to the invention includes a first tube 2 , a second tube 3 , a scaffold chamber 4 , a first valve 5 and a second valve 6 is shown. The first tube 2 which is shown in FIG. 1 in an essentially vertical position is made of silicone being gas permeable particular for oxygen and carbon dioxide. On the top longitudinal or axial end of the first tube 2 a 0.2 μm first filter 21 is mounted by means of a luer-lock barbed connector for preventing exchange of microorganisms and particles into and out of the first tube 2 . The first filter 21 has a first pump adapter 22 for connecting a pump. On the bottom longitudinal or axial end the first tube 2 is connected to a tube adapter 511 of a housing 51 of the first valve 5 .
The first valve 5 includes an actuator 52 with an essentially cylindrical main body which in FIG. 1 is shown horizontally extending into the housing 51 . At the one longitudinal end of the actuator 52 being arranged outside the housing, i.e. on the right hand end of the actuator 52 in FIG. 1 , the actuator 52 has a medium adapter 521 . Between the medium adapter 521 and the housing 51 , the actuator 52 further comprises a flange portion 523 to which two arms 522 are arranged extending parallel to the main body of the actuator 52 . As can be best seen in FIG. 2 the flange portion 523 of the actuator 52 has an essentially rectangular shape wherein it is horizontally arranged and wherein the arms 522 extend from the longitudinal ends thereof. The arms 522 of the actuator 52 extend into respective guidances 513 being arranged as horizontal slits in the housing 51 . The arms 522 and guidances 513 allow for a stable movement of the actuator 52 , for preventing a rotational movement of the actuator 52 around its longitudinal axis and for determining a stroke of the actuator via a length of the guidances 513 .
Opposite to the tube adapter 511 , i.e. in a downward direction, the housing 51 passes over into a scaffold adapter 512 being unitary built with an upper first part 41 of a casing of the scaffold chamber 4 . The first part 41 of the casing of the scaffold chamber 4 includes a bayonet mount structure 411 which engages into a corresponding bayonet mount structure 421 of a second part 42 of the casing of the scaffold chamber 4 . Thereby, the casing of the scaffold chamber 4 is in a closed position and the bayonet mount structures 411 , 421 together provide a safety closing mechanism of the scaffold chamber 4 . The second part 42 is unitary built with a scaffold adapter 612 of a housing 61 of the second valve 6 . The second valve 6 is identical to the first valve 5 wherein compared to the first valve 5 it is arranged upside down such that the scaffold adaptor 612 of its housing 61 extends upwardly and a tube adaptor 611 of its housing 61 extends downwardly. Guidances 613 of the housing 61 and an actuator 62 with a medium adapter 621 , a flange portion 623 and two arms 622 are arranged corresponding to the respective parts of the first valve 5 . The bayonet mount structure 411 of the first part 41 and the bayonet mount structure 421 of the second part 42 are arranged such that the actuator 52 of the first valve 5 and the actuator 62 of the second valve 6 extend in parallel when the bayonet mount structure 411 of the first part 41 engages the bayonet mount structure 421 of the second part 42 .
The tube adapter 611 of the housing 61 of the second valve 6 is connected to a second wide portion 33 of the second tube 3 which in FIG. 1 extends vertically. The second wide portion 33 of the second tube 3 is glued to a narrow portion 32 of the second tube 3 which describes a U turn. The gluing between the second wide portion 33 of the second tube 3 and the narrow portion 32 of the second tube 3 generates a conical shape that improves the fluidodynamic of the system and reduces cell settling on essentially horizontal surfaces. Also, the reduced diameter of the narrow portion 32 of the tube 3 is intended to increase flow speed in use such that cell settling in an essentially horizontal section of the second tube 3 can be reduced or even prevented. The end of the narrow portion 32 of the second tube 3 is again glued to a first wide portion 31 of the second tube 3 which in FIG. 1 extends vertically. Similar as mentioned before, the gluing between the end of the narrow portion 32 of the second tube 3 and the first wide portion 31 of the second tube 3 generates a conical shape that improves the fluidodynamic of the system and reduces cell settling on essentially horizontal surfaces. As the first tube 2 , the second tube 3 is also made of silicone being gas permeable particular for oxygen and carbon dioxide.
On the top longitudinal or axial end of the first wide portion 31 of the second tube 3 a 0.2 μm second filter 34 is mounted by means of a luer-lock barbed connector for preventing exchange of microorganisms and particles into and out of the second tube 3 . The second filter 34 has a second pump adapter 35 for connecting a pump. The first pump adapter 22 of the first filter 21 and the second pump adapter 35 of the second filter 34 differ in shape in order to make sure that the correct side of the pump is connected to corresponding first tube 2 or second tube 3 .
In FIG. 3 and FIG. 4 an exploded view of the scaffold chamber 4 of the bioreactor 1 is shown. In fact, FIG. 3 and FIG. 4 show the scaffold chamber 4 in a disassembled or open position in which the bayonet mount structure 411 of the first part 41 of the casing is disengaged from the bayonet mount structure 421 of the second part 42 of the casing. Thereby, a scaffold holder 7 and blocking adapters 8 are unloaded from the casing of the scaffold chamber 4 . The blocking adapters 8 which both are made of silicone comprise a top first blocking adapter 81 and a bottom second blocking adapter 82 which both are made of silicone. In order that the blocking adapters 8 can be conveniently mounted in a correct manner, the first blocking adapter 81 is colored on its top side and the second blocking adapter is colored on its bottom side.
The scaffold holder 7 is essentially cylindrical and cup shaped. At its outer surface, the scaffold holder is provided with planar gripping surfaces 71 allowing for conveniently handling the scaffold holder 7 . Near its top and bottom end recesses 72 are circumferentially arranged about the outer surface of the scaffold holder 7 . In each of the recesses 72 a sealing O-ring 73 is arranged allowing for sealing a space between the scaffold holder 7 and the scaffold chamber 4 when the scaffold holder 7 is arranged inside the scaffold chamber 4 such that the scaffold holder 7 is held in the scaffold chamber 4 by friction forces between the sealing rings 73 and the scaffold chamber 4 .
In FIG. 5 cross-sections of the first valve 5 , the scaffold chamber 4 , the blocking adapters 8 , the scaffold holder 7 and the second valve 6 are shown. The housing 51 of the first valve 5 has an essentially cylindrical horizontal through hole as a female portion 514 . The actuator 52 is extending through the female portion 514 of the housing 51 wherein on one side, the right hand side, the flange portion 523 of the actuator 52 is arranged outside the housing 51 and on the other side, the left hand side, the actuator 52 has a circumferential recess outside the housing 51 in which a stop cramp 527 is snapped in. By means of this stop cramp 527 it can be prevented that the actuator 52 is removed out of the female portion 514 of the housing 52 into the direction of the medium adapter 521 , i.e. to the right. The actuator 52 has vertical though bore 524 which in the operation position shown in FIG. 5 connects the tube adapter 511 with the scaffold adapter 512 . The actuator 52 further has a duct 525 extending from the medium adapter 521 in an axial or horizontal direction to a certain extent and then turning by 90° in an upward vertical direction. In the operation position of the first valve shown in FIG. 5 , the medium adapter 521 is neither connected to the tube adapter 511 nor to the scaffold adapter 512 . Adjacent to the through bore 524 and the vertical opening of the duct 525 , the actuator 52 has circumferential recesses with sealing O-rings 526 . These sealing rings 526 allow for preventing any substance or contaminating agent entering or exiting out of the female portion 514 of the housing 51 or biasing the through bore 524 with the duct 525 .
The first blocking adapter 81 and the second blocking adapter 82 each have a vertical through hole 812 , 822 and a scaffold receiver 811 , 821 . Even though other shapes are also possible, both blocking adapters 8 are identically formed wherein they are arranged upside down in relation to each other such that the scaffold receiver 811 of the first blocking adapter 81 is directed to and adjacent to the scaffold receiver 821 of the second blocking adapter 82 . Thereby, the scaffold receiver 811 of the first blocking adapter 81 and the scaffold receiver 821 of the second blocking adapter 82 together form a chamber for accommodating a scaffold in a safe and fixed position. The blocking adapters 81 , 82 allow a tight sealing between the scaffold and the blocking adapters 81 , 82 themselves, so that medium can effectively run through the porous scaffold instead of tangentially. The blocking adapters 8 are dimensioned to be tightly arranged inside the cup-shaped scaffold holder 7 such that they are held by friction between the blocking adapters 8 and inner surfaces of the scaffold holder 7 . The bottom side of the scaffold holder 7 has a through hole allowing medium passing top down through the scaffold and the through holes 812 , 822 of the blocking adapters 8 to exit the scaffold holder 7 .
As described above in connection with FIG. 1 and FIG. 2 , the second valve 6 is identical to the first valve 5 wherein compared to the first valve 5 it is arranged upside down. In particular, as can be seen in FIG. 5 , its housing also comprises a female portion 614 and its actuator 62 also comprises a circumferential recess with a stop cramp 627 , a vertical through bore 624 , a duct 625 having a horizontal and a vertical section as well as circumferential recesses with sealing O-rings 626 .
FIG. 6 shows the same component as FIG. 5 wherein contrary to the operation position of FIG. 5 the first valve 5 and the second valve 6 are shown in FIG. 6 in a medium change position. In this position, the actuators 52 , 62 are horizontally moved into the direction of the stop cramps 527 , 627 , i.e. to the left, until the flange portions 523 , 623 contact the respective housing 51 , 62 . Thereby, the ducts 525 , 625 connect the tube adapters 511 , 611 with the medium adapters 521 , 621 of the respective valve 5 , 6 . Like this, medium can be added to or removed from the internal of the bioreactor 1 via the medium adapters 521 , 621 . For example, the medium adapter 521 , 621 can be connected to a syringe which provides medium into the bioreactor 1 .
In use of the bioreactor 1 , once the scaffold is loaded into the blocking adapters 8 inside the scaffold holder 7 and inside the closed scaffold chamber 4 , a cell suspension as medium can be provided into the bioreactor through the medium adapter 521 , 621 of one of the valves 5 , 6 . Then the medium is moved in alternated directions by means of a syringe pump (or peristaltic) connected to the first filter 21 and second filter 34 for the time the culture requires while the valves 5 , 6 are in the operation position. During this movement, the medium perfuses the sample and cell eventually attach to it. When medium needs to be changed, the valves 5 , 6 can be moved to the medium change position by sliding the actuators 52 , 62 , exhaust medium is removed, fresh medium is injected, the valves 5 , 6 are moved to operation position and the culturing continues.
In FIG. 7 an embodiment of a rack 9 is shown which is intended for mounting and handling a plurality of bioreactors 1 as described above in connection with FIGS. 1 to 6 . The rack 9 includes a frame having an essentially circle-disk-shaped frame base 97 with five evenly arranged, circle-segment-shaped recesses 971 . The frame base 97 is turnably or rotatably mounted on top of a circle-disk-shaped rack base 93 as base of the rack 9 . A linear handle rod 95 is centrally connected to the frame base 97 in a rotatably fixed manner. The handle rod 95 vertically extends from the frame base 97 in an upward direction when the rack base 93 is arranged on a horizontal surface such as on a table or the like. At its top end the handle rod 95 passes over into a handle grip 94 wherein the handle rod 95 and the handle grip 94 together form an operating handle of the rack 9 . Near the handle grip 94 a circular disk 96 having plural tube slits 961 at its circumferential edge is mounted to the handle rod 95 wherein the handle rod 95 centrally traverses the circular disk 96 .
In each of the recesses 971 of the frame base 97 a circle-disk-shaped unit base 912 of a removable unit 91 is arranged. From a top surface of the unit base 912 of each removable unit 91 a unit rod 911 vertically extends in an upward direction passing over into a crosspiece 913 . Thereby, the unit rod 911 is connected to the unit base 912 at an eccentric position thereof. Each of the crosspieces 913 is slightly bent around the handle rod 95 as a central axis of the rack 9 wherein at its horizontal edges clamping slits 9131 are arranged.
In each of the clamping slits 9131 of the crosspieces 913 of the units 91 a connection rod 922 of a mounting structure 92 is clamped such that the connection rods 92 extend in an essentially vertical direction. At its bottom end each of the connection rods 922 passes over into a guiding arc 923 having a peripheral groove 9231 . On the top end of each of the connection rods 922 an essentially horizontal and essentially rectangular plate 921 is mounted as tube holder. Each of the plates 921 has a first clamping recess 9211 as clamping portion and a second clamping recess 9212 as clamping portion at each of its shorter side edges.
In use of the rack 9 , bioreactors 1 as described with regard to FIGS. 1 to 6 can be arranged in the rack 9 as follows: The first tube 2 of the bioreactor 1 is clamped into the first clamping recess 9211 of the plate 921 of one the mounting structures 92 . The narrow portion 32 of the second tube 3 of the bioreactor 1 is arranged into the groove 9231 of the guiding arc 923 of said mounting structure 92 and thereby turned by about 180°. The first wider portion 31 of the second tube 3 of the bioreactor is then clamped into the second clamping recess 9212 of the plate 921 of said mounting structure 92 .
The connection rod 922 of the mounting structure 92 is then clamped into one of the slits 9131 of the crosspiece 913 of one of the removable units 91 . Optionally, a further mounting structure 92 with a further bioreactor 1 can be clamped into the other one of the slits 9131 of the crosspiece 913 of said removable unit 91 . The unit base 912 of the removable unit 91 is then positioned into one of the recesses 971 of the frame base 97 of the rack 9 . External tubes such as, e.g., air delivery tubes being connected to the bioreactor 1 can be clamped into the tube slits 961 of the disk 96 of the rack 9 .
The rack 9 allows for safely holding one to ten bioreactors 1 in a preferred upright position. Thereby, the valves 5 , 6 of all bioreactors 1 mounted to the rack 9 are conveniently accessible from the outside of the rack 9 . Further, each of the bioreactors 1 in the rack 9 can easily be selected and accessed by turning the frame base 97 with respect to the rack base 93 , e.g. via the handle grip 94 , up to a desired position. In order to avoid for example wrapping up air tubes, rotation of the frame base 97 can be limited, e.g., to less than 360°. By means of the removable units 91 the bioreactors 1 can conveniently be mounted to and dismounted from the rack 9 wherein it can be assured that the bioreactors 1 are in a correct position and a wrong insertion can be prevented. In summary, the rack 9 allows for a convenient and flexible handling of plural bioreactors 1 in an organized and structured manner.
While the invention has been illustrated and described in detail in the drawings and foregoing description, such illustration and description are to be considered illustrative or exemplary and not restrictive. It will be understood that changes and modifications may be made by those of ordinary skill within the scope and spirit of the following claims. In particular, the present invention covers further embodiments with any combination of features from different embodiments described above and below.
The invention also covers all further features shown in the FIGS. 1-7 individually although they may not have been described in the afore or following description. Also, single alternatives of the embodiments described in the figures and the description and single alternatives of features thereof can be disclaimed from the subject matter of the invention or from disclosed subject matter. The disclosure includes subject matter consisting of the features defined in the claims or the exemplary embodiments as well as subject matter including the features.
Furthermore, in the claims the word “comprising” does not exclude other elements or steps, and the indefinite article “a” or “an” does not exclude a plurality. A single unit or step may fulfill the functions of several features recited in the claims. The mere fact that certain measures are recited in mutually different dependent claims does not indicate that a combination of these measures cannot be used to advantage. The terms “essentially”, “about”, “approximately” and the like in connection with an attribute or a value particularly also define exactly the attribute or exactly the value, respectively. The term “about” in the context of a given numerate value or range refers to a value or range that is, e.g., within 20%, within 10%, within 5%, or within 2% of the given value or range. Any reference signs in the claims should not be construed as limiting the scope.
The present disclosure comprises the following further embodiments of racks intended for mounting and handling a plurality of bioreactors according to the invention.
Embodiment 1 is a rack for mounting a plurality of bioreactors according to the invention, including
a frame with a plurality of mounting structures wherein each mounting structure includes a tube holder arranged to hold a first tube of one of the plurality of bioreactors and a second tube of the one of the plurality of bioreactors, and
a guiding arch arranged to turn the first tube or the second tube of the one of the plurality of bioreactors.
Embodiment 2 is a rack according to embodiment 1, wherein each of the tube holders of the plurality of mounting structures includes a plate with two clamping portions arranged to clamp the first tube and the second tube of one of the plurality of bioreactors.
Embodiment 3 is a rack according to embodiment 1 or 2, including a base wherein the frame is turnably mounted on the base such that the frame is turnable about an essentially vertical axis when the rack is positioned on the base.
Embodiment 4 is a rack according to any one of embodiments 1 to 3, including an operating handle.
Embodiment 5 is a rack according to any one of embodiments 1 to 4, wherein each of the plurality of mounting structures or a group mounting structures of the plurality of mounting structures is arranged as a removable unit.
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A bioreactor for preferably three-dimensional cell culturing comprises a scaffold chamber, a first tube, a second tube and a first valve with a scaffold adapter, a tube adapter and a medium adapter. The first valve has a housing with a longitudinal female portion ending in an opening and a longitudinal actuator being arranged through the opening of the female portion of the housing such that the actuator is arranged partially inside the housing and partially outside the housing, wherein the actuator of the first valve is axially moveable relative to the housing of the first valve between a first position in which the first valve is in the operation position and a second position in which the first valve is in the medium change position. By providing the actuators in the first valve which is applied by axial movements, operation of the bioreactor can be comparably simple and safe.
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CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] This application claims the benefit of U.S. provisional application No. 61/902,087 filed on Nov. 8, 2013, which is hereby incorporated by reference in its entirety.
FIELD OF THE INVENTION
[0002] The present disclosure relates to methods and compositions for treating systemic infections of crop species.
BACKGROUND OF THE INVENTION
[0003] Huanglongbing (HLB), commonly known as citrus “greening” disease, is one of the top three most damaging diseases of citrus in Africa, America and Asia. HLB is naturally transmitted by psyllids, and experimentally by grafting or dodder ( Cuscuta spp.). The disease was shown to be graft-transmissible in 1956 (Lin, 1956) and therefore it was thought to be caused by a putative virus. However, in 1970, sieve tube restricted bacteria were discovered in affected trees. First thought to be mycoplasma-like (Laflèche and Bové, 1970), they were soon recognized as walled bacteria (Saglio et al., 1971; Bové and Saglio, 1974) of the Gram negative type (Gamier et al., 1984) and finally shown to be species of alpha proteobacteria (Jagoueix, et al. 1994). Two species were recognized: Candidatus Liberibacter asiaticus ( Las ) for the disease in Asia and Ca. L. africanus ( Laf ) for the disease in Africa.
[0004] In 2004, when HLB was seen for the first time in the Americas and more precisely in São Paulo State, Brazil, two liberibacter species were identified: (i) a new species, Ca. L. americanus ( Lam ), infecting most of the affected trees, and (ii) the known Asian liberibacter, Las, present in a minority of trees (Teixeira et al., 2005). All three citrus liberibacters are uncultured and phloem-limited. That is, these bacteria live in plants exclusively within living plant phloem cells. Las is the most widely distributed by far. Today, HLB has been identified in states ranging from Florida, Louisiana, and California.
[0005] With no effective treatment options available in the market, there is a growing demand for new technologies to combat its spread.
SUMMARY OF THE INVENTION
[0006] The disclosure teaches compositions useful for protecting or treating plants against intracellular bacterial attack and infection and particularly for treatment of existing plants infected with systemic Liberibacter species, comprising at least one aromatic aldehyde species, in concentrations sufficient for eliciting plant defense responses. This disclosure also teaches use of at least one polar solvent that is useful for delivery and penetration of the aldehyde into plant cells.
[0007] In some embodiments, the present invention teaches compositions and methods useful for curing and protecting crops, including tree crops, against intracellular bacterial disease, including disease caused by bacterial species of the genus Liberibacter, comprising at least one aromatic aldehyde species.
[0008] In some embodiments, the application or injection of the composition of the present invention results in a reduction in the number of bacteria. In other embodiments, the application or injection of the composition results in a reduction in the number of bacteria, the incidence of disease, or the incidence of disease symptoms. Thus for example in some embodiments, application of compositions of the present invention improves the growth or fruit yield of Liberibacter infected plants.
[0009] In some embodiments, the curing and protecting of plants, is measured against an infected control plant that has not been treated with the compositions. In other embodiments, the reduction in bacteria, incidence of disease, or incidence of disease symptoms are measured against an infected control crop that has not been treated with the compositions.
[0010] In some embodiments, the application or injection of the composition results in a partial clearance of the bacteria from the plant, as compared to an untreated infected plant. In further embodiments, the partial clearance may be 5%, 10%, 15%, 20%, 25%, 30%, 35%, 40%, 45%, 50%, 60%, 65%, 70%, 75%, 80%, 85%, 90%, 95%, 96%, 97%, 98%, or 99%.
[0011] In other embodiments, the application or injection of the composition results in the plant being cured.
[0012] In some embodiments, the aromatic aldehyde species of the present invention are selected from the group consisting of cinnamaldehyde, coniferyl aldehyde, carvacrol, and geriniol. In a particular embodiment, the composition comprises cinnamaldehyde as the aromatic aldehyde.
[0013] In some embodiments, the composition comprises a short chain (C 1 -C 6 ) alcohol or dimethyl sulfoxide (DMSO) solvents for the application and cell penetrating delivery of the aldehyde formulation.
[0014] In some embodiments taught herein, the polar solvent is at least one selected from the group consisting of methanol, ethanol, propanol, butanol, pentanol, hexanol and DMSO. In some embodiments, the polar solvent is ethanol. In other embodiments, the polar solvent is DMSO.
[0015] In some embodiments of the present invention, the method for curing and/or controlling intracellular bacteria in plants comprises injecting a plant with a composition comprising at least one aromatic aldehyde.
[0016] In some embodiments, the method of injection of a plant is by pressurized syringe.
[0017] In another embodiment, the method of injection of a plant is by drip bag.
[0018] In some embodiments of the present invention, the method for curing and/or controlling intracellular bacteria in plants comprises foliar spray of a composition comprising at least one aromatic aldehyde species.
[0019] In some embodiments, the intracellular bacteria infecting the plant are limited to the phloem.
[0020] In some embodiments, the intracellular bacteria infecting the plant are Liberibacters.
[0021] In some embodiments, the composition utilized in the taught methods comprises cinnamaldehyde as an aromatic aldehyde.
[0022] In another particular embodiment, the composition utilized in the taught methods comprises ethanol as a polar solvent for the aromatic aldehyde.
[0023] Further taught herein are compositions comprising (a) at least one aromatic aldehyde; and (b) at least one polar solvent, wherein said at least one aromatic aldehyde comprises cinnamaldehyde and at least one polar solvent comprises DMSO.
[0024] In some embodiments, the methods taught herein include the step of injecting or spraying one or more parts or tissues of a diseased plant, or a plant susceptible to attack by pathogens, with cinnamaldehyde, and a penetrating solvent in an amount sufficient to control growth of target pathogenic organisms.
[0025] In some embodiments, the compositions taught herein are effective as antibacterial curing agents against infections of Liberibacter, including, but not limited to Ca. L. asiaticus, causing Huanglongbing (HLB) disease.
[0026] In some embodiments, the composition relates to an injectable solution of aromatic aldehyde in greater than 5% ethyl alcohol.
[0027] In some embodiments, the composition relates to an injectable solution of aromatic aldehyde in up to about 100% DMSO.
[0028] In other embodiments, the taught composition is a solution comprising about 1.5% cinnamaldehyde in about 50% DMSO.
[0029] In other embodiments, the taught composition is a solution comprising about 1.5% cinnamaldehyde in about 100% DMSO.
[0030] The compositions of cinnamaldehyde and plant cell penetrating solvent such as DMSO or ethanol according to the present invention provide enhanced permeation of cinnamaldehyde, and combined with the natural defense systems of plants, or combined with a synergistic additional element, either a chemical or the genetically enhanced defense systems of plants, provides a prevention, inhibition, and/or cure for diseases caused by Liberibacters and likely other bacteria that live within living plant cells.
[0031] In some embodiments, the present invention teaches methods for treating a plant infected with a Liberibacter, said method comprising: contacting or injecting one or more parts of said plant with a composition comprising (i) at least one aromatic aldehyde; and (ii) at least one penetrating polar solvent; wherein said treated plant has reduced levels of Liberibacter.
[0032] In some embodiments, the aromatic aldehyde used in the methods of the present invention comprises cinnamaldehyde.
[0033] In some embodiments, the at least one polar solvent used in the methods of the present invention comprises DMSO.
[0034] In some embodiments, the methods of the present invention use a composition wherein the at least one aromatic aldehyde comprises cinnamaldehyde and the at least one polar solvent comprises DMSO.
[0035] In some embodiments the composition of the present invention is contacted with said plant by foliar spray.
[0036] In other embodiments, the composition of the present invention is injected into the plant.
[0037] In some embodiments, the methods of the present invention treat Liberibacter infections which are causing or caused citrus greening disease in the plant.
[0038] In some embodiments the Liberibacters of the present invention are selected from the group consisting of Ca. L. asiaticus, Ca. L. africanus and Ca. L. americanus.
[0039] In some embodiments, the methods of the present invention cure the plant from the Liberibacter infection.
[0040] In some embodiments, the treated plant of the present invention is a citrus tree or seedling.
[0041] Thus, In some embodiments, the present invention teaches a method for treating a plant infected with a Liberibacter, said method comprising: a) contacting or injecting one or more parts of said plant with a composition comprising (i) at least one aromatic aldehyde; and (ii) at least one penetrating polar solvent; wherein said at least one aromatic aldehyde comprises cinnamaldehyde and said at least one polar solvent comprises DMSO, and wherein the Liberibacter is selected from the group consisting of Ca. L. asiaticus, Ca. L. africanus and Ca. L. americanus, and wherein said treated plant has reduced levels of Liberibacter.
[0042] In some embodiments, the present invention teaches a composition for reducing the levels of Liberibacter in an infected plant, said composition comprising: (a) at least one aromatic aldehyde; and (b) at least one penetrating polar solvent, wherein the at least one aromatic aldehyde comprises cinnamaldehyde and the at least one polar penetrating solvent comprises DMSO.
[0043] In some embodiments the composition of the present invention is applied as a foliar spray.
[0044] In some embodiments the foliar spray is applied to the point of run-off.
[0045] In other embodiments, the composition of the present invention is injected into the plant.
[0046] In some embodiments, the composition of the present invention cures Liberibacter infected plants from their Liberibacter infection.
[0047] In some embodiments the composition of the present invention reduces the levels Liberibacter infection which causes citrus greening disease.
[0048] In some embodiments the present invention teaches the use of qPCR to detect Liberibacter infection.
BRIEF DESCRIPTION OF THE DRAWINGS
[0049] FIG. 1 . Effect of Carvacrol, Cinnamaldehyde and Geraniol against E. coli cells. Twenty microliter drops of three chemicals (at 100% strength) were placed on paper assay discs on top of E. coli lawn. Control disc included a solution of 70% ethanol without any added essential oil. Dotted line circles indicate zone of inhibition. Photo taken at 24 hrs after plating.
[0050] FIG. 2 . Effect of Carvacrol, Cinnamaldehyde and Geraniol against Liberibacter crescens cells. Twenty microliter drops of three chemicals, each diluted to a concentration of 2mg/ml were placed on paper assay discs on top of L. crescens lawn. Control disc included a solution of 70% ethanol without any added essential oil. Dotted line circles indicate zone of inhibition. Photo taken at 5 days after plating.
[0051] FIG. 3 . Normalized percent infection rate with Las of Hamlin citrus trees grafted onto Swingle citrumello rootstock, as measured over a period of approximately seven months. Results are presented as % Las infection (total number of positive leaf samples (assessed by qPCR as described above) divided by the total number of leaf samples taken per treatment on a given sampling date). Samples were taken monthly over a period of 6-7 months. Each bar in FIG. 3 represents average % Las infection for each treatment of 10 trees, and annotated by month sampled. The “0 month” samples are pooled averages of all trees sampled in each treatment before any treatments. Data are presented are normalized such that pre-treatment infections are 100%. Non-overlapping Standard Errors are significant at P<0.05. The control group comprises 5 trees that were sprayed with 50% DMSO and 5 trees that were injected with 50% DMSO. The experimental treatments are as follows, Treatment 1: trunk injection with 40 ml of 1.5% (w/v) cinnamaldehyde and 50% DMSO, followed by reapplication at month 4; Treatment 2: foliar spray 800 ml of 1.5% cinnamaldehyde in 50% DMSO, followed by reapplication at month 4.
[0052] FIG. 4 . Hamlin orange fruit yield, measured by pounds per tree, represented as total fruit weight per tree measured. The control and experimental groups are as described above in FIG. 3 .
DETAILED DESCRIPTION OF THE INVENTION
[0053] Citrus Greening
[0054] Huanglongbing (HLB), commonly known as citrus “greening” disease, is caused by a partially systemic bacterial infection of trees and other crop species, leading to leaf discoloration and reduced fruit production. In Florida, the spread of the invasive HLB disease presents a major threat to the citrus industry, whose loses due to this infection have reached millions of dollars per year. Since the insect vector has reached Texas and California, it is only a matter of time until the disease breaks out in those states as well.
[0055] HLB has been associated with infections from three liberibacter species: Candidatus Liberibacter asiaticus ( Las ) for the disease in Asia, Ca. L. africanus ( Laf ) for the disease in Africa, and Ca. L. americanus ( Lam ), for the disease in the Americas.
[0056] All three citrus liberibacters are uncultured and phloem-limited. That is, these bacteria live in plants entirely within living plant phloem cells. Las is the most widely distributed by far. In the whole of Asia, from the Indian subcontinent to Papua-New Guinea, HLB is exclusively caused by Las and transmitted by the Asian citrus psyllid, Diaphorina citri. Prior to 2004, Las was reported present only in Asia; it is now reported present in North, Central and South America. In Africa and Madagascar, HLB is caused by Laf and transmitted by the African citrus psyllid, Trioza erytreae. The “African” disease occurs in cool areas, often above 600 m altitude, with temperatures below 30° C. Both Laf and T. erytreae are native to Africa (Hollis, 1984; Beattie et al., 2008; Bové, 2013) and both are heat sensitive (Moran and Blowers, 1967; Catling, 1969; Schwarz and Green, 1972; Bové et al., 1974). In Brazil, both Las and Lam are transmitted by D. citri, the Asian citrus psyllid. Lam is significantly less heat tolerant than Las (Lopes et al., 2009b).
[0057] Beside the three citrus Liberibacters associated with HLB, three non-citrus Liberibacter species have been described. Ca. L. solanacearum ( Lso ), has been identified as the causal agent of serious diseases of potato (“Zebra chip”), tomato (“psyllid yellows”) and other solanaceous crops in the USA, Mexico, Guatemala, Honduras, and New Zealand (Hansen et al., 2008; Abad et al., 2009; Liefting et al., 2009; Secor et al., 2009). In solanaceous crops, Lso is vectored by the tomato/potato psyllid Bactericera cockerelli. More recently, a different haplotype of Lso was found infecting carrots in Sweden, Norway, Finland, Spain and the Canary Islands (Alfaro-Fernandez et al., 2012a, 2012b Munyaneza et al., 2012a, 2012b; Nelson et al., 2011). The carrot haplotype of Lso is spread by the carrot psyllid Trioza apicalis, which does not feed on Solanaceae. A fifth species of Liberibacter, Ca. L. europaeus ( Leu ) was recently found in the psyllid Cacopsylla pyri, the vector of pear decline phytoplasma. With C. pyri as the vector, Leu was transmitted to pear trees in which the liberibacter reached high titers but did not induce symptoms, thus behaving as an endophyte rather than a pathogen (Raddadi et al., 2011). Finally, a sixth species of Liberibacter, Liberibacter crescens ( Lcr ), was recently characterized after isolation from diseased mountain papaya (Babaco). Except for Lcr, which is not known to be pathogenic, all other described Liberibacters are pathogenic and must be injected into living plant cells by specific insects. Furthermore, the pathogenic Liberibacters can only live within specific insect and plant cells; as obligate parasites, they do not have a free living state.
[0058] To date, Lcr is the only Liberibacter t o be grown in axenic culture (Leonard et al., 2012), and thus can serve as a proxy for in vitro testing of antimicrobial chemicals. Lcr has not been reported to date to have been successfully reinoculated and grown in any plant. In plants, Liberibacters live entirely within living phloem cells. They become partially systemic in plants, moving from the site of injection by phloem to the roots and to newly forming leaf and stem tissues. Exposure of these bacteria to chemicals that may control them requires that the chemicals first penetrate multiple plant or insect cell layers and then to move in a systemic or semi-systemic manner.
[0059] Disease Adaptations may Help Citrus Greening Bacteria Avoid Triggering the Plant Innate Immune System
[0060] Despite the fact that Las and Lam have an intact outer membrane and presumably Lso does as well (Wulffe et al, 2014), most of the genes required for lipopolysaccharide (LPS) biosynthesis that are found in Las and Lso are missing from Lam, including lpxA, lpxB, and lpxC, which are involved in the first steps of the biosynthesis of lipid-A. Lack of LPS in Gram-negative species is very rare but the barrier function served by the LPS may not be needed by pathogenic Liberibacters. If the LPS is not needed as a barrier function in one Liberibacter then it may not function well as a barrier in the others, which may provide opportunities for unusual chemical control measures that would not likely work against bacteria with typical LPS barriers. Broad-spectrum antibiotics injected into trees have resulted in some degree of success, including penicillin G (Aubert and Bove, 1980; Zhang, Duan et al., 2010; Zhang, Powell et al., 2011).
[0061] Indeed, the barrier function normally provided by the LPS may be at least partially compensated by production of other classes of lipids in the outer membrane. For example, Treponema denticola was shown to be missing LPS but possessing instead a lipoteichoic acid-like membrane lipid, core structure and repeating units that functioned as a substitute permeation barrier (Schultz et al., 1998). Similarly, Sphingomonas paucimobilis (Kawahara et al., 1991) and S. capsulate (Kawahara et al., 2000) are devoid of LPS, but have as substitutes glycosphingolipids containing (S)-2-hydroxymyristic acid. In addition, Sorangium cellulosum produces sphingolipids as the major lipid class in the outer membrane, together with ornithine-containing lipids and ether lipids (Keck et al., 2011).
[0062] The loss of the Lam LPS indicates a distinct selection advantage served by losing the LPS, which is a major elicitor of plant innate immunity, or natural defense response. The LPS is one of several classic “pathogen-associated molecular patterns” or PAMPs, which are generally conserved molecules of microbial origin that are recognized by specific plant receptors, often in a synergistic manner, to trigger both early and late defense responses, including the oxidative burst, salicylic acid accumulation and callose deposition (Zipfel & Robatzek, 2010). Importantly, a defective LPS can still be capable of inducing PAMP triggered immunity (Deng et al., 2010).
[0063] Plant pathogenic microbes must either avoid PAMP recognition or actively suppress the plant defense responses that result from such recognition (Hann et al., 2010). Clearly, defects in the LPS barrier function would render Lam much more sensitive to innate plant immune responses than to most plant pathogenic microbes, but loss of all LPS components capable of PAMP activity should result in a reduced response in the first place.
[0064] In addition to missing nearly all LPS encoding genes, Lam is also missing a key outer membrane protein, OmpA, which helps stabilize the outer membranes of Gram negative bacteria, providing its structural shape, and anchoring it to the peptidoglycan layer (Smith et al. 2007). OmpA is the most abundant outer membrane protein in Enterobacteria (Bosshart et al. 2012); it is present at 100,000 copies cell-1 in E. coli (Koebnik et al. 2000). In E. coli, OmpA is believed to be a weak porin, involved in diffusion of nonspecific small solutes across the outer membrane (Sugawara and Nikaido 1992). OmpA is a major PAMP (Jeannin et al., 2002).
[0065] The phosphatidylcholine (PC) synthase pathway (de Rudder et al., 1999), which is unique to a small number (10-15%) of bacteria, including Rhizobium and Agrobacterium (Geiger et al., 2013) is found in all sequenced Liberibacters ( Lam _551; CLIBASIA_03680; CKC_04930; B488_05590), and could enable PC biosynthesis from the abundant choline present in either plant or insect host. In those bacteria synthesizing PC, PC strongly affects the physicochemical properties of the bacterial membranes (Geiger et al., 2013). Agrobacterium tumefaciens mutants lacking PC are markedly impaired in virulence and are hypersensitive to detergent (Wessel et al., 2006). Finally, Thermus thermophilus has no LPS but polar glycolipids and a phosphoglycolipid were detected in the outer membrane (Leone et al., 2006).
[0066] Although a nearly complete set of flagellar biosynthetic genes were reported in Las, some of the flagella biosynthetic genes were reported as pseudogenes (Duan et al., 2009). However, no Las or Lam flagella have been reported observed in any publications, despite numerous electron micrographs of these bacteria infecting plants and psyllids (for example, Bove, 2006). The lack of flagella indicates inability to produce or activate flagellin expression, resulting in loss of this PAMP activity. Both Las and Lam have clearly evolved a strategy of PAMP avoidance, due to an intracellular lifestyle that depends upon avoidance of activation of host defense and cell death responses. Any chemicals that trigger plant defense responses, such as salicyclic acid (SA) (Pieterse et al., 1996) or neonicotinoid pesticides (Ford et al., 2010) would place the Liberibacter outer membrane barrier function as a likely very sensitive last line of defense against these plant defenses.
[0067] Liberibacter spread is controlled primarily and poorly through control of the psyllid vector, primarily through the use of neonicotinoid pesticides. There are no known effective control measures known against the systemic Liberibacter pathogens in plants, and no known way to cure an infected plant. Since the HLB disease causes such severe citrus fruit losses and eventually death of the citrus tree, and since citrus trees in groves can last 15-25 years, these trees represent a considerable investment. A cure for the disease is urgently needed.
[0068] Treating Citrus Greening (Huanglongbing or HLB).
[0069] The present invention is based in part on the discovery that aromatic aldehydes, when combined with a solvent penetrant such as DMSO, can provide a beneficial phytotoxic composition capable of treating HLB caused by liberibacter infections. While the inventors do not wish to be bound by any one theory of function, they hypothesize that penetration of low levels of aldehydes through the plant cells by the action of DMSO causes failure of the Liberibacter outer membrane barrier function. Thus the inventors hypothesize that when combined with the non-lethal phytotoxic stress responses caused by the application of the compositions of the present invention, a beneficial systemic clearing effect is caused in the plant.
[0070] Cinnamaldehyde as a Disinfectant
[0071] Cinnamaldehyde is an organic aromatic aldehyde compound that is best known for giving cinnamon its flavor and odor. The pale yellow viscous liquid occurs naturally in the bark of cinnamon trees and other species of the genus Cinnamomum. Plants that make essential oils such as cinnamaldehyde reportedly synthesize the compounds in plastids, where they are released into the cytoplasm and secreted through the surrounding plasmalemma (cell membrane) and are at least locally transported into specialized cells that developed lignified and suberized (thickened) cell walls, become metabolically inactive, and compartmentalize these often toxic components from metabolically active cells (Geng et al., 2012 and references therein). Cinnamaldehyde can account for 60%-90% of the essential oils of some plant species, an amount that is toxic to surrounding metabolically active cells of the producing plant (Geng et al., 2012). Cinnamaldehyde is well known to be phytotoxic when used as an insecticide on herbaceous plants (Cloyd & Cycholl, 2002).
[0072] The high volatility and phytoxicity of cinnamaldehyde has led to recommendations for its use primarily as a disinfectant (Pscheidt and Ocamb, 2014). Because of its disinfecting properties, cinnamaldehyde has also found limited use in agricultural settings for surface contact pest control, when combined with additional preservative compounds. One plant essential oil previously used in agricultural applications and now discontinued was ProGuard® 30% Cinnamaldehyde Flowable Insecticide, Miticide and Fungicide (U.S. Pat. Nos. 6,750,256 B1 and 6,251,951 B1), containing the chemical preservative o-phenylphenol. U.S. Pat. No. 4,978,686 discloses that an antioxidant is required for use with cinnamic aldehyde for a composition which is used for application to crops. A method of protecting crops from attack of pests including insects using a composition comprising cinnamaldehyde and also requiring an antioxidant is disclosed in U.S. Pat. No. 4,978,686. Protection of crops against insect pests by applying an aqueous composition containing a cinnamaldehyde is disclosed in French patent application 2529755. U.S. Pat. No. 2,465,854 describes an insecticidal composition containing a cinnamaldehyde derivative.
[0073] In all these cases, however, cinnamaldehyde has only been effective as a contact insecticide, nematicide, miticide or fungicide, applied to the plant surface as a spray or as a soil drench, but with no established value beyond that of a disinfectant. Not contemplated or suggested were applications of cinnamaldehyde to control bacterial infections of plants, particularly to control internal bacterial infections of plants or insects, nor more particularly to control of bacteria that colonize plants or insects intracellularly, since contact with such pathogens would not likely occur, and in addition, either phytotoxicity or insect toxicity would be expected.
[0074] In some embodiments, the cinnamaldehyde of the present invention may be prepared by various synthetic methods known to those skilled in the art. For example, see, J. March, ed., Appendix B, Advanced Organic Chemistry: Reactions, Mechanisms, and Structure, 2nd Ed., McGraw-Hill, New York, 1977. Cinnamaldehyde may be prepared synthetically, for example, by oxidation of cinnamyl alcohol (Traynelis et al., J. Am. Chem. Soc. (1964) 86:298) or by condensation of styrene with formylmethylaniline (Brit. patent 504,125). Cinnamaldehyde may also be obtained by isolation from natural sources as known to those skilled in the art. Non-limiting examples of cinnamaldehyde sources include woodrotting fungus, Stereum subpileatum, or species of the genus Cinnamomum among other sources (Birkinshaw et al., 1957. Biochem. J. 66:188). In particular, cinnamon bark extract has been approved as a GRAS (Generally Recognized as Safe) material for food use based on 21 CFR (Code of Federal Regulation) part 172.515 (CFR 2009). Cinnamon bark extract contains multiple active compounds, including cinnnemaldehyde, that inhibit microorganisms (Burt 2004).
[0075] A number of the aromatic and aliphatic aldehydes may also find use in the subject invention, such as benaldehyde, acetaldehyde, piperonal, and vanillin, all of which are generally regarded as safe (GRAS) synthetic flavoring agents (21 CFR 172.515). In some embodiments, Coniferyl aldehyde may also find use in the subject invention.
[0076] Cell Penetrants
[0077] The present invention provides for plants, seeds, seedlings and plant parts such as fruit substantially free of systemic bacterial plant pathogens, particularly those plants, seeds, seedlings and plant parts previously infected with systemic bacterial pathogens of the genus Liberibacter. In some embodiments, the present invention also provides methods for controlling further systemic bacterial pathogen infections of plants using at least one aromatic aldehyde and a polar solvent and plant cell penetrant.
[0078] In some embodiments, the at least one aromatic aldehyde is combined with a cell penetrant such as benzyl alcohol.
[0079] In other embodiments, the at least one aromatic aldehyde is combined with a DMSO cell penetrant. While DMSO has been demonstrated to be effective as a cell penetrant, its phytotoxicity has always been considered to be a negative attribute, limiting its practical application in agricultural settings.
[0080] The present invention discloses the surprising finding that the phytotoxicity of aromatic aldehydes such as cinnamaldehyde, in penetrating solvents such as DMSO, if appropriately calibrated, can be used to enhance a plant's natural resistance against certain bacterial pathogens that systemically infect a plant, which is to our knowledge a previously unrecognized property of these compounds. In addition, the present invention discloses a synergistic anti-bacterial effect of aldehydes in combination with DMSO applied at discernably phytotoxic levels.
[0081] Compositions and Methods of Treating Citrus Greening
[0082] In some embodiments, the present invention teaches the use of cinnemaldehyde and solvent either alone or in combination with other active or inactive substances. In some embodiments, the compositions of the present invention may be applied by spraying, soil drenches, pouring, dipping, in the form of concentrated liquids, solutions, suspensions, powders and the like, containing such concentration of the active compound as is most suited for a particular purpose at hand. Cinnamaldehyde is highly hydrophobic and phytotoxic to plants when used at the standard rate of 4.98 ml per liter of a 30% solution normally used for contact disinfection (equal to 1.49 ml cinnamaldehyde per liter or 0.15%). Cinnamaldeyde's hydrophobic properties in particular can limit its ability to effectively function as an antibacterial agent aqueous environments (Kalemba and Kunicka 2003).
[0083] The inventors of the present invention discovered that in order to more effectively use aromatic aldehydes in foliar sprays or injectable formulations, although the aldehyde and solvent can be formulated alone, the aldehyde can be rendered more penetrating by including a surfactant such as Tween 80 or Silwet L77. In some embodiments of the present invention, other Liberibacter -curing compounds which can be used alone or in conjunction with the cinnamaldehyde include conferyl aldehyde, benaldehyde, acetaldehyde, piperonal, and vanillin, along with the terpene carvacrol.
[0084] In some embodiments, the present invention relates to a sprayable or injectable solution of Liberibacter curing compounds in greater than 5% ethyl alcohol or DMSO.
[0085] In other embodiments, the invention relates to a solution of aldehydes and any suitable polar solvent.
[0086] In some embodiments of the present invention, the composition for treating plants infected with Liberibacters comprises about 0.001%, 0.01%, 0.02%, 0.03%, 0.04%, 0.05%, 0.06%, 0.07%, 0.08%, 0.09%, 0.1%, 0.2%, 0.3%, 0.4%, 0.5%, 0.6%, 0.7%, 0.8%, 0.9%, 1%, 2%, 3%, 4%, 5%, 6%, 7%, 8%, 9%, 10%, 11%, 12%, 13%, 14%, 15%, 16%, 17%, 18%, 19%, 20%, 25%, 30%, 35%, 40%, 45%, 50%, 55%, 60%, 65%, 70%, 75%, 80%, 85%, 90%, 95%, or 100% of a Liberibacter curing compound.
[0087] In an embodiment of the present disclosure, the solution to treat plants infected with Liberibacters comprises about 0.001% to 10%, or 0.01% to 10%, or 0.1 to 10%, or 1 to 5%, or 1 to 10% of a Liberibacter curing compound.
[0088] In some embodiments the Liberibacter curing compound is an aromatic aldehyde.
[0089] In a particular embodiment the aromatic aldehyde is cinnamaldehyde:
[0000]
[0090] In another embodiment, the aromatic aldehyde is coniferyl aldehyde:
[0000]
[0091] In some embodiments, Liberibacter curing compounds are selected from the group consisting of cinnamaldehyde, conferyl aldehyde, benaldehyde, acetaldehyde, piperonal, and vanillin, along with the terpene carvacrol.
[0092] In some embodiments of the present disclosure, the Liberibacter curing compound is solubilized in about 1%, 2%, 3%, 4%, 5%, 6%, 7%, 8%, 9%, 10%, 11%, 12%, 13%, 14%, 15%, 16%, 17%, 18%, 19%, 20%, 25%, 30%, 35%, 40%, 45%, 50%, 55%, 60%, 65%, 70%, 75%, 80%, 85%, 90%, 95%, 99% or 100% polar solvent. In some embodiments the protic solvent is ethanol, methanol, isopropanol, and acetic acid among others.
[0093] In some embodiments of the present disclosure, the Liberibacter curing compound is solubilized in about 1%, 2%, 3%, 4%, 5%, 6%, 7%, 8%, 9%, 10%, 11%, 12%, 13%, 14%, 15%, 16%, 17%, 18%, 19%, 20%, 25%, 30%, 35%, 40%, 45%, 50%, 55%, 60%, 65%, 70%, 75%, 80%, 85%, 90%, 95%, 99% or 100% DMSO.
[0094] In some embodiments, the formulation includes cinnamaldehyde and/or coniferyl aldehyde in a formulation involving DMSO. One formulation for treating Liberibacter infected citrus, potato or tomato, contains cinnamic aldehyde and/or coniferyl aldehyde, 0.001% to 10% by weight in 70% ethanol or 50% DMSO. In some embodiments, the total amount of aldehyde(s) present in the formulation is 1.5% or less. The formulations are effective and stable without the use of antioxidants, although particular aldehydes may have inherent antioxidant properties, for example, coniferyl aldehyde. Stability of the formulation can be evaluated by a variety of methods, including accelerated tests in which a formulation of interest is exposed to elevated temperatures over a set time. Samples of the formulations are taken at regular intervals and analyzed chemically by methods known to those skilled in the art to determine the rate and nature of degradation.
[0095] The most effective amount for compositions including cinnamaldehyde and/or coniferyl aldehyde which may find use and can be determined using protocols such as those described in the Examples. In some embodiments an effective treatment amount is about 0.01 g/l, 0.02 g/l, 0.03 g/l, 0.04 g/l, 0.05 g/l, 0.06 g/l, 0.07 g/l, 0.08 g/l, 0.09 g/l, 0.1 g/l, 0.2 g/l, 0.3 g/l, 0.4 g/l, 0.5 g/l, 0.6 g/, 0.7 g/l, 0.8 g/l, 0.9 g/l, 1 g/l, 2 g/l, 3 g/l, 4 g/l, 5 g/l, 6 g/l, 7 g/l, 8 g/l, 9 g/l, 10 g/l, 11 g/l, 12 g/l, 13 g/l, 14 g/l, 15 g/l, 16 g/l, 17 g/l, 18 g/l, 19 g/l, 20 g/l, 25 g/l, 30 g/l, 35 g/l, 40 g/l, 45 g/l, 50 g/l, 55 g/l, 60 g/l, 65 g/l, 70 g/l, 75 g/l, 80 g/l, 85 g/l, 90 g/l, 95g/l, or 100 g/l (w/v) of liberibacter curing compound. In some embodiments an effective treatment amount of liberibacter curing compound is 0.01 g/l to 25 g/l. These protocols also can be used to optimize each formulation for specific conditions as well as for use on specific plants to minimize phytotoxicity while maximizing the antipathogenic effect of the formulation.
[0096] In some instances, the efficacy of the formulation can be increased by adding one or more other components, i.e., a compound other than cinnamaldehyde to the formulation where it is desirable to alter particular aspects of the formulation. As an example, it may be desirable for certain applications to decrease the phytotoxicity or to increase the antipathogenic effect of the formulation (e. g. mean disease resistance of 60% or better, with a least about 70% or greater, see below) or both.
[0097] In some embodiments, the additional component(s) minimize phytotoxicity while increasing the antipathogenic effect of the formulation. Of particular interest is the use of a component(s) which is a synergist to increase the mean disease resistance while minimizing the phytotoxic effect as related to a particular formulation. By “synergistic” is intended a component which, by virtue of its presence, increases the desired effect by more than an additive amount.
[0098] A synergistic effect can be defined by applying the Colby formula (Colby, R. S., “Calculating Synergistic and Antagonistic Responses of Herbicide Combinations”, 1967 Weeds, vol. 15, pp. 20-22), i.e. (E)=X+Y−(X*Y/100).
[0099] The concentration of one or more of the other formulation ingredients can be modified while preserving or enhancing the desired phytotoxic and antipathogenic effect of the formulation. Of particular interest is the addition of components to a formulation to allow for a reduction in the concentration of one or more other ingredients in a given formulation while substantially maintaining efficacy of the formulation. Combination of such a component with other ingredients of the formulation can be accomplished in one or more steps at any suitable stage of mixing and/or application.
[0100] Detection of Liberibacter Infection
[0101] In some embodiments, the methods and compositions of the present invention reduce the levels of Liberibacter bacteria in infected plants. In some embodiments, the reduction is measured as a reduced bacterial titer. In other embodiments, the effectiveness of the treatments and compositions is measured by the curing of a percentage of treated plants.
[0102] In some embodiments the present invention teaches methods and compositions of curing citrus greening disease, wherein cure means the reduction of bacterial titer to the point where it is no longer detectable for an extended period of time. In some embodiments the extended period of time is 3 months, 6 months, or 9 months.
[0103] In some embodiments, the present invention teaches methods of detecting Liberibacter infections in plants.
[0104] In some embodiments, Liberibacters are detected via polymerase chain reaction (PCR) in which known sequences of the liberibacter organism are amplified and detected as a proxy for the presence of the organism itself. In some embodiments, the PCR of the present invention is quantitative PCR (qPCR) in which the presence of Liberibacters is quantified based on the number of PCR cycles required to reach a threshold quantity of gene copy product.
[0105] In other embodiments, the present invention teaches alternative methods of detecting Liberibacter infections including reverse transcriptase PCR, Northern Blots, Southern Blots, and Western Blots. In other embodiments the present invention also teaches methods of detecting Liberibacter infections via bacterial cultures of infected tissues, and immuno-labeling of infected tissues.
[0106] In other embodiments, the present invention teaches methods of detecting infected plants by the presence of citrus greening disease phenotypes described herein.
EXAMPLE 1
Effect of Cinnamaldehyde, Carvacrol and Geraniol on E. Coli.
[0107] The essential oils cinnamadehyde (Aldrich, W228605; ≧98% purity), carvacrol (Aldrich, W224502; ≧98% purity) and geraniol (Aldrich, 163333; 98% purity) were purchased Sigma-Aldrich (St. Louis, Mo.). A single colony of E. coli Stratagene strain “Solopack” was inoculated in 5 ml of Luria Broth (LB) liquid medium with shaking at 37° C. overnight. Two hundred μl of the E. coli overnight cultures were placed on an LB agar plate, and spread evenly with glass beads. The bacterial culture was allowed to absorb into the LB medium. Within 30 min after absorption, 20 μl drops of the three essential oils (cinnamaldehyde, carvacrol or geraniol) were separately placed without dilution on 6 mm discs (Whatman, Cat No. 2017-006; GE healthcare Life Science) and the treated disks were placed on top of the plates with E. coli. The plates were then incubated for 24 hrs. Photos were taken at 24 hrs after plating (see FIG. 1 ). Experiments were repeated, with the same results.
[0108] Consistent with the literature, the results were that all three chemicals were inhibitory of the growth of E. coli, with carvacrol more inhibitory than cinnamaldehyde, which was in turn more inhibitory than geraniol.
EXAMPLE 2
Effect of Cinnamaldehyde, Carvacrol and Geraniol on Liberibacter Crescens.
[0109] Experiments similar to those conducted in Example 1 were conducted using L. crescens strain BT-1 ( Lcr ), except that Lcr was cultured using BM7 medium, top agar was used, and the three chemicals (cinnamaldehyde, carvacrol and geraniol) were diluted with 70% ethanol to concentrations ranging from 2 mg/ml 0.125 mg/ml. BM7 medium contains 2 g alpha ketoguraric acid, 10 g N-(2-Acetamido)-2-aminoethanesulfonic acid, N-(Carbamoylmethyl) taurine, 3.75 g KOH, 150 ml Fetal bovine Serum, 300 ml TNM-FH in 1 Liter (L) water. Agar was added at 20 g/L for solid medium). Lcr BT-1 bacteria were incubated at 29 ° C. with shaking until reaching an optical density at 600 nm (OD600) of 0.5 -0.6. At this point, 500 μl of the cultures were added to 4 ml of 0.6% BM7 top agar, mixed well and then poured on the top of one BM7 plate and allowed to solidify. Immediately after solidifying, 20 μl drops of the three essential oils (cinnamaldehyde, carvacrol and geraniol) were placed using two-fold serial dilutions in 70% ethanol ranging from 2 mg/ml to 0.125 mg/ml on 6 mm discs and the treated disks were placed on top of the plates with Lcr. The plates were then incubated for 5 days. Photos were taken 5 days after plating. A control solution of 70% ethanol without any added essential oil was also placed on a disk and applied at the same time in each experiment. Experiments were repeated twice (see FIG. 2 ).
[0110] The results showed that only cinnemaldehyde and carvacrol were inhibitory of the growth of Lcr, with surprisingly strong inhibition by cinnamaldehyde at 2 mg/ml and only slight inhibition by carvacrol at the same concentration (a concentration of carvacrol, but not cinnamaldehyde, that is phytotoxic; refer Example 3 below). Geraniol was not inhibitory to Lcr at these levels. Cinnamaldehyde was also inhibitory in these tests to a level of 1 mg/ml. The Minimum Inhibitory Concentration (MIC) of cinnamaldehyde was 0.005 mg/ml.
EXAMPLE 3
Phytotoxic Effect of 10% Cinnamaldehyde, Carvacrol and 70% Ethanol Foliar Sprays on Citrus
[0111] To test the phytoxicity of cinnamaldehyde or carvacrol in 70% ethanol, and 70% ethanol alone on citrus plants, we applied 1% (w/v) and 10% (w/v) cinnamaldehyde or carvacrol (each dissolved in 70% ethanol) on Swingle rootstocks (˜6 inches to 1 foot tall) by spraying to the point of run-off of the spray and also sweet orange (˜3 foot tall) by painting one or both sides of a portion of the leaf surface. We also applied 70% ethanol as control in these two methods.
[0112] The results were that even 1% carvacrol in 70% ethanol was highly phytotoxic to citrus and to sweet orange leaves, observable by 24 hours after treatment. By contrast, cinnamaldehyde at 1% in 70% ethanol, and 70% ethanol alone, were not at all phytotoxic to citrus. Cinnamaldehyde at 10% w/v in 70% ethanol was moderately phytotoxic, producing chlorosis and leaf curling, but not defoliation.
EXAMPLE 4
Phytotoxic Effect of Cinnamaldehyde, Carvacrol and 70% Ethanol Soil Drench on Citrus
[0113] To further test the phytoxicity of cinnamaldehyde or carvacrol in 70% ethanol, and 70% ethanol alone on citrus plants, we applied 1% and 10% cinnamaldehyde or carvacrol (each dissolved in 70% ethanol) on Swingle rootstocks (˜6 inches to 1 foot tall) by adding sufficient liquid to soil of potted citrus to the point of run-off of the drench. We also applied 70% ethanol as control in these two methods.
[0114] The results were that carvacrol at 8 mg/ml (1%) of 70% ethanol was highly phytotoxic to citrus as a soil drench, observable by 60 hrs after treatment. By contrast, cinnamaldehyde at 1% in 70% ethanol, and 70% ethanol alone, were not at all phytotoxic to citrus applied as a soil drench. Cinnamaldehyde at 10% w/v in 70% ethanol was moderately phytotoxic, producing chlorosis and leaf curling, but not defoliation.
EXAMPLE 5
No Effect of 1% Cinnamaldehyde and 70% Ethanol Spray on Curing Las -Infected Citrus
[0115] To test the ability of 1% cinnamaldehyde to cure Las from systemically infected Pineapple Sweet Orange citrus plants grown from seeds and maintained in a greenhouse, we first graft-inoculated the plants, waited for symptoms to appear (about 6 months later) and then tested for presence of Las infection by semi-quantitative polymerase chain reaction (qPCR or PCR) tests. Granular imidacloprid was applied at recommended rates to all greenhouse grown plants. The plants were confirmed infected in multiple tests over a period of at least 3 months. We then applied 1% (w/v) cinnamaldehyde (dissolved in 70% ethanol) by spraying the foliage of infected sweet orange plants to the point of run off of the spray (˜3 foot tall trees). Subsequent qPCR tests performed 1-2 weeks later were qPCR positive and remained positive for at least several months. Positive samples were defined as those reaching a C t (threshold cycle) value of less than or equal to 35, using qPCR primers and methods as described by Li et al (2006). The C t value a relative measure of the concentration of target in the qPCR reaction. Control citrus plants sprayed with 70% ethanol alone were qPCR positive and remained positive for at least several months.
[0116] These results indicated that commercially available formulations of cinnamaldehyde, none of which to our knowledge were formulated with DMSO, would not by themselves kill Las or cure Las infected citrus, due to the protection afforded by their intracellular existence in plants.
EXAMPLE 6
Effect of 0.3% and 1.5% Cinnamaldehyde in 50% DMSO Sprayed onto HLB Symptomatic, Field Grown Citrus Moved to Pots.
[0117] To test the ability of sprayed cinnamaldehyde to cure Liberibacter from systemically infected sweet orange trees by spraying to run-off and using 50% DMSO as a penetrating solvent, approximately 3 year old mature Hamlin sweet orange trees grafted onto Swingle rootstock and exhibiting strong Huanglongbing symptoms in a field situation were pruned to approximately 4 to 5 feet in height, dug out of the field, placed in large (25 gallon) pots, brought into a greenhouse and tested for presence of Las infection by PCR. The plants were confirmed infected in multiple tests over a period of 2 weeks. These plants had been treated with imidacloprid in the field and granular imidacloprid was applied at recommended rates to all greenhouse grown plants.
[0118] We then applied 0.3% and 1.5% and cinnamaldehyde (dissolved in 50% DMSO) by spraying the foliage to the point of run off of the spray. The 1.5% cinnamaldehyde treated sweet orange trees, already stressed by uprooting and repotting, completely defoliated 6-7 days later; the 0.3% cinnamaldehyde treated plants appeared unaffected. Approximately 2 weeks later, new shoots began to emerge from the 1.5% treated plants, and the following week, new shoots were large enough to begin PCR tests for presence of Las.
[0119] The plants treated with 1.5% cinnamaldehyde in 50% DMSO were completely Las negative, but the 0.3% treated plants remained infected. Subsequent qPCR tests performed each week for the next nine months confirmed that the 1.5% treated plants were cured, with no detectable levels of Liberibacter infection and no citrus greening symptoms.
[0120] Control trees sprayed or injected with only 50% DMSO also defoliated but subsequently emerging new shoots either died or were qPCR positive. This demonstrated that DMSO alone, was not sufficient to treat Liberibacter infection.
[0121] The results from these experiments showed the surprising results that 1.5% cinnamaldehyde in 50% DMSO could be utilized to cure Las infections of citrus by spraying re-potted—and therefore highly stressed—citrus trees to run-off.
EXAMPLE 7
Effect of 1.5% Cinnamaldehyde and 100% DMSO Injected into HLB Symptomatic, Field Grown Citrus Moved to Pots
[0122] To test the ability of cinnamaldehyde to cure Liberibacter from systemically infected sweet orange trees when delivered using DMSO by injection, approximately 3 year old mature Hamlin sweet orange trees grafted onto Swingle rootstock and exhibiting strong Huanglongbing symptoms in a field situation were pruned to approximately 4 to 5 feet in height, dug out of the field, placed in large (25 gallon) pots, brought into a greenhouse and tested for presence of Las infection by PCR. These plants had been treated with imidacloprid in the field and granular imidacloprid was applied at recommended rates to all greenhouse grown plants. The plants were confirmed infected in multiple tests over a period of 2 weeks.
[0123] We then used two spring loaded syringes (Chemj et Tree Injectors; Queensland Plastics, Australia) on each tree. Each injector held 20 ml volume of injected material; in this case 1.5% (w/v) cinnamaldehyde in 100% DMSO. The injectors were placed in the trees by drilling a ½″ hole ca. ⅘ of the way through the diameter of each trunk, at a site approximately 12-14″ above the soil line. The injector was screwed firmly into place and the spring loaded syringe was then released, resulting in pressurized injection of the solution.
[0124] The 1.5% cinnamaldehyde injected sweet orange trees, already stressed by uprooting and repotting as in Example 6, completely defoliated 6-7 days later. Approximately 2 weeks later, new shoots began to emerge from these treated plants, and the following week, new shoots were large enough to begin PCR tests for presence of Las.
[0125] The 1.5% treated plants were completely negative, and subsequent PCR tests performed each week for the next 9 months confirmed that the 1.5% cinnamaldehyde injected plants remained completely PCR negative and were thus cured. This demonstrated that 1.5% cinnamaldehyde in 100% DMSO could be utilized to cure Las infections of citrus by injecting re-potted—and therefore highly stressed—citrus trees.
EXAMPLE 8
Effect of 1.5% Cinnamaldehyde and 50% DMSO on Liberibacter -Infected Citrus Trees Grown in Commercial Groves by Trunk Injection and by Spray Application
[0126] Most of the trees in an entire commercial grove of well maintained, four year old Hamlin trees grafted onto Swingle citrumello rootstock and treated regularly with imidacloprid insecticide, a plant SAR inducer (Ford et al., 2010), were found to be heavily diseased with classic symptoms of HLB, including blotchy mottling, yellowing of some branches, and premature fruit drop. Highly symptomatic citrus trees were selected, numbered and all were completely randomized as to treatment. Subsequent qPCR testing of 2-3 randomly sampled leaves per tree taken from different branches of each symptomatic tree resulted in a Las positive infection rate of greater than 70% of the trees in the grove.
[0127] Ten symptomatic trees were randomly selected for trunk injection (Treatment 1 in FIG. 3 ) as outlined in Example 7, using 40 mls of 1.5% (w/v) cinnamaldehyde and 50% DMSO, and another 10 infected trees were randomly selected for spray applications using 800 ml of the same treatment in a manner similar to that used in Example 6, but using 800 ml to cover a much larger, four year old, field grown tree, such that there was no run-off (Treatment 2 in FIG. 3 ). Five trees each were injected and 5 trees sprayed (Controls in FIGS. 3 and 4 ) using 50% DMSO.
[0128] Results are presented as % Las infection (total number of positive leaf samples (assessed by qPCR as described above) divided by the total number of leaf samples taken per treatment on a given sampling date). Samples were taken monthly over a period of 6-7 months. Each bar in FIG. 3 represents average % Las infection for each treatment of 10 trees, taken month by month. The “0 month” samples are pooled averages of all trees sampled in each treatment before any treatments. Data are presented are normalized such that pre-treatment infections are 100%. Non-overlapping Standard Errors are significant at P<0.05.
[0129] From these results, it is clear that 40 ml 1.5% Cinnamaldehyde in 50% DMSO injected into large, field grown (4 year old) Hamlin citrus trees (Treatment 1 in FIG. 3 ) resulted in a significant reduction of Las infection (from about 100% to about 35% infection), and the result lasted for about 3 months. Spray treatments using 800 mls of 1.5% Cinnamaldehyde in 50% DMSO (Treatment 2 in FIG. 3 ), also had a statistically significant effect on Las infection levels, but the effect lasted only for 2 months, and appeared less effective overall at the applied application rate, based on an analysis of the total fruit yields measured from all treatments (see FIG. 4 ). Treatments 1 and 2 were reapplied in this field trial; both treatments were reapplied 4 months later to the same trees in the manner described. Again, similar results were observed, with infection levels becoming significantly reduced using both injection or spraying methods.
[0130] For the fruit yield data presented in FIG. 4 , all trees were harvested at the same time in the fall (normal for Hamlin oranges in that field), and total fruit weight per tree measured. Treatment 1 yielded 66 pounds of fruit per tree, which was significantly higher than the yield of 45 pounds of fruit per tree from the control group (labeled “Control” in FIG. 4 ), while Treatment 2 yielded only 35 pounds of fruit per tree, which was not significantly different from the yield of the control group.
EXAMPLE 9
Effect of 1.5% Cinnamaldehyde and 5-50% DMSO on Liberibacter -Infected Potato, Tomato, Celery, and Carrot Plants
[0131] To test the ability of cinnamaldehyde to cure Liberibacter from systemically infected potato, tomato, celery, and carrot plants, including Ca. L. solanacearum and new species of Liberibacters yet to be described, the presence of Liberibacter infection will be tested by PCR using methods well known to those skilled in the art. 1.5% cinnamaldehyde (dissolved in 5-50% DMSO) will be applied to infected potato, tomato, celery and carrot plants by spraying the foliage of plants to the point of run off of the spray. Subsequent PCR tests will be performed 1-2 weeks later using PCR. It is expected that these subsequent PCR tests will be negative or will show reductions of titers after treatment.
[0132] Significantly reduced infection rates and increased produce yields are expected.
EXAMPLE 10
Effect of Carvacrol and 5-50% DMSO on Liberibacter -Infected Liberibacter -Infected Potato, Tomato, Celery, Citrus and Carrot Plants
[0133] To test the ability of Carvacrol to cure Liberibacter from systemically infected potato, tomato, celery, citrus, and carrot plants, including Ca. L. solanacearum and new species of Liberibacters yet to be described, the presence of Liberibacter infection will be tested by PCR using methods well known to those skilled in the art. 0.5%-10% carvacrol (dissolved in 5-50% DMSO) will be applied to infected potato, tomato, celery, citrus, and carrot plants by spraying the foliage of plants to the point of run off of the spray. Subsequent PCR tests will be performed 1-2 weeks later using PCR. It is expected that these subsequent PCR tests will be negative or will show reductions of titers after treatment.
[0134] Significantly reduced infection rates and increased produce yields are expected.
[0135] Unless defined otherwise, all technical and scientific terms herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Although any methods and materials, similar or equivalent to those described herein, can be used in the practice or testing of the present invention, the preferred methods and materials are described herein. All publications, patents, and patent publications cited are incorporated by reference herein in their entirety for all purposes.
[0136] The publications discussed herein are provided solely for their disclosure prior to the filing date of the present application. Nothing herein is to be construed as an admission that the present invention is not entitled to antedate such publication by virtue of prior invention.
[0137] All references, articles, publications, patents, patent publications, and patent applications cited herein are incorporated by reference in their entireties for all purposes. However, mention of any reference, article, publication, patent, patent publication, and patent application cited herein is not, and should not be taken as an acknowledgment or any form of suggestion that they constitute valid prior art or form part of the common general knowledge in any country in the world.
[0138] While the invention has been described in connection with specific embodiments thereof, it will be understood that it is capable of further modifications and this application is intended to cover any variations, uses, or adaptations of the invention following, in general, the principles of the invention and including such departures from the present disclosure as come within known or customary practice within the art to which the invention pertains and as may be applied to the essential features hereinbefore set forth and as follows in the scope of the appended claims.
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Liefting, L. W., Weir, B. S., Pennycook, S. R., Clover, G. R. G. 2009. ‘ Candidatus Liberibacter solanacearum ’, associated with plants in the family Solanaceae. Int. J. Sys. Evol. Microbiol. 59:2274-2276.
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Leone, S., Molinaro, A., Lindner, B., Romano, I., Nicolaus, B., Parrilli, M., Lanzetta, R., and Holst, O. 2006. The structures of glycolipids isolated from the highly thermophilic bacterium Thermus thermophilus Samu-SA1. Glycobiology. 16:766-775.
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[0185] Schwarz, R. E., and Green, G. C. 1972. Heat requirements for symptom suppression and inactivation of the greening pathogen. Proceedings 5th Conference of the International Organization of Citrus Virologists, University of Florida Press, Gainesville, Fla., 44-51.
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[0189] Sugawara, E., and Nikaido, H. 1992. Pore-forming activity of OmpA protein of Eschericha coli. J. Bio. Chem. 267:2507-2511.
[0190] Teixeira, D. C., Saillard, C., Eveillard, S., Danet, J. L., da Costa, P. I., Ayres, A. J. and Bové, J. 2005. “ Candidatus Liberibacter americanus ”, associated with citrus huanglongbing (greening disease) in Sao Paulo State, Brazil. Int. J. Sys. Evol. Microbiol. 55:1857-62.
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[0194] Zhang M Q, Powell C A, Zhou L J, He ZL, Stover E, Duan Y P. 2011. Chemical compounds effective against the citrus Huanglongbing bacterium Candidatus Liberibacter asiaticus in planta. Phytopathology 101:1097-1103.
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Methods and compositions based upon using phenolic aromatic aldehydes (ex: cinnamaldehyde, benzaldehyde) are provided, which find use as agents for treating, preventing, or curing systemic bacterial infections of living plants, in particular against Gram negative bacteria and more particularly species of Liberibacter, including Ca. Liberibacter asiaticus. The agent compositions described are used synergistically with other antimicrobial compounds, such as those that plants manufacture or release as a result of biotic or abiotic stresses, including the application of the aldehydes, proteins, whether produced by recombinant methods or not, or by essential oils such as carvacrol or allicin. Methods of applying the compositions for agriculture use are disclosed.
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BACKGROUND OF THE INVENTION
[0001] 1. Field of the Invention
[0002] This invention relates to heat exchangers generally, and, more particularly, to heat exchange processes and to heat exchangers that contain and utilize fluidized small solid particles to improve the transfer of heat on one side of the wall that separates two fluids.
[0003] 2. Background Art
[0004] High heat transfer rates have been reported for surfaces immersed in small solid particles that are suspended and kept in motion by an upward flow of a fluid. The overall heat transmission coefficient of a heat exchanger is in the range from 35 to 50 BTU/hr° F.ft 2 (i.e. British thermal unit per hour-degree Fahrenheit-square foot). Details of the heat exchanger are described in my pending U.S. patent application Ser. No. 09/028,053 filed on Feb. 23, 1998. The heat exchanger includes a fluidized bed of small solid particles that are suspended in a flow of a fluid in which the downward tendency of the small solid particles to fall by gravity is equaled by the upward drag force of the fluid flow. The heat exchanger includes a plurality of flat surfaced pipes or tubes, a top woven wire mesh or perforated sheet disposed on top surfaces of the flat surfaced pipes, and a grid plate disposed on bottoms of the flat surfaced pipes. The small solid particles are disposed between the flat surfaced pipes and between the top woven wire mesh and the grid plate. This heat exchanger, however, needs additional new features for the top woven wire mesh or perforated sheet and the grid plate to make the heat exchanger more efficient.
SUMMARY OF THE INVENTION
[0005] It is an object of the present invention to provide an improved heat exchanger exhibiting increased efficiency.
[0006] It is another object to provide a heat exchanger that maintains the same capacity although constructed smaller in size.
[0007] It is still another object to provide a heat exchanger having folded and shaped woven wire mesh or perforated sheets able to reduce the overall pressure drop within the heat exchanger during operational service.
[0008] It is yet another object to provide an improved orifice plate equipped with a plurality of orifices allowing fluid passage.
[0009] It is a further object to provide a heat exchanger having a more efficient fluidized bed.
[0010] It is also an object to provide a heat exchanger able to improve heat exchange rates by using small solid particles having tetrahedron or pyramid shapes.
[0011] These and other objects may be achieved with a heat exchanger that contains solid particles in a fluidized bed inside the heat exchanger, that has heat transfer surfaces that are not immersed in the solid particles, that has a loosely packed fluidized bed of small solid particles, that generally only allows a bubbling boiling movement of the solid particles direction rather than allowing a circulating motion, that does not need to use devices to restrain the fluidized bed, does not require any special coating on the heat exchanger surface, that has no vertical tubes, that maintains the two fluids exchanging beat separate from each other, does not require using heating elements in the fluidized bed, that uses flat walls to increase the heat transfer coefficient, that does not use slits or slots, that does not have a space between the distributor plate and the bottom of the tube inlets that creates circulating fluid patterns, that does not require embedding larger particles in the fluidized bed, and uses small solid particles with shapes that allow for an increased amount of heat exchange. This should allow heat exchangers of all types to be made smaller than priorly possible while still maintaining the same level of heat transfer between the two fluids.
[0012] The heat exchanger includes flat surfaced pipes or tubes conveying one of the fluids involved horizontally. The flat surfaced pipes are spaced-apart from each other and firmly attached to a grid plate that is perforated with orifices that introduce the other fluid involved in the heat exchange process and flowing upward and between the flat surface pipes. A top woven wire mesh or perforated sheet is held tightly against the tops of the flattened pipe or tubes to keep the small solid particles from falling out from a top portion of the heat exchangers between the tops of the flattened pipe when the heat exchangers are handled. The bottom woven wire mesh or perforated sheet is held tightly against the bottom or inlet side of the grid plate to keep the small solid particles from draining out from a bottom portion of the heat exchanger between the bottoms of the flattened pipe whenever the heat exchanger has no upward flowing fluid through the orifices. The small solid particles are disposed to move within a heat exchanging space defined between the flat surfaced pipes and between the top woven wire mesh or perforated sheet and the bottom woven wire mesh or perforated sheet. Bubbles are formed above the orifices whenever more fluid is introduced through the orifices than will pass through the spaces between the small solid particles.
[0013] The woven wire mesh or perforated sheets on the top and bottom can be folded or shaped to both increase their respective surface areas and decrease the volume of the heat exchanging space which will thereby reduce the overall pressure drop when in service. Some versions of the improved heat exchangers may be constructed without any orifice plate. The orifice plate may contain one or more orifices in a given enclosed area. The orifices may be round, square or of some other shape. Tetrahedron or pyramid shaped particles may be used for the small solid particles to be manufactured.
BRIEF DESCRIPTION OF THE DRAWINGS
[0014] A more complete appreciation of this invention, and many of the attendant advantages thereof, will be readily apparent as the same becomes better understood by reference to the following detailed description when considered in conjunction with the accompanying drawings in which like reference symbols indicate the same or similar components, wherein:
[0015] [0015]FIG. 1 is a cross-sectional view of the heat exchanger that is at a right angle to the flat surfaced pipe or tubing that conveys one of the fluids horizontally;
[0016] [0016]FIG. 2 is a cross-sectional view taken along lines II-II′ of FIG. 1;
[0017] [0017]FIGS. 3A, 3B, 3 C and 3 D are top views of the orifice plate showing various configurations and types of orifices that may be employed in the construction of a heat exchanger in accordance with the principles of the present invention;
[0018] [0018]FIG. 4 is a cross-sectional view of another embodiment of the heat exchanger constructed according to the principles of the present invention;
[0019] [0019]FIG. 5 is a cross-sectional view taken along lines V-V′ of FIG. 4; and
[0020] [0020]FIGS. 6A, 6B, 6 C and 6 D are three-dimensional views of small particles that may be manufactured that are with shapes of tetrahedrons or pyramids for use in a heat exchanger constructed according to the principles of the present invention.
DESCRIPTION OF THE PREFERRED EMBODIMENT
[0021] Turning now to the drawings, FIG. 1 is a cross-sectional view of a heat exchanger when viewed at a right angle to a plurality of parallel and horizontally spaced-apart flat surfaced pipes or tubes 1 that convey one of the fluids involved in a heat exchange process horizontally. The direction of the second fluid that is conveyed through the heat exchanger is denoted by arrows A. Small solid particles 2 are drawn as triangles to represent tetrahedrons, which is one of the preferred shapes for particles. Preferably, particles 2 are solid. Flattened pipe or tube 1 is attached to a grid plate 3 that is perforated with the orifices 4 that introduce the other fluid involved.
[0022] Top woven wire mesh or perforated sheet 5 is held tightly against the tops of the flattened pipe or tube 1 to keep the particles 2 from falling out when the heat exchanger is handled. The angle θ between the flattened top surface of pipe 1 and the neighboring downward fold of top woven wire mesh or perforated sheet 5 can be between approximately 30° and 90°. The folded or shaped top woven wire mesh or perforated sheet 5 increases its surface area and decreases the volume of a heat exchanging space which will thereby reduce the overall pressure drop when in service.
[0023] Bottom woven wire mesh or perforated sheet 6 is held tightly against the bottom or inlet side of the grid plate 3 to keep the particles 2 from draining out from between neighboring pipes 1 whenever the heat exchanger has no upwardly flowing fluid through the orifices as indicated by the upwardly rising direction of arrows A. Bubbles 7 are formed above the orifices 4 whenever more fluid is introduced through the orifices 4 than will readily pass through the interstices between solid particles 2 .
[0024] [0024]FIG. 2 is a cross-sectional view of the heat exchanger that is taken along cross-sectional line II-II′ in FIG. 1. The side of pipe 1 that conveys the horizontally flowing fluid is shown as well as its fluid flow that is indicated by arrows B that point from left to right. Particles 2 , grid plate 3 perforated by orifices 4 , upper wire mesh 5 , lower wire mesh 6 , and bubbles 7 are shown again. Pitch divider fins 8 are spaced-apart from each other and coupled to two spaced-apart and adjacent flat surfaces of pipes 2 facing each other and are provided in order to increase heat transfer surface even when the heat exchanger is not pitched for drainage. Particles 2 move within the heat exchanging space defined by the two spaced-apart pitch divider fins 8 , two spaced-apart flat surfaces of pipes 1 , upper wire mesh 5 , and lower wire mesh 6 .
[0025] [0025]FIG. 3A shows a top view of grid plate 3 where shown in FIGS. 1 and 2. There is only one orifice 4 shown in the area bounded by the walls of the flattened pipe or tubing 1 and two adjacent pitch divider fins 8 .
[0026] [0026]FIG. 3B shows a second embodiment of grid plate 3 constructed according to the principle of the present invention. One orifice is shown centered in the area bounded by the walls of the flattened pipe or tubing 1 and two adjacent pitch divider fins 8 with four other orifices 4 located each one in each corner.
[0027] [0027]FIG. 3C shows a third embodiment of grid plate 3 . Four orifices 4 are shown in the area bounded by the walls of the flattened pipe or tubing 1 and two adjacent pitch divider fins 8 .
[0028] [0028]FIG. 3D shows a fourth embodiment of grid plate 3 . Eight orifices 4 are shown in the area bounded by the walls of the flattened pipe or tubing 1 and two adjacent pitch divider fins 8 . Four of orifices 4 are shown as squares. The orifices 4 can be round, square, elliptical or polygonal.
[0029] [0029]FIG. 4 is a cross-sectional view of the heat exchanger that is taken at a right angle to the flat surfaced pipe or tubing 1 that conveys one of the fluids involved horizontally. The small solid particles 2 are drawn as triangles to represent tetrahedrons (which is one of the preferred solid shapes). The flattened pipe or tubing 1 is firmly attached to bottom woven wire mesh or perforated sheet 6 which is shown as formed into flat-sided alternating ridges and groves. Note that there is no grid plate 3 required for this construction. The top woven wire mesh or perforated sheet 5 is held tightly against the tops of the flattened pipe or tubing 1 to keep the small solid particles 2 from falling out when the heat exchangers are handled. Note that the top woven wire mesh or perforated sheet 5 is now shown as being formed into rounded alternating ridges and groves which will result in less pressure drop through the heat exchangers when in service. The large dark arrows A that point up indicate the upward flowing fluid. Bubbles 7 are formed above the bottom woven wire mesh or perforated sheet 6 whenever more fluid is introduced than will pass through the spaces between the small solid particles 2 .
[0030] [0030]FIG. 5 is a cross-sectional view of the heat exchanger that is taken at a right angle to FIG. 4 as shown in FIG. 4. The side of the flattened pipe or tubing 1 that conveys the horizontally flowing fluid is shown as well as its fluid flow that is indicated by the large dark arrows B that point from left to right. The small solid particles 2 , the top woven wire mesh or perforated sheet 5 , the bottom woven wire mesh or perforated sheet 6 , and the bubbles 7 are shown again as shown in FIG. 4. Pitch divider fins 8 are shown as being provided for increased heat transfer surface even when the heat exchanger is not pitched for drainage.
[0031] [0031]FIG. 6A shows a shape of small solid particles having a tetrahedron that has all four equilateral triangles of the same size where the side lengths are all equal. FIG. 6B shows a tetrahedron that has four triangular faces that are not necessarily equal including the case where all four triangles could be of different dimensions. FIG. 6C shows a pyramid that has four triangles that are of equal dimensions and the base is a square. FIG. 6D shows a polyhedron that has a polygonal base with triangular sides that meet at a common vertex. The tetrahedron shown as FIG. 6A is expected to be the most used shape for the small solid particles to be manufactured.
[0032] According to the present invention as described above, the heat exchanger is reduced in size and exhibits much higher heat transfer rates when using the grid plate perforated with a plurality of orifices, the folded or shaped woven wire mesh or perforated sheets on the top and bottom of the heat exchanger, and tetrahedron or pyramid shaped small solid particles. The use of folded or shaped woven wire mesh or perforated sheets reduce the overall pressure drop within the heat exchanger when in service
[0033] Although the preferred embodiment of the present invention has been shown and described, it will be appreciated by those skilled in the art that changes may be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the claims and their equivalents.
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Heat exchangers utilizing flat surfaced passages to contact, contain and utilize fluidized small solid particles is provided. Top and bottom woven wire mesh or perforated sheet corrugated with rounded or flat-sided ridges are attached to respective top and bottom sides of said passage to increase its surface and to prevent said small solid particles from exiting said heat exchanger. A variety of shapes of the small solid particles are provided to further enhance the heat transfer rate. More energy efficient systems of all kinds will result from the use of these smaller heat exchangers.
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BACKGROUND OF THE INVENTION
1. Statement of the Technical Field
The inventive arrangements relate to directional networks that can cover terrestrial and airborne nodes over hundreds of nautical miles, and more particularly to long range TDMA time slot scheduling in peer-to-peer directional networks.
2. Description of the Related Art
Peer-to-peer mobile ad hoc networks (MANET) using directional antennas are known in the art. These MANET networks can use a variety of communications formats including Time Division Multiplexed Access (TDMA) arrangements. Further, they are characterized by independence from fixed infrastructures and by peer-to-peer distributed control mechanisms and protocols. In TDMA type MANET networks, each node can communicate during a specified time period or time slot. In order to coordinate such communications, each node can include a clock which is synchronized with a highly stable time reference. For example, this stable time reference can be derived from a satellite-based GPS signal. It should be noted that TDMA cellular systems often rely on synchronization to base stations to establish system timing and to compensate for propagation delay differences. Such TDMA cellular systems include, but are not limited to, global systems for mobile communications (GSM), Integrated Digital Enhanced Network (iDENs) systems, 802.16 based broadband wireless access network systems, and TDMA satellite communications (SATCOM) systems.
Still, each TDMA node can be expected to have a significant total time base uncertainty. Also, propagation delay between nodes can create additional timing uncertainties that change in real time as the mobile nodes move relative to one another. In order to manage these timing uncertainties, prior art systems use a base station infrastructure to create a hub and spoke typology. These base stations are usually, but not necessarily, fixed in location. The mobile nodes operate as “spokes” or “clients” to the basestation hubs and synchronize their transmissions to those base stations.
A MANET is an infrastructureless network that uses peer-to-peer control mechanisms and therefore does not have base stations to provide a central timing reference. Therefore, there is a need in a TDMA MANET for a new time synchronization method that can compensate for variable propagation delay and other propagation uncertainty in the absence of a central infrastructure.
In a TDMA MANTET, a transmitted RF burst is can be transmitted within a time slot as close to the beginning of the time slot as possible. The time slot length can be selected to exceed the maximum RF burst length by an amount of time referred to as the “guard time.” This guard time is used to accommodate any timing uncertainties at either the transmitter or receiver, and the maximum propagation time delay. If the range delay between the transmit node and the receive node exceeds the allocation in the guard time, a maximum length RF burst will spill over into the following time slot at the receiver. This spillover can cause interference if such following time slot is in use for communications as between other nodes.
Conventional MANET networks using TDMA generally choose a guard time which is based (at least in part) on the maximum permitted range between nodes. In this regard, networks which are designed to accommodate larger distances between nodes can require larger guard times. These larger guard times are necessary to accommodate potentially longer propagation delays between distant nodes. This approach can provide acceptable results for a limited network range. However, for networks operating over hundreds of nautical miles, the guard time can become relatively lengthy in duration. Such lengthy guard periods restrict the available time for other nodes to communicate with each other, leading to inefficiencies in the overall network. For example, a system which has 88% efficiency with an operating range of 11 nautical miles can have an efficiency of only 16% if the operating range is extended to 440 nautical miles.
In order to address this problem, several existing TDMA wireless systems have used range adjusted timing systems. However, such systems have generally only been applied in hub-spoke type networks. The problem becomes more considerably more complex in the case of ad-hoc peer-to-peer networks. Accordingly, a new approach is needed for ad-hoc peer-to-peer communications networks to facilitate TDMA communications which are capable of providing efficient communications over larger geographic areas.
SUMMARY OF THE INVENTION
The invention concerns a method and apparatus for scheduling time division multiple access (TDMA) communications among a plurality of nodes arranged to form a wireless ad hoc mobile network. The nodes communicate with each other using directional antennas and a TDMA scheduling process. The nodes have knowledge of the range between the transmitting node and other nodes within the radio line of sight of the transmitting node. The method includes a scheduling process for scheduling at least one transmit time slot during which a first one of the plurality of nodes transmits wireless data to a second one of the plurality of nodes. The scheduling process includes automatically selecting a candidate time slot for the transmit time slot. The scheduling process also includes determining whether transmissions during the candidate time slot will (1) cause interference with communications of any of the plurality of nodes that are located in a defined transmit antenna beam of the first node, or (2) be subject to interference when received at the second node as a result of transmissions from any of the plurality of nodes located in a defined receive antenna beam of the second node.
A data epoch is defined for the TDMA process. The data epoch includes a recurring time period which defines an overall timing cycle for the TDMA process. Each data epoch is sub-divided in time to form a plurality of mini-slots, each comprising a fractional duration of the data epoch. The scheduling process includes selecting the candidate time slot to have a duration which includes a plurality of M contiguous mini-slots. The scheduling process further includes automatically selecting the candidate time slot to include any contiguous group of M mini-slots contained within the data epoch.
The scheduling step further includes automatically selecting a receive time slot for the second node. The receive time slot length corresponds to the transmit time slot, but the arrival time is automatically adjusted in time to compensate for a propagation delay between the first node and the second node, which is directly known a priori or derived from prior knowledge of the range between the nodes. In this regard, the receive time slot can comprise a different contiguous group of mini-slots as compared to the transmit time slot. Significantly, the second node automatically determines the receive time slot exclusive of any centralized controller for the mobile ad hoc network. According to a preferred embodiment, the scheduling process is a distributed process which is cooperatively performed in a process which involves at least at the first node and the second node.
The scheduling step further includes automatically selecting an alternative candidate time slot. For example, the alternative candidate time slot will be selected if it is determined that transmissions from the first node to the second node during the initially selected candidate time slot will (1) cause interference with communications of any of the plurality of nodes that are located in the defined transmit antenna beam of the first node, or (2) be subject to interference when received at the second node as a result of transmissions from any of the plurality of nodes located in the defined receive antenna beam of the second node.
The method also includes a second scheduling step. The second scheduling step involves scheduling at least a second transmit time slot during which the second one of the plurality of nodes to transmit wireless data to the first one of the plurality of nodes. The second scheduling step also makes use of a distributed scheduling process. The second scheduling step includes automatically selecting a second candidate time slot for the second transmit time slot and determining whether transmissions during the second candidate time slot will (1) cause interference with communications of any of the plurality of nodes that are located within the radio line of sight of the second node, or (2) be subject to interference when received at the first node as a result of transmissions from any of the plurality of nodes located in a defined receive antenna beam of the first node. If the nodes use directional antennas, then this step includes a consideration of the antenna pattern and beam location when the potential to cause interference is evaluated.
The inventive arrangements also include an alternative method for scheduling time division multiple access (TDMA) communications among a plurality of nodes using directional antennas in a mobile ad hoc network. The alternative method includes arranging a plurality of nodes to form a wireless ad hoc mobile network. The nodes communicate with each other using directional antennas and a TDMA process. The method includes using a peer-to-peer distributed scheduling process. The distributed scheduling process includes automatically scheduling for each node at least one transmit time slot for transmitting wireless data to a neighboring one of the plurality of nodes. The method also includes automatically scheduling for each node a receive time slot for receiving signals transmitted from a neighboring one of the plurality of nodes during a respective one of the transmit time slots. Significantly, each of the receive time slots corresponds to a time of a respective one of the transmit time slots, but is automatically adjusted delayed in time to compensate for a propagation delay between nodes.
The scheduling step further includes automatically selecting at each node a candidate time slot for the transmit time slot and determining whether transmissions during the candidate time slot will (1) cause interference with communications of any of the plurality of nodes that are located in a defined transmit antenna beam of the node, or (2) be subject to interference when received at the neighboring node resulting from transmissions from any of the plurality of nodes located in a defined receive antenna beam of the neighboring node.
In the alternative embodiment, a data epoch is defined for the TDMA process. The data epoch includes a recurring time period which defines an overall timing cycle for the TDMA system. Each data epoch is sub-divided in time to form a plurality of mini-slots, each comprising a fractional duration of the data epoch. Significantly, the transmit time slot is selected to have a duration which includes a plurality of M contiguous mini-slots. The scheduling process further includes automatically selecting the transmit time slot to include any contiguous group of M mini-slots contained within the data epoch.
According to yet another embodiment, the invention includes a distributed system for scheduling time division multiple access (TDMA) communications among a plurality of nodes using any combination of omni or directional antennas in a mobile ad hoc network. The system includes a plurality of nodes arranged to form a wireless ad hoc mobile network that communicate with each other using directional antennas and a TDMA process. A processor for performing scheduling functions is provided at each node. The processor at each node cooperates with processors at other nodes to cooperatively schedule at least one transmit time slot during which a first one of the plurality of nodes transmits wireless data to a second one of the plurality of nodes. The processor is further configured to automatically select a candidate time slot for the transmit time slot. The processor cooperates with at least one other processor in another node to determine whether transmissions during the candidate time slot will (1) cause interference with communications of any of the plurality of nodes that are located in a defined transmit antenna beam of the first node, or (2) be subject to interference when received at the second node resulting from transmissions from any of the plurality of nodes located in a defined receive antenna beam of the second node.
The TDMA process includes a data epoch comprising a recurring time period which defines an overall timing cycle for the TDMA process. Each data epoch is sub-divided in time to form a plurality of mini-slots, each comprising a fractional duration of the data epoch. The processor in each node that is used for scheduling processing is configured for selecting the candidate time slot to have a duration which includes a plurality of M mini-slots. Notably, the processor is configured to automatically select the candidate time slot to include any contiguous group of M mini-slots contained within the data epoch.
The processor at each node is also configured to automatically select a receive time slot for the second node corresponding to a time of the transmit time slot, wherein the receive time slot is automatically adjusted in time to compensate for a propagation delay between the first node and the second node. Significantly, the processor used for scheduling at the second node automatically determines the receive time slot exclusive of any centralized controller for the mobile ad hoc network. The receive time slot includes a different contiguous group of mini-slots as compared to the transmit time slot.
The TDMA process includes a “neighbor database” at each node that maintains knowledge of the location of or equivalently the relative range and angles between the plurality of nodes within the radio line of sight of the first node. The neighbor database also includes knowledge of the currently scheduled transmit and receive timeslots at the plurality of nodes included in the neighbor database.
The TDMA process includes a method for populating the database of node locations of the plurality of nodes. Those skilled in the art will appreciate that there are numerous methods available to populate a database with this information. The methods include broadcast or multicast transmissions between the nodes or downloads from an external source.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a drawing that is useful for understanding timing problems which occur in mobile ad hoc networks.
FIG. 2 is a timing diagram that is useful for understanding timing problems which occur in mobile ad hoc networks.
FIG. 3 is a timing diagram that is useful for understanding timing problems which occur in mobile ad hoc networks.
FIG. 4 is a block diagram of a wireless mobile node that can be used to implement the present invention.
FIG. 5 is a timing diagram that is useful for understanding a timing relation between data epochs, mini-slots, and time slots.
FIG. 6 is a drawing that shows a planar geometry of several nodes which is useful for understanding the invention.
FIG. 7 is a timing diagram that is useful for understanding potential sources of interference in FIG. 6 .
FIG. 8 is a drawing that shows the planar geometry of several nodes in FIG. 6 with different antenna pattern overlays.
FIG. 9 is a timing diagram that is useful for understanding potential sources of interference in FIG. 8 .
FIG. 10 is a flowchart that is useful for understanding an interaction among various nodes in a mobile ad hoc network.
FIG. 11 is a flowchart that provides additional detail relating to step 1016 in FIG. 10 .
FIG. 12 is a flowchart that provides additional detail relating to step 1102 in FIG. 11 .
FIG. 13 is a flowchart that provides additional detail relating to step 1106 in FIG. 11 .
FIG. 14 is a flowchart that provides additional detail relating to step 1210 in FIG. 12 .
FIG. 15 is a flowchart that provides additional detail relating to step 1308 in FIG. 13 .
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
Conventional approaches to peer-to-peer, ad-hoc TDMA communication networks are based on knowing only the maximum range between nodes. This concept is illustrated in FIGS. 1-3 . FIG. 1 shows a two-dimensional layout of a group of nodes in a prior art TDMA based mobile ad hoc network (MANET). In FIG. 1 , the transmitting node is node 102 . In this example, the system has a guard time that is designed to accommodate maximum range indicated by the radius of the circle 103 . Nodes 104 are within this radius. Node 106 - 1 is outside this radius. Node 106 - 2 is further outside the radius as compared to node 106 - 1 .
Referring now to FIG. 2 there is shown a conventional time slot 200 . The time slot has a duration 201 , a maximum RF burst time 202 , and a guard time 203 . The guard time is provided to accommodate range uncertainty as well as other timing uncertainties at the receiver and transmitter. An RF burst 206 is shown within the maximum burst time 202 . Referring again to FIG. 1 , it can be understood that transmissions from node 102 to node 106 - 1 or 106 - 2 , which are of the maximum RF burst length, will contaminate the following (or later) time slot for node 106 - 1 , 106 - 2 because these nodes are each located beyond the radius of the maximum range circle 103 .
An alternative illustration of the foregoing concept is provided in FIG. 3 . The transmit RF burst 206 of maximum length is shown in time slot n. At a node 104 the RF burst 206 arrives within slot n because node 104 is within the maximum guard time protected range. When RF burst 206 is received at a node 106 - 1 (beyond maximum protected range) the transmission will cause interference for node 106 - 1 in time slot n+1. At a more distant node 106 - 2 , the transmission will cause interference in time slot node n+2. As will be appreciated by those skilled in the art, transmitted RF bursts 206 that are not of maximum length may or may not contaminate the following time slot(s).
In FIGS. 1-3 , the length of the guard period 203 can be defined so that it comprises a greater portion of the total time 201 comprising time slot 200 . Increasing the length of time of the guard period in this way can allow more distant nodes, such as nodes 106 - 1 , 106 - 2 to receive the RF burst 206 within the guard period for a time slot n. Thus, if it is known that the network must cover a larger area, a longer guard period can be selected. However, it will be appreciated that increasing the guard period in this way will decrease the time available for the RF burst 206 . This has the undesirable effect of reducing efficiency.
The invention will now be described more fully hereinafter with reference to accompanying drawing FIGS. 4-15 , in which illustrative embodiments of the invention are shown. This invention, may however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein.
In order to overcome the deficiencies of the prior art, an embodiment of the invention includes a peer-to-peer TDMA type mobile ad hoc network comprised of a plurality of individual nodes. The individual nodes communicate with each other within an ad-hoc network environment. Significantly, information concerning the range between node pairs is estimated and exploited. Consequently, the scalability, latency, and efficiency of the TDMA communication system can be significantly enhanced.
The inventive arrangements advantageously include a distributed long range scheduler function as part of each node. The distributed long range scheduler determines specific times when node pairs can communicate so as to avoid interfering with one another. Heuristics produce an efficient distributed schedule for communication between node pairs. This schedule is advantageously based on information which includes both node range and angle (i.e. direction). Accurate time references are provided at each node and nodes exchange position estimates so that each node can maintain an estimate of range to its various neighbors. Further, unlike conventional arrangements which provide a time axis measured in fixed time slots per epoch, the inventive arrangements make use of a plurality of mini-slots. A plurality of mini-slots can be arbitrarily selected to define a time slot which is thereafter used for communications from one node to another node. The time slot is independently evaluated by each node to determine whether its use will cause interference with neighboring nodes. Each node independently adjusts its schedule to account for the link delay. Further, transmit and receive time slots are scheduled separately to allow for more efficient use of available time.
Referring now to FIG. 4 , there is provided a simplified block diagram for a wireless mobile node 404 that is useful for understanding the present invention. The wireless mobile node can be used in a wireless communication network as described herein. The wireless mobile node 404 is comprised of a directional antenna 405 , a transceiver 406 , and a control unit 408 . The wireless mobile node 404 can optionally include an omni-directional antenna 402 .
The transceiver 406 , the omni-directional antenna 402 and the directional antenna 405 collectively enable wireless communications between the wireless mobile node 404 and a plurality of other nodes having a similar configuration in the network. In this regard, it should be appreciated that the omni-directional antenna 402 is configured to send and/or receive signals in any direction. The directional antenna 405 is configured to selectively send and/or receive signals in a desired direction. The directional antenna 405 can include, but is not limited to, a phased array antenna. The omni-directional antenna 402 and directional antenna 405 are coupled to the transceiver 406 so that RF signals can be communicated to and from each of these antennas. In an alternative embodiment, the omni-directional antenna 402 can be omitted and omni-directional communications can be provided by scanning a directional antenna beam through a wide range of azimuth and elevation angles.
The transceiver 406 can include conventional RF circuitry (not shown) and a modem (not shown) for receiving and transmitting RF signals. The transceiver 406 is electrically connected to the unit 408 so that received signals demodulated by the transceiver 406 can be communicated to the control unit 408 . Similarly, baseband digital data and control signals can be communicated from the control unit 408 to the transceiver 406 .
The control unit 408 is comprised of processor 410 , antenna control unit 412 , a clock 414 , and node position unit 416 . The antenna control unit 412 can control a direction of an antenna beam associated with the directional antenna 405 . The antenna control unit 412 can optionally be included as part of the transceiver 406 . Clock 414 provides a highly accurate and stable time reference for each node. The accuracy of the clock 414 can be maintained by any suitable means. For example, a GPS timing signal can be used for this purpose. As will be appreciated by those skilled in the art, GPS timing signals can provide a highly accurate time reference. Thus, clock 414 can be synchronized with clocks of other wireless mobile nodes forming part of the network described herein. The clocks are preferably synchronized to within a fractional portion of a mini time-slot (described below in greater detail). According to one embodiment, the time references can advantageously be selected so that a clock 414 associated with each wireless mobile node 404 is synchronized to within 100 nanoseconds of other nodes in the network. Still, the invention is not limited in this regard.
The control unit 408 also includes a node position unit 416 . The node position unit 416 is configured to allow the wireless mobile node 404 to identify its position. For example, the node position unit 416 can advantageously include a GPS receiver and GPS processing circuitry suitable for allowing the wireless mobile node 404 to precisely locate its position at any terrestrial or airborne location. If a GPS receiver is used, the GPS timing data can be used as described above to aid in synchronizing the clocks 414 in each of the wireless mobile nodes 404 .
The control unit 408 also includes a memory device 450 . The memory device 450 stores several different types of information. For example, the memory device 450 can includes a neighbor information table 420 , epoch schedule 422 , a receive (Rx) interference profile 424 , a transmit (Tx) interference profile 426 , and a neighbor time-slot usage profile 428 . The various types of information stored in memory device 450 will be discussed below in greater detail. The various components forming the control unit 408 can communicate with each other by means of a suitable data bus 418 .
Those skilled in the art will appreciate that the architecture described herein for wireless mobile node 404 is one possible example of a wireless mobile node which can be used with the present invention. However, it should be understood that the invention is not limited in this regard. Instead, any other suitable wireless mobile node architecture can also be used without limitation.
An overview of the basic operation of wireless mobile network utilizing a plurality of wireless mobile nodes 404 according to the inventive arrangements will now be provided. According to an embodiment of the invention, individual network nodes 404 use a neighbor discovery process. The neighbor discovery process includes an exchange of position information so that each node has the coordinates of neighboring nodes. This position information allows the range information and relative direction of such neighbor nodes to be calculated. Range information and direction information is used for purposes of performing interference calculations. Interference calculations also include consideration of propagation delays between nodes and required antenna beam pointing directions based on the known node locations.
The present invention is unlike conventional MANET systems that utilize conventional TDMA technology. In such conventional TDMA systems, periods of time are divided into epochs, and communication between nodes occurs in time slots which are sub-portions of each epoch. Significantly, each time slot in a conventional system will have a fixed timing position in each epoch. Nodes in the ad hoc network which need to communicate are assigned time slots for such communications. However, this fixed timing creates problems for long range communications.
The present invention also divides time into a series of epochs. However, the timing of the time slots used for communications between nodes is not fixed. State differently, it can be said that the timing position of each time slot is not fixed within each epoch. In the present invention, the position of time slots within each epoch can be arbitrarily selected by the nodes in accordance with an algorithm. The algorithm is selected for minimizing potential interference among neighbor nodes.
In order to allow for time slots to have timing positions which are arbitrarily defined within an epoch, the present invention introduces the concept of mini-slots, which are some fraction of the duration of a time slot. For example, each mini-time slot can have a duration which is ⅛ of the duration of a time slot. This concept can be better understood with reference to FIG. 5 . In FIG. 5 , there is shown a timing diagram 500 for a TDMA type mobile ad hoc network according to the inventive arrangements. The timing diagram shows a series of data epochs 504 which are fixed divisions of time. Each epoch 504 is sub-divided into a plurality of N mini-slots 506 . According to an embodiment of the invention, a time slot 508 can be comprised of contiguous groups of M mini-slots. For example, each time slot 508 can be comprised of 8 mini-slots 506 (M=8). Each time slot 508 can have an arbitrarily defined starting position (subject to interference calculations) that corresponds to a starting time of any selected mini-slot.
In order to understand how time slot timing, range, direction and propagation information is used to mitigate interference, an example is useful. FIG. 6 shows a planar geometry of several nodes where node 404 2 (the transmitting node) is attempting to schedule a transmit time slot consisting of five mini-slots (M=5) with node 404 4 (the receiving node). In FIG. 6 , the transmit beam pattern 602 is shown for node 2 . Nodes 404 4 , 404 6 , 404 7 and 404 9 are located within range and in the beam pattern. A time slot scheduler can be used to automatically select a timing position for a transmit time slot that will minimize interference to neighboring nodes.
The scheduler process begins by selecting a candidate set of mini-slots which will define the position of the transmit time slot for node 404 2 . FIG. 7 is a timing diagram 700 which shows the time base at nodes 404 2 , 404 4 , 404 6 , 404 7 and 404 9 . It is assumed that clocks 414 at the nodes 404 1 - 404 9 are synchronized to fractions of a mini-slot.
The timing diagram shows that a candidate set of mini-slots MT 2 -MT 6 can be selected at node 404 2 which define a possible timing position for time slot 702 . In order to determine whether this timing position will cause interference with neighboring nodes, the timing position of time slot 702 is mapped to the corresponding time intervals at nodes 404 4 , 404 6 , 404 7 and 404 9 . These corresponding time intervals 704 , 706 , 707 , 709 are offset from time slot 702 because of the propagation delay “d” between the nodes. Propagation delay can be determined if the transmitting node 404 2 knows the relative position of neighbor nodes 404 6 , 404 7 and 404 9 . The corresponding time interval for the receiver node 404 4 , is 704 . The corresponding time intervals mapped to the location of nodes 404 6 , 404 7 and 404 9 are respectively 706 , 707 , 709 . Time intervals 706 , 707 , 709 represent the time intervals at nodes 404 6 , 404 7 and 404 9 during which the signal will arrive from node 404 2 if transmitted during time slot 702 .
It should be understood that during the time intervals 706 , 707 , 709 , a transmitted signal from node 404 2 will cause interference at nodes 404 6 , 404 7 and 404 9 if the antenna beams of these nodes are pointed in the direction of transmitting node 404 2 . For example, it can be observed that transmitting node 404 2 can be within a receive antenna beam 606 of node 404 6 during a transmit time interval. Notably, transmitting node 404 2 can advantageously be provided with position and timing schedule for neighbor nodes to determine the direction in which its neighbor node antennas are pointing during each mini-slot. If transmitting node 404 2 determines that any one of nodes 404 6 , 404 7 and 404 9 are in fact scheduled to receive signals (1) from a direction which coincides with transmitting node 404 2 , and (2) such signals are scheduled to be received during the intervals 706 , 707 , 709 , then it can conclude that the transmissions from node 404 2 during time slot 702 will cause interference. If transmitting node determines that interference will occur, then a different candidate time slot 702 is advantageously selected.
If node 404 2 determines that time slot 702 will not cause interference to the receivers of nodes 404 6 , 404 7 and 404 9 then a second analysis can be performed. This second analysis can determine whether any nodes in the antenna beam of receiver node 404 4 will be transmitting in the direction of node 404 4 during the time interval corresponding to time slot 702 (as adjusted for propagation delay). This analysis is shown in FIGS. 8 and 9 . FIG. 8 shows a planar geometry 800 which is similar to the one shown in FIG. 6 . However, in FIG. 8 , nodes 404 6 , 404 7 and 404 9 are omitted for greater clarity since they are not part of this analysis. It can be observed in FIG. 8 that nodes 404 1 , 404 2 , 404 3 and 404 5 are located within the range and in the receiver beam pattern 812 of node 404 4 .
FIG. 9 shows a timing diagram which includes segment of the time base at several nodes 404 1 - 404 5 . It is assumed that clocks 414 at the nodes 404 1 - 404 4 are synchronized to fractions of a mini-slot. In FIG. 9 , the timing position of time interval 704 is mapped to the corresponding time intervals at nodes 404 1 , 404 3 , and 404 5 . These corresponding time intervals 901 , 903 , 905 are offset from time slot 704 because of the propagation delay “d” between the nodes. FIG. 9 shows that node 404 4 will experience interference during time interval 704 if nodes 404 1 , 404 3 , or 404 5 transmit toward node 404 4 during time periods 901 , 903 , or 905 . If node 404 4 has transmission schedules and position information for nodes 404 1 , 404 3 , or 404 5 then it can determine whether time interval 704 is an acceptable receive time for node 404 4 . In the same way, node 404 4 can determine whether time interval 702 is an acceptable transmit time slot for node 404 2 .
The flowcharts in FIGS. 10-14 will now be used to explain how the concepts discussed above in relation to FIGS. 6-9 can be applied in a mobile ad hoc network. FIG. 10 provides a basic overview of a mobile ad hoc network process 1000 . It will be understood that the scheduler process described in relation to FIGS. 6-9 requires detailed information regarding the identification, position, and communication schedule of neighbor nodes. Process 1000 is useful for understanding how such information is exchanged. Still, it should be understood that the process 1000 merely discloses one possible process for exchange of such data and the invention is not intended to be so limited. Instead, any other process for exchanging node identification, position, and communication schedule can be used. Further, it should be understood that all of the foregoing information can be exchanged using one or more control channels. For example, one or more mini-slots can be defined as control channels which are reserved for exchange of such information.
The process 1000 begins in step 1002 and continues with step 1004 . In step 1004 , nodes in a network engage in a neighbor discovery process. Neighbor discovery processes in mobile ad hoc networks are generally well known. Accordingly, the details of this process will not be described here. However, it should be understood that the neighbor discovery process involves transmission of “hello” messages to neighboring nodes using a control channel. The “hello” message can be broadcast to neighboring nodes by any suitable means. For example, the “hello” message can be transmitted by using an omni-directional antenna 402 or a scanned beam provided by directional antenna 404 .
The “hello” message can include node identifier information and a position report for the node which transmits the message. Each node determines its own position using the node position unit 416 . Each node also collects identifying information and position information from its neighbors using these “hello” messages.
In step 1006 , information derived from the neighbor discovery process in step 1004 is used to populate (and/or update) neighbor information tables at each node. For example, node identification and position information can be stored in a neighbor information table 420 . Each node further maintains an epoch schedule 422 which provides timing information for the occurrence of each data epoch 504 . Timing of mini-slots 506 can also be derived from the epoch schedule 422 .
The network process 1000 continues with step 1008 in which each node periodically communicates to its neighbors a transmit schedule for that node. In step 1010 , each node also periodically broadcasts to its neighbors a receive schedule for that node. In step 1012 , each node stores neighbor transmit and receive information in the table in FIG. 4 identified as the neighbor time slot usage profile 428 .
The process continues in step 1014 in which each node uses processor 410 to apply topology control rules to the information stored in its neighbor information table 420 . The topology control rules can be stored in memory device 450 . The topology control rules are used to select one or more neighbor nodes with which communication links should be established. Topology control rules for mobile ad hoc networks are well known in the art and therefore will not be described here in detail. However, it should be understood that such topology control rules can allow a node to determine whether communication links with various neighbor nodes should be established, maintained, or terminated.
In step 1016 , new communication links are formed with selected neighboring nodes as determined by the topology control rules. This process of forming links with new nodes will be described in more detail in relation to FIGS. 11-14 . In step 1018 , certain communication links are terminated with selected neighbor nodes as determined by topology control rules. In step 1020 , a determination is made as to whether the network process should be terminated for any reason. If so, then the process terminates in step 1022 . Alternatively, the process continues with step 1004 and repeats.
FIG. 11 shows a series of steps which provide further detail concerning step 1016 in FIG. 10 . Step 1016 involves one node forming a communication link with a selected neighbor node. Establishing this communication link begins with selection of a suitable time slot when a first node (transmitter node) will transmit data to a second node (receiver node).
As shown in FIG. 11 , step 1016 includes a series of steps which can begin with step 1102 . Step 1102 includes using a scheduler process at the transmitter node to generate a list of candidate transmit time slots for transmissions from the transmitter node to the receiver node. The scheduler process can be performed by processor 410 executing a programmed set of instructions. Alternatively, the scheduler process can be implemented as any other combination of hardware and software. Step 1102 is described in greater detail in FIG. 12 . In general, however, the list of candidate time slots can be generated using an interference analysis similar to that described in relation to FIGS. 6-7 . In this regard it may be noted that in FIGS. 6 and 7 the transmitter node was node 404 2 and the receiver node was 404 4 .
In step 1104 , the list of candidate transmit time slots can be communicated from the transmitter node to the receiver node. Any suitable means can be used for communicating this candidate transmit time slot list from the transmitter node to the receiver node. For example, a dedicated control channel can be used for this purpose. Still, the invention is not limited in this regard.
In step 1106 , the candidate transmit time slot list is received and used at the receiver node to determine which of the proposed candidate time slots are acceptable. Step 1106 is described in greater detail in FIG. 13 . In general, however, acceptable candidate time slots can be determined using a process similar to that previously described in relation to FIGS. 8-9 . Following steps 1106 , the receiver node will now be aware that transmitter node wishes to establish a transmit time slot for communications to receiver node. Consequently, the receiver node can initiate another process similar to that described in step 1016 for the purpose of establishing a transmit time slot for communications from the receiver node to the transmitter node. To avoid redundancy, that process will not be described here.
Continuing on now with step 1108 , a message can be sent from the receiver node to the transmitter node. The message identifies those transmit time slots proposed by the transmitter node which are determined to be acceptable to the receiver node. In step 1110 , this message is received at transmitter node. The process continues on to step 1112 in which the receiver node begins listening for transmissions from the transmitter node during the time slot which has been accepted by the transmitter node. In step 1114 data transmissions can begin from the transmitter node to the receiver node using the time slot that has been selected. Thereafter, the process can continue on to step 1018 as previously described.
Referring now to FIG. 12 , there is provided a more detailed description of the processes associated with step 1102 in FIG. 11 . Step 1102 involves using a scheduler process at the transmitter node to generate a list of candidate transmit time slots for transmissions from the transmitter node to the receiver node. As an aid to understanding, step 1102 will be described with reference to FIG. 5 .
The process can begin with step 1202 in which the scheduler process at the transmitter node selects a candidate transmit time slot beginning at mini-slot n and comprised of M mini-slots that are contiguous with each other. For example, in FIG. 5 a candidate time slot can be time slot 508 which begins at mini-slot 4 and continues through mini-slot 11 (M=8). In step 1204 , the scheduler process checks the transmitter node's transmit and receive schedule to determine whether any of the M mini-slots comprising the candidate time slot is already in use at the transmit node (for receiving or transmitting). The transmitter node's transmit and receive schedule can be stored in memory 450 . If any of the M mini-slots are currently in use, then the candidate time slot is not acceptable and the process continues to step 1206 . In step 1206 , the value of n is incremented and the step 1204 is repeated with a different set of M mini-slots. For convenience, the value of n can be incremented by 1. However, the invention is not limited in this regard. For example, the value of n could be incremented by M or any other value.
In step 1204 , if none of the M mini-slots are currently in use at the transmitter node, then the process continues on to step 1208 . In step 1208 , the scheduler process determines whether any of the M mini-slots are in use at the receiver node. Information concerning time slot usage at the receive node can be obtained from the neighbor time slot usage profile 428 which is stored in memory device 450 . If any of the time slots are currently in use at the receiver node, the process can return to step 1206 where the value of n is incremented to select a different set of M mini-slots. Alternatively, if the M mini-slots are not in use at the receiver node, then the process continues on to step 1210 .
In step 1210 , the scheduler process in the transmitter node determines whether the transmitter node's use of the M mini-slots associated will cause interference to neighboring nodes located in the transmit beam of the transmitter node (when pointed toward the receiver node). This process for mitigating interference is described below in more detail in relation to FIG. 14 . If the scheduler process determines that use of the M mini-slots by the transmitter node will cause interference to neighboring nodes, then the process returns to step 1206 and an alternative set of mini-slots is selected for evaluation. Conversely, if the scheduler process determines that use of the M mini-slots by the transmitter node will not cause interference to neighboring nodes, then the process continues on to step 1212 .
In step 1212 , the candidate time slot comprised of the M mini-slots is added to a list of candidate time slots which can be used. Thereafter, in step 1214 , a determination is made as to whether the candidate transmit time slot list is complete. This determination can be based on any one of several considerations. For example, the list can be deemed complete when a predetermined number of candidate transmit time slots have been identified. Alternatively, the list can be complete when all possible candidate time slots have been considered.
Referring now to FIG. 14 , there is provided a more detailed description of the process associated with step 1210 in FIG. 12 . It may be recalled from the discussion regarding FIG. 12 , that step 1210 generally involves a scheduler process at the transmitter node. The scheduler process is used to evaluate potential interference caused by the transmitting node's use of the M mini-slots associated with the candidate time slot. In particular, this scheduler process determines whether the transmissions by the transmitter node during the candidate time slot, using an antenna beam pointing toward the receiver node, will cause interference to other neighboring nodes that are also located in the transmit beam. As an aid in understanding, the process will be described with reference to FIGS. 6 and 7 in which node 404 2 is considered the transmitter node and node 404 4 is considered to be the receiver node.
The process in FIG. 14 begins with step 1402 in which the transmitter scheduler at the transmitter node determines a direction that it's transmit beam will be pointed for the purpose of communicating with the receiver node. In the context of FIGS. 6 and 7 , this means that the node 404 2 will determine which direction its antenna beam 602 should point for communications with node 404 4 . Once the direction of the transmitter beam has been determined in step 1402 , the scheduler process at the transmitter node ( 404 2 ) will determine in step 1404 whether there are any neighbor nodes that are contained within the transmit beam. If not, then it can be assumed that the transmitter node's use of the M mini-slots will not cause interference to any other nodes and the process will continue on to step 1412 .
Alternatively, if it is determined in step 1404 that there are neighbor nodes contained within the transmit beam, then the process continues on to step 1406 . For example, in FIG. 6 nodes 404 6 , 404 7 , 404 9 are in the transmit beam 602 (in addition to node 404 4 ). In step 1406 the scheduler process determines whether there are any neighbor nodes in the transmit beam that are scheduled to be receiving during the candidate transmit time slot as adjusted for propagation delay. This concept is illustrated in FIG. 7 . In step 1406 , the transmitter scheduler would determine whether any of the nodes 404 6 , 404 7 , 404 9 are scheduled to be receiving during time intervals 706 , 707 , 709 . If not, then it can be assumed that no interference will occur and the scheduler process continues on to step 1412 . Otherwise, the scheduler process goes on to step 1408 .
In step 1408 , a determination is made as to whether any of the receive beam of the neighbor nodes is pointing toward the transmitter during the candidate transmit time (adjusted for propagation delay). In the context of FIG. 7 , this would mean determining whether the antenna beams of any of the nodes 404 6 , 404 7 , 404 9 are pointing toward the transmitter node 404 2 . In FIG. 6 , it can be observed that antenna beam 606 of node 404 6 is pointing toward the transmitter node 404 2 during time interval 706 . In this example, the scheduler process would continue on to step 1410 and determine that the transmitter node's use of the M mini-slots associated with a particular candidate time slot will cause interference to the other nodes located in the transmit beam. The process would then continue on to step 1206 in FIG. 12 . Alternatively, the scheduler process continues to step 1412 and determine that the transmitter node's use of the M mini-slots will not cause interference. From step 1412 , the process continues on to step 1212 where the candidate time slot is added to the candidate time slot list.
It may be recalled from FIG. 11 that once a suitable list of candidate transmit time slots has been compiled in step 1102 , this list is communicated to the receiver in step 1104 . Thereafter, in step 1106 the scheduling process at the receiver determines which, if any, of the candidate time slots are acceptable. Step 1106 will now be described in further detail with reference to FIG. 13 . The process can begin in step 1302 when the receiver scheduler receives the list of candidate transmit time slots at the receiver node. The process continues on to step 1304 in which the receiver scheduler selects the first candidate time slot on the list for evaluation.
The evaluation process begins in step 1306 with the receiver scheduler process at the receiver node determining whether the M mini-slots corresponding to the candidate transmit time slot are still idle and are therefore available. This step is somewhat redundant because a similar check is performed in step 1208 . However, it will be appreciated that the transmit and receive schedule at the receiver node will often contain scheduling information for the receiver mode that is more current than the corresponding information for the receiver node that is stored in at the transmitter node. Accordingly, step 1306 is a useful verification that the M mini-slots are still idle.
If the M mini-slots are determined to be no longer idle, then the process continues on to step 1312 where the receiver scheduler process determines whether there are any more candidate transmit time slots on the candidate transmit time slot list. Alternatively, in step 1306 , if the M mini-slots associated with a candidate time slot are in fact available, then the process continues on to step 1308 .
In step 1308 , the receiver scheduler process at the receiver node determines whether the receiver node will experience interference from network nodes other than the transmitter node. Step 1308 is described in greater detail in relation to FIG. 15 . However, it should be understood that the receiver scheduler process in step 1308 determines whether the receiver node will experience interference from other neighboring nodes during the M mini-slots corresponding to the candidate transmit time slot (as adjusted in time to compensate for propagation delay). If, in step 1308 , the receiver scheduler process determines that no interference will result from neighboring nodes, then the process continues on to step 1108 in FIG. 11 . In step 1108 , a message is sent to the transmitter node indicating that the candidate time slot is acceptable to the receiver node. Alternatively, if the receiver scheduler process determines that the receiver node will experience interference from other neighboring nodes, then the process continues on to step 1312 .
In step 1312 , the receiver scheduler process determines whether there are any other candidate time slots on the candidate time slot list. If so, then the receiver scheduler process continues on to step 1316 where the next candidate time slot is selected. Alternatively, if there are no more candidate time slots on the list, the receiver scheduler process continues on to step 1314 in which the receiver node notifies the transmitter node that none of the candidate time slots are acceptable. The receiver scheduler process then returns to step 1102 in FIG. 11 , where a new list of candidate time slots is generated at the transmitter node.
Referring now to FIG. 15 , the processes associated with step 1308 will now be described in greater detail. The process in FIG. 15 begins with step 1502 in which the scheduler process at the receiver node determines a direction that it's receive beam will be pointed for the purpose of receiving communications from the transmitter node. In the context of FIGS. 8 and 9 , this means that the node 404 4 will determine which direction its receiver antenna beam 812 will need to point towards for communications with node 404 2 . Once the direction of the receiver antenna beam 812 has been determined in step 1502 , the scheduler process at the receiver node ( 404 4 ) will determine in step 1504 whether there are any neighbor nodes that are contained within the receiver antenna beam 812 .
If it is determined in step 1504 that there are no neighbor nodes contained within the receiver antenna beam 812 , then the process continues in step 1512 . In step 1512 , the scheduler process determines that the receiver node 404 4 will not experience interference from other transmitting nodes during the time interval corresponding to the M mini-slots (as adjusted for propagation delay). Accordingly, the process will thereafter continue on to step 1108 in FIG. 11 .
Alternatively, if it is determined in step 1504 that there are neighbor nodes contained within the receiver antenna beam 812 , then the process continues on to step 1506 . For example, in FIG. 8 nodes 404 1 , 404 3 , 404 5 are in the receiver antenna beam 812 (in addition to node 404 2 ). Accordingly, the process would continue on to step 1506 in the example shown in FIG. 8 .
In step 1506 the scheduler process at the receiver node determines whether transmitted signals from any neighbor nodes in the receiver beam 812 can potentially be received at the receiver node 404 4 during any of the mini-slots corresponding to the time interval 704 . This concept is illustrated in FIG. 9 . Recall that time interval 704 is the period of time during which a transmission from transmitter node 404 2 will actually be received at receiver node 404 4 (assuming that the signal is transmitted from node 404 2 during time slot 702 ). Similarly, time intervals 901 , 903 , 905 represent those transmission time intervals for nodes 404 1 , 404 3 , 404 5 that will result in signals actually being received at receiver node 404 4 during time interval 704 .
In step 1506 , if none of the nodes 404 1 , 404 3 , 404 5 are actually scheduled to be transmitting during the time periods 901 , 903 , 905 , then it can be concluded that no interference will be caused at the receiver node 404 4 during time interval 704 . In that case, the transmit time slot 702 would be an acceptable time slot during which node 404 2 can transmit to node 404 4 , and the scheduler process continues on to step 1512 . Conversely, if any of the nodes 404 1 , 404 3 , 404 5 are actually scheduled to be transmitting during the time periods 901 , 903 , 905 , then such transmissions can potentially cause interference at the receiver node 404 4 during time interval 704 . In that case, the transmit time slot 702 may not be an acceptable time slot during which node 404 2 can transmit to node 404 4 . Accordingly, the scheduler process will continue on to step 1508 .
In step 1508 , a determination is made as to whether an antenna beam of any neighbor nodes that is actually pointed toward the receiver 404 4 during a time interval when the receiver is expecting to receive signals from the transmitter node. In the context of FIG. 9 , this would mean determining whether the antenna beams of any of the nodes 404 1 , 404 3 , 404 5 are pointing toward the receiver node 404 4 during time intervals 901 , 903 , 905 . If so, then the scheduler continues on to step 1510 where it determines that other transmitters will cause interference to the receiver if the transmitter node uses the M mini-slots associated with a candidate transmit time slot such as slot 702 . Following step 1510 , the scheduler process at the receiver node continues on to step 1312 in FIG. 13 . In step 1312 the scheduler process checks to see if other candidate time slots are available and continues on as described above.
The invention described and claimed herein is not to be limited in scope by the preferred embodiments herein disclosed, since these embodiments are intended as illustrations of several aspects of the invention. Any equivalent embodiments are intended to be within the scope of this invention. Indeed, various modifications of the invention in addition to those shown and described herein will become apparent to those skilled in the art from the foregoing description. Such modifications are also intended to fall within the scope of the appended claims.
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Method and apparatus for scheduling time division multiple access (TDMA) communications among a plurality of peer nodes arranged to form a wireless ad hoc mobile network. The peer nodes communicate with each other using directional antennas and a TDMA process. The method includes a scheduling process for scheduling at least one transmit time slot during which a first one of the plurality of peer nodes transmits wireless data to a second one of the plurality of peer nodes.
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BACKGROUND OF THE INVENTION
[0001] 1. Field of the Invention
[0002] The present invention relates generally to market research service and more specifically to the methods and systems for collecting perception data points related to a given item from a set of respondents by offering an incentive that benefits the respondent or respondents who submit data points that match most closely to a calculated value of the data points collected.
[0003] 2. Description of the Related Art
[0004] In general, market research plays an important role in understanding the wants, needs and behaviors of the market place, both in the current and future trends. Market research is often applied in business-to-business and business-to-consumer applications. The implementation of a market research program requires a significant amount of investment in money, time and resources. When someone requires a better understanding of the market place, they will obtain information using an in-house market research service, third party market research service, or both.
[0005] There is a need to simplify a complex, time-consuming and potentially expensive process of recruiting individuals or companies and assigning them to surveys. This is a long existing problem in all areas of market research. In an effort to increase participation and response rate by respondents, incentives consistently exert positive effect on response rates in surveys.
[0006] It may not be feasible to award each respondent with incentives as this method may make it very expensive to do a market research. One way to minimize the cost of incentives and encourage participation in surveys is to offer the chance to win prizes for the respondents. While response rates may be higher than survey methods with no incentive, there is a problem in that various survey methods with incentives may not get respondents interested in providing accurate perception data points. There is a need for a market research method that get respondents interested in providing accurate data points in surveys and awarding an incentive to those who submit data points that match most closely to a calculated value (e.g. average) of the data points collected.
[0007] Furthermore, there is a need for a market research service provider to give greater convenience and control for an initiator of the service over how much incentive to supply thus the cost of doing market research.
[0008] There are services that provide, for example, pricing reports of commodity items. Such services may lack flexibility in researching specialty items or providing accurate and up-to-date reports for a local market or dynamic industry. For example, a service like Kelly Blue Book may not be able to give an accurate pricing report for a specific model that has been individually modified, has a special attribute, or faces changing demand of a local market. It is generally accepted that local professionals in related industries (e.g., car dealership) will be more likely to give accurate perceived value of an item to be surveyed. There is a need for a service that offers considerably greater information and convenience to a prospective market research initiator who needs to obtain timely survey data that may take advantage of local or industry related knowledge.
SUMMARY OF THE INVENTION
[0009] The present invention relates generally to methods for collecting accurate perception data points related to a given item from a set of respondents by offering an incentive that benefits the respondent or respondents who submit data points that match most closely to a calculated value of the data points collected.
[0010] It is one aspect of the invention to provide a method for collecting perception data points by a market research service provider that offers considerably greater information and convenience to prospective initiators of market research service who desire to have a given item be assessed and offer the chances to win incentives to encourage accurate assessment and participation by respondents. It is still another aspect of the invention to provide a method to help one to understand how others perceive the value of a given item so that one may make an educated judgment on how to price such item. The object of the invention is that the more accurate the perception data given by respondents, the more likely the respondents will win the incentive.
[0011] This methodology has many applications in market research, especially in establishing price points for new products, but there are many other fields which could benefit from this type of perception assessment such as financial analysis for synthesizing market predictions, or in human resources for setting job salaries.
[0012] Other objects, features and advantages of the present invention will become apparent to those skilled in the art from the detailed description. It is to be understood, however, that the detailed description and specific examples, while indicating preferred embodiments of the present invention, are given by way of illustration and not limitation. Many changes and modifications within the scope of the present invention may be made without departing from the spirit thereof, and the invention includes all such modifications and equivalents thereof.
DESCRIPTION OF THE FIGURES
[0013] The invention is illustrated by way of example, and not by way of limitation, in the figures of the accompanying drawings in which like reference numerals refer to similar elements and in which:
[0014] FIG. 1 is a flow diagram for the process of incentivized collective perception assessment of one embodiment in accordance with the invention.
[0015] FIG. 2 illustrates a flow diagram that illustrates a part of the process showing the logic of awarding incentive to respondent(s).
[0016] FIG. 3 is a diagram of a computer system context.
DETAILED DESCRIPTION OF THE INVENTION
[0017] A method and system for incentivized collective perception assessment is described. In the following description, for the purposes of explanation, numerous specific details are set forth to provide a thorough understanding of the present invention. It will be apparent, however, to one skilled in the art that the present invention may be practiced without these specific details. In other instances, well-known structures and devices are shown in diagram form to avoid unnecessarily obscuring the present invention.
[0018] In this Specification and in the claims that follow, the terms recited below are associated with the following basic definitions:
[0019] Incentive: Any tangible or non-tangible benefit offered for participation in the process.
[0020] Initiator: Any entity or group of entities, living or non-living, which initiates the execution of the process.
[0021] Item: Any good, service or intangible that may be conveyed as stimulus to a respondent.
[0022] Network: One or more connections for enabling communication between or among users.
[0023] Perception: Singular data point or set of data points provided by a respondent and refers to the ability to analyze the item, objectively or subjectively, not necessarily cognitively, and provide a response.
[0024] Process: The invention that is the subject of this patent and described in the Specification.
[0025] Respondent: Any entity or group of entities, living or non-living, that participates in the process by providing a perception response. The respondent may participate in the process voluntary or by invitation.
[0026] Stimulus: Presentation of an item to respondent through any combination of physical, textual, visual, auditory, or electronic means.
[0027] Process
[0028] FIG. 1 illustrates one embodiment of the process of incentivized collective perception assessment. Meaningful survey results typically require perceptions from a non-biased population. In certain embodiments, user account mechanism during the process attempts to prohibit users from participating in a particular survey multiple times. Respondents should have no knowledge of others' perceptions and alerting them of a duplicate perception would give them some knowledge about the other's perception, thus mechanisms in the process attempts to limit respondents from accessing such knowledge. A survey could have one or more dimensions (e.g. price and favorability on a scale of 1 to 10). Each respondent will typically be allowed to submit one perception data point per dimension during one execution of the process, however, a variation of this process could allow for respondents to submit a given number of data points per dimension. Each user account with an associated user account identification is restricted to one response, in attempt to prevent respondents from exploiting the process to gain incentives, by linking the user account to one or more personal unique identifying information such as, for example, a physical postal address, bank account for receiving incentive, driver license number, social security number, or e-mail address.
[0029] A new user may enter the process at step 101 as initiator. A current user, in response to a need for some collective assessment of an item, may enter the process at step 102 as an initiator. A user account interface interacts with a new user to collect pertinent information about the user and stored in an information repository such as a database for user account. In certain embodiments, demographic data may be collected from the user during the steps 101 of creating a user account, and stored in the information repository for user account. The demographic data is collected from users pertaining personal information such as, for example, age, martial status, address, number and age of any children, occupation, annual income, etc. The process is executed by an initiator, or by a proxy at the request of the initiator, in response to a need for some collective assessment of an item. At the beginning of the process at step 101 , an initiator interacts with an interface to set up an account with the market research service provider.
[0030] At the step 102 , the initiator, or by a proxy at the request of the initiator, interacts with an interface to develop content for a survey of an item. When the initiator tries to create a survey for a common item, listing development interface may present an interactive template in which initiator may furnish description of the item, including, for example, image, odor, sound, taste, text, and texture. The interface with a common item template interacts with the initiator by using a generic form with descriptive entries for which respondents may use such information to evaluate the item and provide their perception. For example, if the item is a house, the interface brings up a real estate template which asks for pertinent information such as, for example, number of bedroom, number of bathroom, square footage, age of the house, picture of the house, map, location, etc. The interface provides the ability to initiators to define and set a range of allowable perceptions within the dimensions established for the item.
[0031] Initiators should exercise caution when setting ranges of allowable perception as too narrow a range can compromise the validity of the perceptions provided by limiting the respondent's ability to provide their true perception as well as giving away the initiator's presumed perception of the whole. This can help to ignore erroneous or disingenuous perceptions.
[0032] After a listing is developed, at step 103 the interface provide the ability to the initiator to designate that the listing is closed or open to any respondents, and set up a duration of time or quotas of submitted perception data points during which the listing remains available to potential respondents. When the listing is designated as closed, the initiator selects a target group of users, based on selected demographics, who are to access the listing and complete the survey until the duration or quota is met. For example, an invitation can be provided to any respondent that fits in a sub-group such as “females, age 21 to 25, home address within 50 miles of zip code 92101”. This would enable a population-specific perception to be collected. In certain embodiments, an initiator may choose to exclude one or more groups of certain demographics from participating in the survey.
[0033] At step 104 , the interface interacts with the initiator to provide an incentive and how incentive may be distributed. In a typical case, the incentive is provided in a form of monetary compensation. In certain embodiments, the incentive may be given to a winner or split equally to a set of winners. This part of the process is explained in more details in the further parts of the Detailed Description as illustrated in FIG. 2 and in the description of step 115 .
[0034] At step 105 , the interface interacts with the initiator to enter destination for survey results. The destination includes, for example, e-mail address, phone number, fax number, postal address, or any combination thereof. At step 106 , the interface provides the initiator with the ability to securely enter payment information. Once the initiator defines the survey, selects a target group of users, determines incentive, and enters survey results destination, a survey price is calculated accordingly for the service and provided to the initiator through the interface. Once an initiator accepts the price of survey, the initiator enters pertinent payment information and authorizes the payment to process. For example, an interface interacts with the initiator allowing the initiator to select a particular form of payment (i.e., credit card, debit card, Paypal, check transfer, etc.). In certain embodiment an initiator is allowed to enter an account number that corresponds to an account or credit line that was previously established. At step 106 , the initiator has the capability of returning to steps 102 through 105 to modify the requested survey parameters to produce a survey price that is acceptable to the initiator.
[0035] The survey created by the initiator is reviewed and screened for propriety and appropriateness for fielding to respondents at step 107 . In certain embodiments, an automated review of the survey is conducted by comparing components of the survey with a database of prohibited words, phrases, pictures, sounds, or themes. In another embodiment, surveys are automatically provided to an individual who is responsible for reviewing propriety of the survey contents.
[0036] Once survey is approved, the listing and survey are generated and attached to an information storage repository such as a database at step 108 based on the parameters and content provided by the initiator. At this step, rules for a range of allowable perceptions within the dimensions set for the item are created and attached to the survey. These rules provide a mechanism for validating the perception data points from respondents input as they participate in a survey. In certain embodiments, errors or logical inconsistencies that are identified are reported to respondent thus enabling them to enter valid perception data point. This mechanism attempts to maximize collection of perception data points from every respondents participating in the survey and avoids discarding invalidated perception data points after the survey is closed. At step 109 , an information repository such as a database is created to store survey results from respondents. In one embodiment, a storage unit is linked through an automated mechanism to each survey and is used to automatically store perception data points from respondents who participate in the survey.
[0037] At step 110 , quotas of submitted perception data points or length of time the listing remains available to users are attached to the database. The automated survey mechanism then fields the survey by causing one or more listings to be launched, activated, or displayed on one or more interfaces used by users who match the target group criteria for the survey set by the initiator. For example, if the initiator specified that the target group for a particular survey would be females 18-32 years of age, then interfaces used by users associated with this target group are selected to display listings for the particular survey for participation. In certain embodiments, the automated survey mechanism scans the user accounts in a database to find target group and generate commands to place the listing on the interfaces for the users in target group using the process.
[0038] The process uses an interface to interact with new users to create user accounts in any time during the process or at step 111 when the listings are active. As previously indicated above, pertinent information about user is collected during user account creation as well as demographics that are then stored in the information repository for user account. In certain embodiments, users may set a preference in the user account to have the automated survey mechanism deliver survey invitations and/or digest of available listings to destinations set by the users. The destination includes, for example, e-mail address, phone number, fax number, postal address, or any combination thereof. In certain embodiments, users may be asked to submit information of how they want to receive incentives and whether they accept service charge for a certain delivery or payment method for their incentive, for example, to their checking account, postal address, Paypal, credit card, etc.
[0039] As previously indicated above, in certain embodiments, an automated survey mechanism that fields the surveys by causing one or more listings to be launched, activated, or displayed on one or more interfaces at step 112 that interacts with users who match the target group criteria for the surveys associated with the listings. In certain embodiment, the automated survey mechanism may also send invitation to users in target group that set a preference in the user account to receive such message. Listings for open surveys are launched, activated, or displayed on one or more interfaces that interact with all users except for the initiator that initiates the survey associated with a particular listing. In certain embodiments, users that lack certain demographic information in the user account information repository are excluded from closed survey invitations for target groups such that their interfaces do not show listings for closed surveys. A search interface can also be provided for respondent to search for listings for surveys to participate in. The search interface can show all surveys that are not targeted to a specific sub-group of users. The search interface can also filter listing results based on a user's demographics to bring up targeted surveys. The listing shows users a brief information about the survey which includes, for example, what kind of item in the survey, duration or quotas for which the survey expire, what kind of incentive being offered for winner, how winner(s) is determined, etc. At this step, a user expresses a desire to activate a listing and participate in the survey associated to the listing. Upon activation of the listing, the user interacts with the survey through an interface and provides one or more perceptions. In certain embodiments, user may choose not to participate in the survey and return to the interface showing listings. The presentation of a survey to a respondent is stimulus for the respondent to provide perception for the assessment of an item.
[0040] At step 113 , and the perception data points linked with user account identifications from respondents participating in the survey are collected and stored in the information repository. At step 114 , after the required number of completed surveys is obtained, or the duration for fielding the survey has expired, access to the listing for the survey is disabled. At this step, in certain embodiments, the listing is automatically removed from one or more interfaces interacting with users by an automated survey mechanism thus eliminating access to the survey by users.
[0041] After close of the survey at step 115 , one or more winners are automatically determined by logic as illustrated in FIG. 2 and incentive is delivered to the user according to preference set in the user account. In certain embodiments, user is contacted through phone, postal address, fax, e-mail, or any combination thereof when the user account doesn't contain information on how incentives are delivered as expressed by the user desire.
[0042] FIG. 2 illustrates a part of the process showing, in certain embodiments, for the logic of awarding incentive to respondent(s) after the close of survey. The logic does not allow respondents with inaccurate perception data points to win the incentive. After the survey closes 201 , perception data point for each respondent and associated user account identification are extracted from the information repository and sorted by perception data point into a list of all survey respondents and their perception data points 203 . For a survey with a single dimension, the accuracy selection algorithm 202 determines one or more calculated values from all of the perception data points by the calculations of median 204 , mean 205 , mode 206 , or any combination thereof. For surveys with multiple dimensions, the perception data points associated with a respondent can be treated as a vector. The accuracy selection algorithm would determine one or more calculated values from all of the perception data points or vectors by calculations of the multi-dimensional median 210 or centroid 212 . The list of all survey respondents 203 is filtered by using one of the following accuracy selection criteria 207 :
[0043] Multi-dimensional median 210 can be calculated using Weiszfeld's Iteration Scheme). As the iteration scheme runs, it converges to the location that minimizes the sum of the distances. Letting q 0 =(q x 0 , q y 0 ) denote an (arbitrary) initial location, the iteration scheme works as follows:
[0000]
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[0044] Centroid 212 can be calculated using this formula:
[0000]
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A) One or more respondents with corresponding perception is selected for the filtered list using the closest match of the perception to one or more calculated values of median 204 , mean 205 , mode 206 , multidimensional median 210 , and/or centroid 212 . If none of the respondents' perception is equal to the calculated scalar or vector value, respondent(s) is then selected to the next closest iteration of perception data point above and/or below the calculated value. If there is more than one respondent with corresponding perception data point that has closest match of the calculated value, all respondents with the closest match are selected for the filtered list.
B) One or more respondents with corresponding perception data point is flagged for the filtered list when the corresponding perception data falls within a given range above and below one or more calculated value of median 204 , mean 205 , mode 206 , multidimensional median 210 , and/or centroid 212 . In one embodiment, the market research service provider may set a given range, preferably between 1 % and 10 % above and below the calculated value. This selection criterion using a given range may be useful when there are a small number of respondents.
[0047] For single dimensional surveys, if all three calculated values (median 204 , mean 205 , and mode 206 ) were used for filter respondents with either accuracy selection criteria 207 , there would be more respondents on the filtered list eligible to win the incentive. For multidimensional surveys, if both the multidimensional median 210 and centroid 212 were used for filter respondents with either accuracy selection criteria 207 , there would be more respondents on the filtered list eligible to win the incentive. In certain embodiments, initiator may select and refine one of the accuracy selection criteria at step 102 . After all of respondents in the database are selected by the accuracy selection criteria 207 and then grouped on the filtered list, one or more winners are selected from the filtered list of respondents by one of the winner selection criteria 208 :
A) A winner is randomly selected from the filtered list of respondents and the incentive will be given to the winner. B) All respondents on the filtered list are all winners and the incentive will be split equally to each winner. Typically, this method is applicable when the incentive is a form of money that can be easily split equally and rounded off.
[0050] At step 116 , the perception data points provided by users are extracted from the information repository. The extracted perception data points are processed, analyzed and formatted using common file formats as a survey report. In certain embodiments, graphical representations of the survey results are generated and inserted into the survey report. At step 117 , the file containing the survey results is sent to the address using a delivery method that was previously provided by the initiator. At step 118 , a receipt confirmation is received from the initiator indicating the file containing the survey results has been received.
[0051] Hardware and System
[0052] One embodiment of the invention is related to the use of a computer system for running the process and interacting with a respondent on a client computer system through a network. According to one embodiment of the invention, a survey is dynamically assigned to a respondent by a computer system in response to a processor executing one or more sequences of one or more instructions contained in main memory. Such instructions may be read into main memory from another computer-readable medium, such as storage device. Execution of the sequences of instructions contained in main memory causes processor to perform the process steps described herein. One or more processors in a multi-processing arrangement may also be employed to execute the sequences of instructions contained in main memory. In alternative embodiments, hard-wired circuitry may be used in place of or in combination with software instructions to implement the invention. Thus, embodiments of the invention are not limited to any specific combination of hardware circuitry and software.
[0053] Computer system includes a bus or other communication mechanism for communicating information, and a processor coupled with bus for processing information. Computer system also includes a main memory, such as a random access memory (RAM) or other dynamic storage device, coupled to bus for storing information and instructions to be executed by processor. Main memory also may be used for storing temporary variables or other intermediate information during execution of instructions to be executed by processor. Computer system further includes a read only memory (ROM) or other static storage device coupled to bus for storing static information and instructions for processor. A storage device, such as a magnetic disk or optical disk, is provided and coupled to bus for storing information and instructions.
[0054] Computer system may be coupled via bus to a display, such as a liquid crystal display (LCD), for displaying information to a computer user. An input device, including alphanumeric and other keys, is coupled to bus for communicating information and command selections to processor. Another type of user input device is cursor control, such as a mouse, a trackball, or cursor direction keys for communicating direction information and command selections to processor and for controlling cursor movement on display. This input device typically has two degrees of freedom in two axes, a first axis (e.g., x) and a second axis (e.g., y), that allows the device to specify positions in a plane.
[0055] The term “computer-readable medium” as used herein refers to any medium that participates in providing instructions to processor for execution. Such a medium may take many forms, including but not limited to, non-volatile media, volatile media, and transmission media. Non-volatile media includes, for example, optical or magnetic disks, such as storage device. Volatile media includes dynamic memory, such as main memory. Transmission media includes coaxial cables, copper wire and fiber optics, including the wires that comprise bus. Transmission media can also take the form of acoustic or light waves, such as those generated during radio wave and infrared data communications.
[0056] Common forms of computer-readable media include, for example, a floppy disk, a flexible disk, hard disk, magnetic tape, or any other magnetic medium, a CD-ROM, any other optical medium, punch cards, paper tape, any other physical medium with patterns of holes, a RAM, a PROM, and EPROM, a FLASH-EPROM, any other memory chip or cartridge, a carrier wave as described hereinafter, or any other medium from which a computer can read.
[0057] Various forms of computer readable media may be involved in carrying one or more sequences of one or more instructions to processor for execution. For example, the instructions may initially be carried on a magnetic disk of a remote computer. The remote computer can load the instructions into its dynamic memory and send the instructions over a telephone line using a modem. A modem local to computer system can receive the data on the telephone line and use an infrared transmitter to convert the data to an infrared signal. An infrared detector coupled to bus can receive the data carried in the infrared signal and place the data on bus. Bus carries the data to main memory, from which processor retrieves and executes the instructions. The instructions received by main memory may optionally be stored on storage device either before or after execution by processor.
[0058] Computer system also includes a communication interface coupled to the bus. Communication interface provides a two-way data communication coupling to a network link that is connected to a local network. For example, communication interface may be an integrated services digital network (ISDN) card or a modem to provide a data communication connection to a corresponding type of telephone line. As another example, communication interface may be a local area network (LAN) card to provide a data communication connection to a compatible LAN. Wireless links may also be implemented. In any such implementation, communication interface sends and receives electrical, electromagnetic or optical signals that carry digital data streams representing various types of information.
[0059] Network link typically provides data communication through one or more networks to other data devices. For example, network link may provide a connection through local area network to a server or to data equipment operated by an Internet Service Provider (ISP). ISP in turn provides data communication services through the worldwide packet data communication network now commonly referred to as the “Internet”. Local network and Internet both use electrical, electromagnetic or optical signals that carry digital data streams. The signals through the various networks and the signals on network link and through communication interface, which carry the digital data to and from computer system, are exemplary forms of carrier waves transporting the information.
[0060] Computer system can send messages and receive data, including program code, through the network(s), network link and communication interface. In the Internet example, a server might transmit a requested code for an application program through Internet, ISP, local network and communication interface. In accordance with the invention, one such application provides for running the process as described herein.
[0061] The received code may be executed by processor as it is received, and/or stored in storage device, or other non-volatile storage for later execution. In this manner, computer system may obtain application code in the form of a carrier wave.
[0062] FIG. 3 illustrates in block form an example of the parties and systems involved in this context. In FIG. 3 , a user is coupled either directly or indirectly to the Internet 306 . For example, a user may be connected to Internet 306 through a local area network 309 , an Internet Service Provider, an Online Service Provider such as AOL, a proprietary server, or any combination thereof. The users referenced in this description are end station devices such as a personal computer, workstation, network computer, etc. In the preferred embodiment, the client and other clients have a processor that executes an operating system and a browser program under control of the operating system. The browser program is an industry-standard World Wide Web browser, such as, for example, Microsoft Internet Explorer, Netscape Navigator, or NCSA Mosaic.
[0063] Connected to the Internet 306 is a plurality of network user clients 301 , 302 , 303 , 304 and 305 . By interfacing with network user clients 301 , 302 , 303 , 304 and 305 , network users can access, display and interact with Web pages that are contained on servers that are coupled to Internet 306 such as the survey process server 310 .
[0064] Through Internet 318 or locally through a network hub 307 , network user clients 301 , 302 , 303 , 304 and 305 can connect to the server 310 . Preferably, network user clients 301 , 302 , 303 , 304 and 305 communicate with the survey process server 310 using industry-standard protocols such as Transmission Control Protocol (TCP), Internet Protocol (IP), and Hypertext Transfer Protocol (HTTP).
[0065] The survey process server 310 run and manages the process described herein and contains storage unit. The survey process server 310 contains interface data that defines an interface that can be used to create a survey. For example, if an initiator requests to define a survey, the survey process server 310 automatically sends interface data over Internet 306 to cause an interface to be displayed on the browser executing on one of the user clients belonging to the initiator. The initiator then interacts with the interface to create a survey. The survey process server 310 also uses the interface interacts with user clients who are respondents. Storage unit on the survey process server 310 is used to store survey results. As network users participate in the surveys, the results are automatically stored in the storage unit on the survey process server 310 . In certain embodiment, a person from a market research service provider that manages the survey process server 310 may interacts with the administrative interface of the survey process server 310 for tasks related to a part of the process described herein such as, for example, screening the survey for propriety for fielding to users, printing and mailing the survey results, etc.
[0066] Alternatives, Extensions
[0067] In describing certain embodiments of the invention, several drawing figures have been used for explanation purposes. However, the invention is not limited to any particular configuration. The invention includes other contexts and applications in which the mechanisms and processes described herein are available to other mechanisms, methods, programs, and processes. Thus, the specification and drawings are, accordingly, to be regarded in an illustrative rather than a restrictive sense.
[0068] Although FIG. 3 depicts a single server 310 running the process, embodiments of the invention are not limited to any particular number of servers running the process. In addition, although server 310 running the process is depicted as a single component, it may actually consist of multiple computing and/or storage units that are configured to perform the functions described herein.
[0069] In addition, in this disclosure, certain process steps are set forth in a particular order, and alphabetic and alphanumeric labels are used to identify certain steps. Unless specifically stated in the disclosure, embodiments of the invention are not limited to any particular order of carrying out such steps. In particular, the labels are used merely for convenient identification of steps, and are not intended to imply, specify or require a particular order of carrying out such steps.
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Methods for collecting accurate perception data points related to a given item from a set of respondents by offering an incentive that benefits the respondent or respondents who submit data points that match most closely to a calculated value of the data points collected. Provides methods for collecting perception data points by a market research service provider that offers considerably greater information and convenience to prospective initiators of market research service who desire to have a given item be assessed and offer the chances to win incentives to encourage accurate assessment and participation by respondents. Helps one to understand how others perceive the value of a given item so that one may make an educated judgment on how to price such item. The object of the invention is that the more accurate the perception data given by respondents, the more likely the respondents will win the incentive.
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RELATED APPLICATION
This application claims priority under 35 U.S.C. §119 to U.S. Provisional application No. 61/364,293, filed Jul. 14, 2010, the entire disclosure of which is incorporated herein by reference.
TECHNICAL FIELD
This invention relates to integrating an ion transport membrane with a gas turbine.
BACKGROUND
Hydrocarbon and carbonaceous feedstock can be converted into H2 and CO synthesis gas mixtures with varying ratios of H2 to CO. Feedstock may include coals, natural gas, oil fractions, bitumen and tar-like refinery wastes, pet-coke and various forms of biomass. The synthesis gas mixtures can be converted into valuable hydrocarbons and chemicals using catalytic processes.
SUMMARY
In some implementations, a system can include an Ion Transport Membrane (ITM) module which separates pure oxygen from pressurized heated air integrated with a gas turbine to produce oxygen. An importantuse for the system is Integrated Gasification Combined Cycle (IGCC) systems with or without CO 2 capture to maximize or otherwise increase system efficiency. These implementations may enable diluent gas with less than 1% O 2 to be mixed safely with H 2 and/or (H 2 +CO) fuel gas. In addition, the combination of the ITM and the gas turbine minimize or otherwise reduce heat energy released in the ITM system that is transferred to the steam system. The air feed to the ITM module may be heated indirectly so that the partial pressure of O 2 in the air is not degraded by direct combustion in the feed air stream. This maximizes or otherwise increases O 2 recovery and minimizes or otherwise reduces air flow for a fixed O 2 production and membrane area. Also, some implementations may avoid or otherwise substantially reduce possible contamination of the ITM membrane from the combustion products.
The details of one or more embodiments of the invention are set forth in the accompanying drawings and the description below. Other features, objects, and advantages of the invention will be apparent from the description and drawings, and from the claims.
DESCRIPTION OF DRAWINGS
FIG. 1 shows the flow scheme for the process in which all the air flow to the ITM module is taken from the discharge of the gas turbine compressor; and
FIG. 2 shows the flow scheme for the process in which there is an external air compressor which together with air flow taken from the discharge of the gas turbine air compressor provides all the air feed to the ITM module.
Like reference symbols in the various drawings indicate like elements.
DETAILED DESCRIPTION
In some implementations, a system may include power generation from a gas turbine in which a carbonaceous or hydro-carbonaceous fuel is gasified using a partial oxidation reaction with pure O 2 generated from an ITM unit. Current systems, using coal or petroleum coke or residual bitumen as fuel, typically employ an O 2 fired partial oxidation process to convert the carbonaceous fuel to a fuel gas comprising H 2 +CO together with feed derived impurities such as H 2 S and others. This fuel gas stream is cooled and impurities such as H 2 S and others are removed. The purified fuel gas is then mixed with nitrogen and optionally steam before being used as fuel in a gas turbine combined cycle power generation system. O 2 used for partial oxidation has traditionally been generated by separating air in a cryogenic air separation unit to produce substantially pure O 2 . The described implementations uses an O 2 ion transport membrane (ITM) comprising mixed metal oxides typically in a perovskite crystal structure with vacancies in the O 2 ion sites. These structures allow the O 2 ions to become mobile in the crystal at high temperatures and the diffusion of O 2 across the membrane becomes possible when there is a difference in activity coefficient across the ITM. The ITM membrane then operates as a short circuited electrochemical cell. In order to operate the ITM unit it is necessary to provide a feed air stream at typically 800° C. to 900° C. with a partial pressure of oxygen of 3 to 4 bar in order to achieve O 2 separation factors of 70% or more from the feed air in the ITM system and produce sufficient O 2 to supply the partial oxidation gasifier. The pure O 2 may diffuse through the ITM membrane and may be available at a pressure typically in the range 0.3 to 0.8 bar. The adiabatically compressed air leaving the gas turbine air compressor may be heated to a temperature in the range 800° C. to 900° C. by direct combustion of a fuel in a first combustor. The heated air then passes through an ITM membrane module where some of the O 2 in the air is separated. The outlet O 2 depleted stream still has sufficient O 2 for combustion of more fuel in the second gas turbine combustor which raises the temperature to the design value for entry into the gas turbine expander.
Gas turbines are very expensive to modify and current high output, high efficiency gas turbines, which are commercially available have limited capability to extract a significant proportion of air leaving the air compressor section for external use in an ITM system. In some implementations, the ITM air flow may be taken not only from the gas turbine compressor discharge up to the maximum flow available but also from a separate air compressor with external heating of the compressed air feed to the ITM unit. When burning H 2 +CO fuel gas, the fuel gas may be diluted primarily with a nitrogen rich gas produced as a by-product of air separation together optionally with steam. This dilution may reduce the flame temperature and thus reduces NOX formation in the combustion. It may also load the turbine to maximize power output. The O 2 depleted non-permeate stream leaving the ITM unit may have excess N 2 and may be effective as a diluent for the H 2 or H 2 +CO fuel gas flow to the gas turbine burner. A typical system may have a fuel gas entering the gas turbine burner at a pressure in excess of the gas turbine air compressor discharge pressure and a composition of approximately 50% inert diluent and 50% (H 2 +CO) or H 2 on a molar basis. The maximum fuel gas temperature may be limited by the design of the gas turbine fuel handling system and is generally below 450° C. The diluent stream which is the ITM non-permeate leaves the ITM module at 850° C. This stream may be derived from an external air compressor. In general, the combined fuel gas and diluent stream may be at a temperature below about 450° C.
In some implementations, the diluent stream may be cooled to produce high pressure steam for the Rankine steam cycle which may be part of the combined cycle. The air feed stream to the ITM is heated to typically 850° C. by one of two methods:
(a) The direct combustion of fuel gas in the auxiliary air stream. This process may produce sufficient heat to raise the temperature of the air stream plus combustion products to 850° C. To illustrate this method, the following cases may be executed:
(i) The air compressor may be isothermal with a discharge condition of 22 bars 75° C. and provide all or substantially all of the air feed to the ITM unit with no air feed flow from the gas turbine. In this case, about 25% of the oxygen in the air may be consumed in direct fuel combustion, and the air flow may have to be increased by about 33% to compensate; and (ii) The air compressor may be adiabatic with a discharge temperature of 486° C. and can mix with a variable quantity of similar temperature air taken from the gas turbine. About 14% of the O 2 may be consumed for fuel combustion with an increased air flow of about 16%. In addition, the compressor power for the adiabatic machine may be 35% higher than the isothermal machine.
The second case (ii) may have a net 18% more power for compression than case (i) but has 45% less heat generated. Based on 1 lb mol air the extra power 0.224 kW hrs/lb mol air compressed, while the saving in heat for case (ii) is 1.27 kW. In general, it may be more efficient to use on an adiabatic air compressor for the external compressor.
(b) It has been proposed that the ITM feed air can be heated from 520° C. to 850° C. in the heat recovery steam generator (HRSG) associated with the gas turbine which would require combustion of more fuel in the gas turbine exhaust to raise its temperature from the range 500° C.-600° C. to the range 900° C.-1000° C. to provide the necessary temperature driving force for heat transfer to the ITM feed air stream. The effect of using fuel gas for direct heating as in case a(ii) compared to indirect heating in the HRSG is to reduce the air flow by 14% saving about 0.174 kW/hrs/lb mol ITM feed air.
The method of indirect heating in the heat recovery steam generator or HRSG may reduce the amount of compressed air flow (no combustion air may be used) but the whole gas turbine discharge flow may be heated from about 600° C. to about 875° C. For a typical integrated gasification combined cycle (IGCC) system, the ITM air flow may be about 25% of the gas turbine air flow when direct combustion heating is used and the ITM module may be designed for 80% O 2 recovery. The heat transferred to the ITM air feed may be available to the power cycle at an efficiency (LHV) of about 60% since it produces power in the gas turbine followed by the power produced in the steam system. The remaining heat from the duct firing used to raise the temperature of the gas turbine exhaust to 875° C. may only be available to produce power at about 40% efficiency in the Rankine steam cycle alone. This means that duct firing in the gas turbine exhaust entering the HRSG to allow indirect heating of the ITM feed air stream is a grossly inefficient use of the H 2 or (H 2 +CO) fuel generated in the gasification system. A detailed analysis of the performance of the duct fired HRSG with indirect heating of the ITM feed air stream is given in the examples.
In all of these cases, in order to produce the diluted fuel gas stream at typically 450° C., heat is recovered from the non-permeate ITM stream by cooling from 850° C. and rejecting this heat into the steam system where the maximum efficiency for the recovered heat to produce power is typically 40% and even with supercritical steam conditions will not exceed 44%. For a General Electric 9FA gas turbine linked to a coal based GE/Texaco quench gasifier, the duct firing heat load based on a normal gas turbine exit temperature of 600° C. would be 168 MW. The duct firing produces a hot gas for ITM feed air heating with a heat load requirement of 52.7 MW. Thus, an extra 115.2 MW of fuel gas must be consumed producing power at say 42% instead of 60% efficiency—a loss of 20.7 MW of electrical power.
The proposed prior art process uses the pressurized ITM non-permeate stream as a diluent for the H 2 or (H 2 +CO) fuel gas stream to reduce the combustion temperature to minimise NOX formation and to maximise turbine flow to fully load the turbine. There is a very significant hazard in this proposal since it is necessary to ensure that there will never be any chance of an O 2 concentration arising which would exceed the lower flammable limit for the mixture and cause an explosion. If we take a conservative view that the ITM O 2 recovery for the direct combustion case with a separate adiabatic air compressor was 70% then the O 2 concentration in the proposed diluent would be about 6% O 2 . This is far too high for safe operation. A level of less than 1% has been accepted in previous IGCC cases, where N 2 from a cryogenic ASU is mixed with fuel gases derived from a gasifier, as the maximum O 2 concentration permissible in the diluent N 2 stream
Integration of ITM O 2 production modules with existing unmodified gas turbines may include an external air compressor supplying part or all of the air flow for O 2 production. In some implementations, the proposed system may allow all or substantially all of the fuel gas combustion heat used for air preheating to be recovered at the gas turbine combustion heat input level so that recovered heat can produce electrical power at 55% to 60% net efficiency. Alternatively or in addition, the fuel gas may be effectively diluted with a nitrogen rich diluent and supplied at a temperature below 500° C. without loss of efficiency caused by transferring heat to the steam system. In addition, the oxygen content of the diluent stream may be reduced to a concentration at the ITM exit to reduce safety hazards when diluent and H 2 or (H 2 +CO) fuel gas at elevated temperature are mixed. Also, the mixture of H 2 or (H 2 +CO) fuel gas and diluent may be within an LHV value for satisfactory combustion in a gas turbine. The range may be for LHV values to be greater than about 120 Btu/scf and that the diluted fuel gas mixture may be at the maximum or otherwise an upper temperature allowed by the gas turbine vendor.
In some implementations, an ITM O 2 generation system coupled to a standard gas turbine modified to burn H 2 or H 2 rich fuel gas may be designed to include or execute one or more of the following: (1) the oxygen production may be sufficient to provide the O 2 required for a gasifier or other process consuming O 2 (e.g., an IGCC process which converts a carbonaceous or hydro-carbonaceous fuel to H 2 or a H 2 rich fuel gas with or without carbon dioxide capture and provides sufficient clean fuel gas to power the gas turbine); (2) the H 2 fuel gas may be diluted with inert gas to reduce NOX level and provide sufficient fuel gas to load the gas turbine but the LHV heating value of the fuel gas may be above 120 Btu/scf to favour combustion; (3) all or substantially all of the fuel gas used for heating air to ITM operating temperature of typically 850° C. may be used as part of the fuel gas input to the gas turbine even in the case when the ITM feed air stream is provided from a separate air compressor; (4) to maximize or otherwise increase O 2 production from a given ITM feed air flow the air may be heated indirectly; (5) the oxygen permeate and non-permeate streams leaving the ITM unit may be transfer the maximum or increased quantity of heat to or become part of the feed streams to either the gas turbine combustor or the upstream gasifier and, in some cases, any high grade heat transferred to the steam system may be minimized or otherwise reduces; (6) the maximum or upper temperature of the diluted H 2 feed gas to the gas turbine combustor may be 450° C. and the maximum or upper O 2 feed gas temperature to the gasifier may be 350° C.; (7) the O 2 content of the diluent to the H 2 fuel gas may be 2.5% O 2 to prevent possible ignition and explosion (e.g., O 2 content below 1% molar); (8) depending on the amount of side-draw air that can be withdrawn from the gas turbine, an air compressor in parallel to the gas turbine compressor may be included to make-up air feed to the ITM module. One or more of these objectives may be achieved by the following ITM gas turbine integration.
The ITM module may be fed with adiabatically compressed air drawn from the gas turbine air compressor discharge or a separate air compressor or both together. The gas turbine side-draw air stream which may form part or all of the air feed to the ITM module may be raised in pressure so that the non-permeate stream which is depleted in O 2 is at a sufficiently high pressure to be mixed with the gas turbine fuel gas stream, which passes through a regulation system and through the burner nozzles before mixing with the main gas turbine compressed air stream. In practice, the pressure may be raised in a single stage compressor by 2 bar to 5 bar. Air compressed isothermally in a separate air compressor may be heated by indirect heat transfer with the O 2 permeate stream from the ITM module in a first stage heat exchanger then mixed with any side-draw air from the gas turbine compressor discharge following compression. The non-permeate stream leaving the ITM module may be raised to a temperature in the range 850° C. to 950° C. in a directly fired combustor using diluted fuel gas. The total ITM feed air stream may then be heated by indirect heat transfer in a heat exchanger against the heated ITM non-permeate stream to raise its temperature in a range from about 800° C. to about 900° C. The ITM non-permeate stream may be heated by direct combustion of fuel gas to raise the temperature to a level sufficiently high to achieve two objectives: (2) to heat the ITM inlet air to 850° C.; and (2) to achieve an exit temperature from the air pre-heater for the non-permeate stream to ensure that when all or part of this stream is used as diluent for the fuel gas, which is close to ambient temperature the resulting mixed temperature is at 450° C. By partially removing O 2 from the non-permeate stream by oxidising fuel gas in the combustor, the resultant O 2 concentration may be kept below 2.5% O 2 (e.g., below 1% molar).
There may be an excess of non-permeate gas which is not needed or otherwise used for fuel gas dilution. This may be reduced in pressure and added to the gas turbine air compressor discharge or injected into the mixing section of the gas turbine combustors. Optionally, the two heat exchangers may be in parallel rather than in series. In a parallel arrangement the oxygen permeate stream which is at sub-atmospheric pressure, typically about 0.3 to 0.8 bar, may be passed through a heat exchanger which heats part of the air feed to the ITM unit. In a typical application, part of the ITM feed air may be heated to 820° C. against O 2 at 850° C. and the parallel heat exchanger may heat the remaining ITM air feed stream against heated non-permeate stream to a higher temperature than 850° C. so that total air stream after mixing was at about 850° C. The low pressure O 2 stream may then pass into a second heat exchanger which heats the compressed O 2 feed for the gasifier to about 350° C.
The system shown in FIG. 1 uses a gas turbine 1 coupled to an electric generator 2 which is also coupled to a steam turbine 3 . The steam is generated in a heat recovery steam generator 4 which includes boiler feed-water treatment and pumps and which is heated by the gas turbine exhaust stream 5 . Part of the air which has been adiabatically compressed in the gas turbine compressor 40 at 18 bar is compressed to 22 bar in compressor 7 . The air stream is heated in the parallel heat exchangers 8 and 9 to form a mixed steam 10 with a temperature of 850° C. The air enters an ITM module 11 where an oxygen stream 12 is separated at a pressure of, for example, 0.6 bar leaving a non-permeate stream 13 . A fuel gas stream 14 is divided into two streams. One stream 15 is the fuel for the gas turbine combustor 16 and the second stream 17 is the fuel for a combustor 18 in which the non-permeate stream 13 is heated to 1380° C. and leaves as stream 19 with an oxygen content of, for example, 1% molar. The oxygen permeate stream cools to 500° C. in heat exchanger 9 and the non-permeate stream cools to 860° C. The oxygen stream 20 leaving 9 is cooled in heat exchanger 21 where it heats the product oxygen stream 22 at 65 bar to 350° C. The intercooled compressor 23 raises the oxygen pressure from 0.35 bar to 65 bar. The non-permeate stream 29 leaving the heat exchanger 8 is cooled in heat exchanger 24 to a temperature at which part 25 can be mixed with the fuel gas stream 15 to give 50% fuel gas+50% diluent fuel gas stream which is at a mixed temperature which is below a maximum or predefined fuel stream inlet temperature specified by the gas turbine vendor which in this case is 450° C. The remaining non-permeate stream 26 is mixed with the exhaust as from the as turbine burner 16 and supply to the expander 42 . Steam can be generated and/or superheated in heat exchanger 24 to increase the power produced in the steam turbine 3 . Note that in order to simultaneously achieve the required temperature and composition of the mixed fuel gas stream 28 which is entering the gas turbine combustor 16 , the stream 29 can be divided so that part 30 bypasses the heat exchanger 24 .
The system shown in FIG. 2 is very similar to the system shown in FIG. 1 with the addition of an external intercooled air compressor 34 which produces half of the total ITM feed air flow 10 as stream 35 at a pressure 0.5 bar higher than the pressure of the gas turbine air side-draw flow leaving the compressor 7 and at a temperature of 75° C. Stream 35 is heated to 192° C. in heat exchanger 9 which cools the oxygen permeate stream 12 at 0.6 bar from the ITM module 11 to 500° C. from 850° C. The oxygen stream 20 leaving heat exchanger 9 is used in heat exchanger 21 to heat the compressed oxygen stream at 65 bar from the compressor 23 to a temperature of 350° C. The externally compressed air stream 36 leaving heat exchanger 9 is heated to about 500° C. in heat exchanger 8 and at this point it is mixed with the gas turbine side-draw air stream which is also at about 500° C. The mixed total air feed stream is then heated to 850° C. The heating medium in heat exchanger 8 is the heated non-permeate stream from the ITM module. The remaining parts of the system are identical to those shown in FIG. 1 .
An approximate scaling exercise is based on published data for Pittsburg No 8 coal used in an IGCC system with carbon monoxide sour shift reactors and 75% CO2 capture. The system may use GE 9FA gas turbines, cryogenic O 2 production and a Texaco quench gasifier with CO 2 capture. Fuel gas dilution may be with steam and some CO 2 . The base case performance follows:
Gross power (gasturbine+steam turbine+expansion turbine)=481 Mw
Cryogenic ASU power=47.7 Mw
Internal power consumption=14.1 Mw
Net power output=419.2 Mw
Net efficiency(LHV)=39%
Using the system described above with an ITM module and an oxygen compressor in place of the cryogenic oxygen plant may gave the following results:
1. All ITM air taken from the gas turbine air compressor outlet
Net Power=466.6 Mw
Net Efficiency=40.52%
2. Half ITM air from the gas turbine and half from a separate air compressor
Net power=462.3Mw
Net efficiency=41.37%
3. All ITM air taken from an separate air compressor
Net power=448.4Mw
Net efficiency=41.2%.
A number of embodiments of the invention have been described. Nevertheless, it will be understood that various modifications may be made without departing from the spirit and scope of the invention. For example, an approximate scaling exercise based on published data for coal IGCC using 9FA gas turbines, cryo O 2 and a Texaco quench gasifier with CO 2 capture showed an efficiency increase (LHV basis) from 39% to 41.65% with a power output increase of 6.8%. Accordingly, other embodiments are within the scope of the following claims.
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A system may include a compressor, a heat exchanger and an ITM. The compressor is configured to receive an air stream and compress the air stream to generate a pressurized stream. The heat exchanger is configured to receive the pressured stream and indirectly heat the pressurized stream using heat from an oxygen stream from an Ion Transport Membrane (ITM). The ITM is configured to receive the heated pressurized stream and generate an oxygen stream and the non-permeate stream, wherein the non-permeate stream is passed to a gas turbine burner and the oxygen stream is passed to the heat exchanger.
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TECHNICAL FIELD
[0001] The present disclosure generally relates to the field of nebulizers for aerosol generation and methods of using same for treating diseases and disorders.
BACKGROUND
[0002] Nebulizers are commonly used for delivering aerosol medication to patients via the respiratory system. Desirably, for efficient delivery of medication, the droplet diameter of the aerosol should be sufficiently small so as to reach the lungs of the patient without being obstructed by objects or organs (such as, the inner surface of the nozzle in the nebulizer and the mouth cavity perimeters) and large enough so as to remain in the lungs during exhalation.
[0003] The main techniques for producing aerosol in nebulizers include vibrating Mesh technology, jet nebulizers and ultrasonic wave nebulizers. Common to these techniques is the challenge to deliver large volume of medication to the patient while keeping the diameter of the droplets within desired limits.
SUMMARY
[0004] The following embodiments and aspects thereof are described and illustrated in conjunction with systems, tools and methods which are meant to be exemplary and illustrative, not limiting in scope. In various embodiments, one or more of the above-described problems have been reduced or eliminated, while other embodiments are directed to other advantages or improvements.
[0005] According to some embodiments, there are provided herein devices, systems and methods for generating aerosol for medication delivery using a porous medium and a displaceable spreading mechanism or liquid absorbing material. The aerosol may be generated by wetting the porous medium. Wetting may include applying the displaceable spreading mechanism thereby spreading liquid on the surface of the porous medium. Alternatively, wetting may include wetting the liquid absorbing material, then pressing it against the porous medium, or a surface thereof, resulting in a relatively uniform wetting of the porous medium. Once the porous medium, or a surface thereof, is wet, applying pressure gradient upon the porous medium results in the generation of aerosol.
[0006] According to some embodiments, applying pressure gradient entails introducing pressurized air to one side of the porous medium. According to some embodiments, applying pressure gradient entails introducing vacuum or sub-atmospheric pressure near one side of the porous medium. According to some embodiments, applying pressure gradient upon the porous medium entails having different pressure levels between two sides or surfaces of the porous medium.
[0007] Advantageously, the devices, systems and methods disclosed herein provide a relatively uniform or homogeneous wetting of the porous surface that may result in small diameter aerosol droplets, and confer the ability to yield such small diameter aerosol drops with high efficiency.
[0008] According to some embodiments, there is provided a nebulizer comprising a porous medium configured to produce aerosols, a displaceable wetting mechanism configured to spread a liquid over the porous medium thereby to wet the porous medium and a gas channel configured to introduce pressure gradient to the porous medium.
[0009] According to some embodiments, the displaceable wetting mechanism may include a rotatable elongated member.
[0010] According to some embodiments, the rotatable elongated member is configured to move across the surface of the porous medium, thereby to homogeneously or semi-homogeneously spread the liquid on the surface.
[0011] According to some embodiments, the elongated member is axially movable. According to some embodiments, the elongated member is movable to cover approximately all the surface of the porous medium.
[0012] The term “approximately” as used herein may refer to the percentage of surface of the porous medium that may be coated with liquid by the spreading movement of the elongated member. Approximately may refer to more than 50% coverage, more than 60% coverage, at least 70% coverage, at least 80% coverage, at least 90% coverage or at least 95% coverage. According to some embodiments, the wetting mechanism further includes an actuator, configured to displace or induce the displacement of the elongated member.
[0013] The term “displacement” as used herein may be interchangeable with any one or more of the terms movement, movement across. This term may refer to the motion of the wetting mechanism across, or along, at least one surface of the porous medium.
[0014] According to some embodiments, the elongated member comprises a first magnet, and the actuator comprises a second magnet, magnetically associated with the first magnet of the elongated member, such that by moving/displacing the second magnet of the actuator, a displacing of the elongated member is induced.
[0015] According to some embodiments, said first magnet may comprise a plurality of magnets. According to some embodiments, said second magnet may comprise a plurality of magnets.
[0016] According to some embodiments, one or more of the plurality of magnets includes an electromagnet. According to some embodiments, the actuator comprises a motor configured to displace the elongated member.
[0017] According to some embodiments, the elongated member is at least partially covered with polytetrafluoroethylene (PTFE), commercially knowns as Teflon®, or any other appropriate coating materials.
[0018] According to some embodiments, the elongated member is an elongated tubular member. According to some embodiments, the elongated member is movable by an actuator, mechanically connected thereto. According to some embodiments, the elongated member is movable by the air-flow within the nebulizer and/or through the porous material.
[0019] According to some embodiments, the elongated member is a roller. According to some embodiments, the elongated member is a smearing device. According to some embodiments, the elongated member is a spreading device. According to some embodiments, the elongated member is configured to force at least portions of the liquid to at least some of the pores of the porous medium.
[0020] According to some embodiments, the nebulizer further comprises a spacer configured to elevate said displaceable wetting mechanism from the surface of said porous medium. According to some embodiments, said spacer is integrally formed with said displaceable wetting mechanism. According to some embodiments, said spacer comprises a protrusion in said displaceable wetting mechanism. According to some embodiments, said spacer is configured to be placed between said displaceable wetting mechanism and the surface of said porous medium. According to some embodiments, said pacer comprises a ring-shaped configured to facilitate low-friction displacement of said displaceable wetting mechanism.
[0021] According to some embodiments, the nebulizer further comprises a liquid deploying mechanism configured to controllably deploy a liquid on the surface of said porous medium for being spread by said displaceable wetting mechanism. According to some embodiments, said liquid deploying mechanism comprises a conduit. According to some embodiments, said conduit has a receiving end, configured to obtain a liquid from a liquid source, and a deploying end, configured to deploy the liquid on the surface of said porous medium. According to some embodiments, said deploying end of said conduit is flexible and configured to flexibly move by the displacement of said displaceable wetting mechanism, thereby deploy the liquid at more than one location on the surface of said porous medium.
[0022] According to some embodiments, the nebulizer further comprises an opening configured to deliver the aerosols to a respiratory system of a subject.
[0023] According to some embodiments, there is provided a nebulizer comprising a porous medium configured to produce aerosols, a liquid absorbing material configured to absorb a liquid, a wetting mechanism configured to press the liquid absorbing material against the porous medium, thereby to wet the porous medium with the liquid absorbed in the liquid absorbing material and a gas channel configured to introduce pressure gradient to the porous medium.
[0024] According to some embodiments, the liquid absorbing material is a sponge, a tissue or foam.
[0025] According to some embodiments, the liquid absorbing material is configured to act as an impactor for aerosols produced by the porous medium.
[0026] According to some embodiments, the liquid absorbing material is configured to act as a filter for aerosols produced by the porous medium.
[0027] According to some embodiments, the liquid absorbing material comprises at least one pharmaceutical composition.
[0028] According to some embodiments, the nebulizer further comprises a first container, configured to contain liquids to be delivered to the liquid absorbing material.
[0029] According to some embodiments, the nebulizer further comprises a second container configured to contain at least one pharmaceutical composition. According to some embodiments, the liquids comprise water.
[0030] According to some embodiments, the gas channel is connected to a gas source.
[0031] According to some embodiments, there is provided a nebulizer cartridge, comprising a porous medium, and a displaceable wetting mechanism configured to spread a liquid over the porous medium, thereby to wet the porous medium.
[0032] According to some embodiments, the porous medium comprises a plurality of pores, wherein at least some of said plurality of pores comprise liquid. According to some embodiments, said liquid comprises a pharmaceutical composition.
[0033] According to some embodiments, the displaceable wetting mechanism further comprises an actuator configured to displace or induce the displacement of the rotatable elongated member. According to some embodiments, the rotatable elongated member comprises a first magnet, and the actuator comprises a second magnet, magnetically associated with said first magnet, such that by moving the second magnet displacement of the rotatable elongated member is induced. According to some embodiments, said first and/or second magnet comprises a plurality of magnets.
[0034] According to some embodiments, the cartridge is configured to be inserted to a nebulizer main body. According to some embodiments, the nebulizer main body comprises an opening configured to deliver aerosols.
[0035] According to some embodiments, the nebulizer main body further comprises a nozzle mechanically connected to the opening.
[0036] According to some embodiments, there is provided a nebulizer cartridge, comprising a porous medium and a liquid absorbing material, configured to be pressed against the porous medium, thereby produce aerosols.
[0037] According to some embodiments, the liquid absorbing material comprises a sponge.
[0038] According to some embodiments, the liquid absorbing material comprises a liquid absorbed therein.
[0039] According to some embodiments, the liquid is a pharmaceutical composition.
[0040] According to some embodiments, the pharmaceutical composition is for treating a disease via inhalation.
[0041] According to some embodiments, the cartridge further comprises a container, configured to contain liquid to be delivered to the liquid absorbing material.
[0042] According to some embodiments, the cartridge is configured to be inserted to a nebulizer main body. According to some embodiments, the nebulizer main body comprises an opening configured to deliver aerosols.
[0043] According to some embodiments, the nebulizer main body further comprises a nozzle mechanically connected to the opening.
[0044] According to some embodiments, the nebulizer further comprises a container, configured to contain liquid to be delivered to the liquid absorbing material.
[0045] According to some embodiments, the liquid comprises a pharmaceutical composition.
[0046] According to some embodiments, there is provided a nebulizer system comprising a housing, an opening in the housing configured to deliver aerosols to a subject, a cartridge, a receptacle configured to receive the cartridge and a gas channel, wherein the cartridge comprises a porous medium configured to produce aerosols and a wetting mechanism configured to spread the liquid absorbing material onto the porous medium.
[0047] According to some embodiments, the nebulizer system further comprises a nozzle, mechanically connected to the opening.
[0048] According to some embodiments, the wetting mechanism comprises a rotatable elongated member. According to some embodiments, the rotatable elongated member comprises an actuator configured to displace or induce the displacement of the rotatable elongated member.
[0049] According to some embodiments, the actuator comprises a shaft, configured to be mechanically connected to the wetting mechanism.
[0050] According to some embodiments, there is provided a nebulizer system comprising a housing, an opening in the housing configured to deliver aerosols to a subject, a cartridge, a receptacle configured to receive the cartridge and a gas channel, wherein the cartridge comprises a porous medium and a liquid absorbing material, configured to be pressed against the porous medium, thereby produce aerosols.
[0051] According to some embodiments, the liquid absorbing material comprises a sponge, a tissue or foam.
[0052] According to some embodiments, the liquid absorbing material comprises at least one pharmaceutical composition at least partially absorbed therein.
[0053] The term “partially absorbed therein” as used herein refers to the percentage of liquid absorbed in the pores of the porous material, wherein 0% refers to a porous material where all of its pores are vacant of liquid. Thus, the term “partially absorbed therein” may refer to a porous material wherein at least 0.005% of the pores contain liquid, or wherein the overall contents of the vacant space within the porous material occupied with liquid is 0.005%. According to some embodiments, partially absorbed therein refers to at least 0.001% liquid contents within the porous material. According to some embodiments, partially absorbed therein refers to at least 0.05% liquid contents within the porous material. According to some embodiments, partially absorbed therein refers to at least 0.01% liquid contents within the porous material. According to some embodiments, partially absorbed therein refers to at least 0.5% liquid contents within the porous material. According to some embodiments, partially absorbed therein refers to at least 0.1% liquid contents within the porous material. According to some embodiments, partially absorbed therein refers to at least 1% liquid contents within the porous material. According to some embodiments, partially absorbed therein refers to at least 5% liquid contents within the porous material. According to some embodiments, partially absorbed therein refers to at least 10% liquid contents within the porous material. According to some embodiments, partially absorbed therein refers to at least 20% liquid contents within the porous material. According to some embodiments, partially absorbed therein refers to at least 30% liquid contents within the porous material. According to some embodiments, partially absorbed therein refers to at least 40% liquid contents within the porous material. According to some embodiments, partially absorbed therein refers to at least 50% liquid contents within the porous material.
[0054] According to some embodiments, the term “partially absorbed therein” may refer to the content of liquid within the volume of pores located on the surface and in the immediate vicinity of the surface (sub surface) of a porous medium. According to some embodiments, the volume of the sub-surface may extend from the surface to a depth of about 50 micron from the surface.
[0055] According to some embodiments, partially absorbed therein refers to a porous material wherein at least 0.5% of the surface and sub-surface pores contain liquid. According to some embodiments, partially absorbed therein refers to at least 1% liquid contents within the surface and sub-surface pores. According to some embodiments, partially absorbed therein refers to at least 10% liquid contents within the surface and sub-surface pores. According to some embodiments, partially absorbed therein refers to at least 20% liquid contents within the surface and sub-surface pores. According to some embodiments, partially absorbed therein refers to at least 30% liquid contents within the surface and sub-surface pores. According to some embodiments, partially absorbed therein refers to at least 40% liquid contents within the surface and sub-surface pores. According to some embodiments, partially absorbed therein refers to at least 50% liquid contents within the surface and sub-surface pores. According to some embodiments, partially absorbed therein refers to at least 60% liquid contents within the surface and sub-surface pores.
[0056] According to some embodiments, the nebulizer system further comprises a first container, configured to contain liquids to be delivered to the liquid absorbing material.
[0057] According to some embodiments, the nebulizer system further comprises a second container configured to contain at least one pharmaceutical composition.
[0058] According to some embodiments, the gas channel is connected to a gas source.
[0059] According to some embodiments, there is provided a method for producing aerosols, the method comprises:
[0060] providing a nebulizer comprising a porous medium configured to produce aerosols, a displaceable wetting mechanism configured to spread the liquid over the porous medium thereby to wet the porous medium and a gas channel, wherein said porous medium is having two sides, a first side facing the displaceable wetting mechanism;
[0061] providing a liquid;
[0062] operating the displaceable wetting mechanism thereby spreading the liquid onto said first side of the porous medium; and
[0063] connecting the gas channel to a pressure source and introducing pressure gradient to the porous medium thereby producing aerosol at the first side of the porous medium, the aerosol comprises droplets of the liquid;
[0064] According to some embodiments, there is provided a method for producing aerosols, the method comprises:
[0065] providing a nebulizer comprising a porous medium configured to produce aerosols, a liquid absorbing material configured to absorb a liquid, a wetting mechanism configured to press the liquid absorbing material against the porous medium, and a gas channel configured to introduce pressure gradient to the porous medium, wherein the porous medium is having two sides wherein a first side is facing the liquid absorbing material;
[0066] providing liquid;
[0067] wetting the liquid absorbing material with the liquid;
[0068] pressing the liquid absorbing material against the porous medium; and
[0069] introducing pressure gradient to the porous medium thereby producing aerosol at the first side of the porous medium, the aerosol comprises droplets of the liquid.
[0070] According to some embodiments, the method further comprises delivering the aerosols to a respiratory system of a subject in need thereof.
[0071] According to some embodiments, the method further comprises providing a pharmaceutical composition and mixing the pharmaceutical composition with the liquid, prior to wetting the liquid absorbing agent.
[0072] According to some embodiments, the liquid absorbing material comprises a pharmaceutical composition.
[0073] According to some embodiments, the method further comprises iterating the following steps at least one more time: pressing the liquid absorbing material against the porous medium, introducing pressure gradient to the porous medium and producing aerosol at the first side of the porous medium, the aerosol comprises droplets of the liquid.
[0074] According to some embodiments, pressing comprises applying a pressing force that varies over iterations.
[0075] According to some embodiments, the method further comprises providing a cleansing liquid and iterating the following steps with the cleansing liquid: wetting the liquid absorbing material with the liquid, pressing the liquid absorbing material against the porous medium, introducing pressure gradient to the porous medium and producing aerosol at the first side of the porous medium, the aerosol comprises droplets of the liquid.
[0076] Certain embodiments of the present disclosure may include some, all, or none of the above advantages. One or more technical advantages may be readily apparent to those skilled in the art from the figures, descriptions and claims included herein. Moreover, while specific advantages have been enumerated above, various embodiments may include all, some or none of the enumerated advantages.
[0077] In addition to the exemplary aspects and embodiments described above, further aspects and embodiments will become apparent by reference to the figures and by study of the following detailed descriptions.
BRIEF DESCRIPTION OF THE DRAWINGS
[0078] Examples illustrative of embodiments are described below with reference to figures attached hereto. In the figures, identical structures, elements or parts that appear in more than one figure are generally labeled with a same numeral in all the figures in which they appear. Alternatively, elements or parts that appear in more than one figure may be labeled with different numerals in the different figures in which they appear. Dimensions of components and features shown in the figures are generally chosen for convenience and clarity of presentation and are not necessarily shown in scale. The figures are listed below.
[0079] FIG. 1 schematically illustrates a nebulizer with a porous medium, according to some embodiments;
[0080] FIG. 2 schematically illustrates a nebulizer with porous medium and medication containers, according to some embodiments;
[0081] FIG. 3 schematically illustrates a nebulizer with a sponge pressed against a porous medium, according to some embodiments;
[0082] FIG. 4 schematically illustrates generation of aerosol within a nebulizer, according to some embodiments;
[0083] FIG. 5 schematically illustrates a nebulizer system, according to some embodiments;
[0084] FIG. 6 shows a cumulative droplet size distribution of an aerosolized aqueous solution of a water soluble dye produced by a nebulizer having (squares), or devoid of (triangles), a liquid absorbing material;
[0085] FIG. 7 shows a cumulative droplet size distribution of an aerosolized aqueous solution of a water soluble dye containing glycerol (5%) produced by a nebulizer having (diamonds), or devoid of (triangles), a liquid absorbing material;
[0086] FIG. 8 shows cumulative droplet size distribution of commercial Ventolin® (5 mg/ml albuterol) aerosol produced by a nebulizer having a liquid absorbing material;
[0087] FIG. 9 a schematically illustrates a nebulizer with a rotatable wetting mechanism and a bottom actuator at side cross section, according to some embodiments;
[0088] FIG. 9 b schematically illustrates a nebulizer with a rotatable wetting mechanism and a bottom actuator at top cross section, according to some embodiments;
[0089] FIG. 9 c schematically illustrates a nebulizer with a rotatable wetting mechanism and a peripheral actuator at side cross section, according to some embodiments;
[0090] FIG. 9 d schematically illustrates a nebulizer with a rotatable wetting mechanism and a peripheral actuator at top cross section, according to some embodiments;
[0091] FIG. 9 e schematically illustrates a nebulizer with a rotatable wetting mechanism and a flexible medication deploying end at side cross section, according to some embodiments;
[0092] FIG. 9 f schematically illustrates a nebulizer with a rotatable wetting mechanism and a flexible medication deploying end at top cross section, according to some embodiments;
[0093] FIG. 9 g schematically illustrates a nebulizer with a rotatable wetting mechanism having protruding ends at side cross sections, according to some embodiments;
[0094] FIG. 9 h schematically illustrates a nebulizer with a rotatable wetting mechanism having protruding ends at top cross section, according to some embodiments;
[0095] FIG. 9 i schematically illustrates a nebulizer with a rotatable wetting mechanism and a spacer at side cross sections, according to some embodiments;
[0096] FIG. 9 j schematically illustrates a nebulizer with a rotatable wetting mechanism and a spacer at top cross sections, according to some embodiments;
[0097] FIG. 10 schematically illustrates nebulizer with a rotatable wetting mechanism and a liquid deploying structure, according to some embodiments;
[0098] FIG. 11 schematically illustrates nebulizer with a rotatable wetting mechanism and a liquid absorbing material, according to some embodiments;
[0099] FIG. 12 schematically illustrates a side cross section of a nebulizer assembly including an aerosolizing cartridge comprising a rotatable wetting mechanism, according to some embodiments;
[0100] FIG. 13 schematically illustrates a nebulizer system assembly with a rotatable wetting mechanism, according to some embodiments;
[0101] FIG. 14 represents the MMAD (diamond) and GSD (circle) values for various aqueous formulations containing a soluble dye tracer;
[0102] FIG. 15 represents fine particle fractions (FPF) of the aqueous formulations shown in FIG. 14 ;
[0103] FIG. 16 represents the mass distribution on Next generation impactor (NGI; an analytical instrument that measures droplet size distribution) plates for formulations 2 (circle), 5 (square) and 6 (triangle); and
[0104] FIG. 17 represents cumulative size distribution plots of Ventolin™ (circle) or insulin (square), produced using a nebulizer having a rotatable wetting mechanism, as a function of effective cut-off diameters (ECD).
DETAILED DESCRIPTION
[0105] In the following description, various aspects of the disclosure will be described. For the purpose of explanation, specific configurations and details are set forth in order to provide a thorough understanding of the different aspects of the disclosure. However, it will also be apparent to one skilled in the art that the disclosure may be practiced without specific details being presented herein. Furthermore, well-known features may be omitted or simplified in order not to obscure the disclosure.
[0106] There is provided, according to some embodiments, a nebulizer comprising a porous medium that is configured to produce aerosol, a liquid absorbing material configured to absorb a liquid, a wetting mechanism configured to press the liquid absorbing material against the porous medium or a first surface of the porous medium, thereby to wet the porous medium with the liquid absorbed in the liquid absorbing material and a gas channel configured to introduce pressure gradient to the porous medium.
[0107] The nebulizer disclosed herein may function as an inhaler under some circumstances. Thus, the terms ‘nebulizer’ and ‘inhaler’ as used herein may be interchangeable.
[0108] The terms ‘medium’ and ‘material’ as used herein are interchangeable.
[0109] Reference is now made to FIG. 1 , which schematically illustrates a nebulizer 100 comprising a porous medium 104 , according to some embodiments. Nebulizer 100 further comprises a sponge 102 , a wetting mechanism 106 , a gas channel 110 and an outlet 112 . Wetting mechanism 106 comprises a rod and a solid plate connected to sponge 102 .
[0110] The terms ‘nozzle’ and ‘outlet’ as used herein are interchangeable.
[0111] In some embodiment, the liquid absorbing material is a sponge, a tissue, a foam material, a fabric or any other material capable of fully or partially retrievably absorbing liquids. Each possibility is a separate embodiment of the invention.
[0112] According to some embodiments, the liquid absorbing material is configured to enable small diameter droplets to pass through the structure thereof and to obstruct large diameter droplets from passing through the material thereof.
[0113] According to some embodiments, the liquid absorbing material is configured to filter the passage of droplets depending on their diameter, such that large diameter droplets are obstructed by the liquid absorbing material.
[0114] The terms ‘sponge’ and ‘liquid absorbing material’ as used herein refer to any material that is capable of incorporating, taking in, drawing in or soaking liquids, and upon applying physical pressure thereto, release a portion or the entire amount/volume of the absorbed liquid. The physical pressure may be achieved for example by pressing the material against a solid structure.
[0115] According to some embodiments, the liquid absorbing material is having two sides, wherein a first side is facing the wetting mechanism and a second side is facing the porous medium. According to some embodiments, the wetting mechanism is a movable solid medium facing the first side of the liquid absorbing material. According to some embodiments, the wetting mechanism is in close proximity to the first side of the liquid absorbing material. According to some embodiments, the wetting mechanism is attached to the first side of the liquid absorbing material.
[0116] The term ‘attached to’ as used herein includes, but is not limited to, linked, bonded, glued, fastened and the like.
[0117] According to some embodiments, the porous medium is having two sides, wherein a first side is facing the liquid absorbing material and a second side is facing the gas channel. According to some embodiments, the first side of the porous medium is facing the liquid absorbing material and the gas channel. According to some embodiments, the liquid absorbing material and the porous medium are in close proximity. According to some embodiments, the first side of the liquid absorbing material and the first side of the porous medium are in close proximity.
[0118] Without being bound by any theory or mechanism, a pressure gradient at the porous medium reflects the presence of value difference between the pressure at the first side of the porous material and the pressure at the second side of the porous material, such that pressure values vary inside the volume of the porous medium. These values range from the pressure value at the first side to the pressure value at the second side of the porous medium.
[0119] According to some embodiments, the gas channel is a gas delivery channel configured to introduce pressure gradient to the porous medium. According to some embodiments, the gas channel is a gas delivery channel configured to introduce pressurized gas to the porous medium. According to some embodiments, the gas channel is a gas suction channel configured to introduce sub-pressurized gas to the porous medium.
[0120] The term ‘channel’ as used herein is interchangeable with any one or more of the terms port, passage, opening, orifice, pipe and the like.
[0121] According to some embodiments, a pressurized gas container is configured to deliver pressurized gas through the gas channel to the porous medium and create an ultra-atmospheric pressure on one side of the porous medium, thereby induce a pressure gradient at the porous medium.
[0122] The term ‘pressurized gas’ as used herein is interchangeable with the term ‘compressed gas’ and refers to gas under pressure above atmospheric pressure.
[0123] According to some embodiments, a vacuum container or sub-atmospheric pressure container is configured to suck gas through the gas channel and create a sub-atmospheric pressure on one side of the porous medium, thereby induce a pressure gradient within the porous medium.
[0124] According to some embodiments, the gas channel is connected to a gas source. According to some embodiments, the gas source is a mobile gas source, such as, a gas container. According to some embodiments, the gas source is a gas pump, configured to introduce pressure gradient in the porous medium by pumping gas to or from the gas delivery channel. According to some embodiments, the gas source is a pressurized gas container, configured to contain pressurized gas and to induce a pressure gradient in the porous medium by releasing pressurized gas to the pressurized-gas delivery channel.
[0125] According to some embodiments, the nebulizer further comprises an opening configured to deliver the aerosols to a respiratory system of a subject. According to some embodiments, the opening is connected to a nozzle. According to some embodiments, the opening is mechanically connected to a nozzle. According to some embodiments, the nozzle is detachable.
[0126] The correlation between droplet size and deposition thereof in the respiratory tract has been established. Droplets around 10 micron in diameter are suitable for deposition in the oropharynx and the nasal area; droplets around 2-4 micron in diameter are suitable for deposition in the central airways (and may be useful for delivering a bronchodilator, such as, salbutamol) and droplets smaller than 1 micron in diameter are suitable for delivery to the alveoli (and may be useful for delivering pharmaceuticals to the systemic circulation, for example, insulin).
[0127] According to some embodiments, the at least one pharmaceutical composition comprises one or more pharmaceutically active agents. According to some embodiments, the one or more pharmaceutically active agents are suitable or may be adjusted for inhalation. According to some embodiments, the one or more pharmaceutically active agents are directed for treatment of a medical condition through inhalation.
[0128] As used herein, a “pharmaceutical composition” refers to a preparation of a composition comprising one or more pharmaceutically active agents, suitable for administration to a patient via the respiratory system.
[0129] According to some embodiments, the pharmaceutical composition further comprises at least one pharmaceutical acceptable carrier. In other embodiments, the pharmaceutical composition may further comprise one or more stabilizers.
[0130] According to some embodiments, the nebulizer provides an aerosol containing a therapeutically effective amount of the pharmaceutical composition. As used herein, the term “therapeutically effective amount” refers to a pharmaceutically acceptable amount of a pharmaceutical composition which prevents or ameliorates at least partially, the symptoms signs of a particular disease, for example infectious or malignant disease, in a living organism to whom it is administered over some period of time.
[0131] The term “pharmaceutically acceptable” as used herein means approved by a regulatory agency of the Federal or a state government or listed in the U.S. Pharmacopeia or other generally recognized pharmacopeia for use in animals and, more particularly, in humans.
[0132] According to some embodiments, the pharmaceutical composition is in a liquid form such as solution, emulsion or suspension. Each possibility represents a separate embodiment of the present invention.
[0133] The pharmaceutical compositions of the invention may be prepared in any manner well known in the pharmaceutical art.
[0134] Useful pharmaceutically acceptable carriers are well known in the art, and include, for example, lactose, glucose, dextrose, sucrose, sorbitol, mannitol, starches, gum acacia, calcium phosphate, alginates, tragacanth, gelatin, calcium silicate, microcrystalline cellulose, polyvinylpyrrolidone, cellulose, water and methylcellulose. Other pharmaceutical carriers can be sterile liquids, such as water, alcohols (e.g., ethanol) and lipid carriers such as oils (including those of petroleum, animal, vegetable or synthetic origin, such as peanut oil, soybean oil, mineral oil, sesame oil and the like), phospholipids (e.g. lecithin), polyethylene glycols, glycerine, propylene glycol or other synthetic solvents. Each possibility represents as separate embodiment of the present invention.
[0135] Pharmaceutical acceptable diluents include, but are not limited to, sterile water, phosphate saline, buffered saline, aqueous dextrose and glycerol solutions, and the like. Each possibility is a separate embodiment of the invention.
[0136] According to some embodiments, the at least one therapeutic agent is selected from the group consisting of a hormone, a steroid, anti-inflammatory agent, antibacterial agent, anti-neoplastic agent, pain relief agent, narcotics, anti-angiogenic agent, siRNA, immuno-therapy related agent, growth-inhibitory agent, apoptotic agent, cytotoxic agent and chemotherapeutic agent. Each possibility is a separate embodiment of the invention.
[0137] According to some embodiments, the at least one pharmaceutical composition comprises albuterol, also known as, salbutamol and Ventolin®.
[0138] According to some embodiments, the medical condition is a pulmonary disease. According to some embodiments, the pulmonary disease is bronchospasm, asthma and chronic obstructive pulmonary disease among others. According to some embodiments, the asthma is allergen asthma or exercise-induced asthma.
[0139] According to some embodiments, the medical condition is a lung disease affecting the air ways, the alveoli or the interstitium, such as, asthma, chronic obstructive pulmonary disease, chronic bronchitis, emphysema, acute bronchitis, cystic fibrosis, pneumonia, tuberculosis, fragile connections between alveoli, pulmonary edema, lung cancer in its many forms, acute respiratory distress syndrome, pneumoconiosis, interstitial lung disease among others.
[0140] According to some embodiments, at least one of the pharmaceutical compositions comprises a therapeutically effective amount of medication for treating one or more of the medical conditions stated hereinbefore.
[0141] In some embodiments the medical condition is a metabolic disease, such as, diabetes mellitus (diabetes) Type 1, Type 2 and gestational diabetes, and the at least one pharmaceutical composition comprises a therapeutically effective amount of inhalable insulin.
[0142] According to some embodiments, the wetting mechanism is a mechanic mechanism configured to apply pressure onto the liquid absorbing medium. According to some embodiments, the wetting mechanism is a pneumatic mechanism configured to apply pressure onto the liquid absorbing medium. In some embodiment the wetting mechanism is coupled with an actuator. According to some embodiments, the wetting mechanism comprises a metering pump adapted to delivering a pre-determined volume of liquid at desired pressure(s) directly to the surface of the porous medium.
[0143] According to some embodiments, the nebulizer is mobile. According to some embodiments, the nebulizer is handheld. According to some embodiments, the nebulizer is powered by a mobile power source.
[0144] There is provided, according to some embodiments, a nebulizer housing configured to host at least one cartridge having a liquid absorbing material. The housing may further include any one or more of a porous medium, an opening, a nozzle connected to the opening, one or more container containing liquids, pharmaceutically active agents and composition comprising same, and a combination thereof.
[0145] According to some embodiments, the nebulizer housing is mobile. According to some embodiments, the housing is handheld. According to some embodiments, the nebulizer is powered by a mobile power source. According to some embodiments, the cartridge is disposable. According to some embodiments, the cartridge is recyclable. According to some embodiments, the liquid absorbing material is disposable. According to some embodiments, the cartridge is reusable.
[0146] According to some embodiments, the nebulizer is configured to communicate wirelessly with servers, databases, personal devices (computers, mobile phones) among others.
[0147] According to some embodiments, the nebulizer is assembled by introducing a cartridge into the housing.
[0148] There is provided, according to some embodiments, a nebulizer system comprising a housing, an opening in the housing configured to deliver an aerosols to a subject, a receptacle configured to receive a cartridge (the cartridge comprises a liquid absorbing material, and a porous medium, having at least one porous surface, configured to produce aerosols and a wetting mechanism configured to press the liquid absorbing material against the porous medium or against a surface of the porous medium), an actuator configured to control the wetting mechanism and a gas channel, to introduce a pressure gradient to the porous medium.
[0149] According to some embodiments, there is provided a nebulizer system comprising a receptacle configured to receive a cartridge. In combination, the nebulizer housing and the cartridge comprise the following elements: a liquid absorbing material, a porous medium having a porous surface, a wetting mechanism and at least one liquid or medication container.
[0150] The elements above may be comprised within the housing or the cartridge in various combinations; some examples of these combinations are given below for exemplary purposes, without limiting the disclosure from other possible combinations.
[0151] According to some embodiments, the housing comprises a receptacle, a porous medium, a liquid or medication container and a wetting mechanism, while the cartridge comprises a liquid absorbing material.
[0152] According to some embodiments, the housing comprises a receptacle, a porous medium and a liquid or medication container, while the cartridge comprises a liquid absorbing material and a wetting mechanism.
[0153] According to some embodiments, the housing comprises a receptacle and a liquid or medication container, while the cartridge comprises a porous medium, a liquid absorbing material and a wetting mechanism.
[0154] According to some embodiments, the housing comprises a receptacle and a porous medium, while the cartridge comprises a liquid or medication container, a liquid absorbing material and a wetting mechanism.
[0155] According to some embodiments, the housing comprises a receptacle while the cartridge comprises a liquid or medication container, a liquid absorbing material a porous medium, and a wetting mechanism.
[0156] According to some embodiments, the housing comprises at least two receptacles, a first receptacle configured to receiving a cartridge comprising a liquid absorbing material, and a second receptacle configured to receive a liquid or medication container.
[0157] According to some embodiments, the liquid absorbing material is presoaked with medication. According to some embodiments, the presoaked liquid absorbing material is hermetically or semi hermetically sealed. According to some embodiments, the seal is configured to be disrupted or otherwise removed upon usage. According to some embodiments, the seal is configured to be automatically disrupted or otherwise removed, for example, by an actuator in the nebulizer system. According to some embodiments, the seal is configured to be manually removed or disrupted by a user prior to use thereof.
[0158] According to some embodiments, the nebulizer system further comprises control mechanism configured to control the release of the liquid from the container containing same, into the liquid absorbing material. According to some embodiments, the control mechanism is configured to control the release of the liquid in a slow and/or gradual release manner According to some embodiments, the nebulizer system further comprises deployment mechanism configured to deploy the medication or liquid from the container containing same and into the liquid absorbing material.
[0159] According to some embodiments, the nebulizer system or cartridge comprises a medication preparation mechanism for mixing the medication with a liquid to enable reconstitution of the medication, or dilution thereof, prior to aerosolization of the composition.
[0160] According to some embodiments, some mechanisms of the nebulizer system are configured to provide homogeneous or semi homogeneous wetting of the porous medium. According to some embodiments, the mechanisms are other than the liquid absorbing material and the wetting mechanism. Examples for such mechanisms include, but are not limited to, spray mechanism, wiping mechanisms and the like.
[0161] Reference is now made to FIG. 2 , which schematically illustrates a nebulizer 200 comprising a porous medium 204 and a sponge 202 , according to some embodiments. Nebulizer 200 further comprises a liquid container 214 and a medication container 216 . Liquid container 214 and medication container 216 are configured to enable deployment of their possibly contained contents to sponge 202 to be pressed against porous medium 204 .
[0162] Reference is now made to FIG. 3 which schematically illustrates a nebulizer 300 comprising a porous medium 304 and a sponge 302 , according to some embodiments. As illustrated, a liquid container 314 and a medication container 316 have had their content deployed to sponge 302 , and sponge 302 is pressed against porous medium 304 by a wetting mechanism 306 . A pressurized gas 318 is delivered to porous medium 304 via a gas channel 310 .
[0163] Reference is now made to FIG. 4 which schematically illustrates generation of aerosol within a nebulizer, according to some embodiments. A nebulizer 400 is introduced comprising a porous medium 404 , a sponge 402 and a nozzle 412 , according to some embodiments. Sponge 402 is released from its previous press and wetting position (press and wetting of porous medium 404 ). A pressurized gas 418 delivered to porous medium 404 via a gas channel 410 introduces a pressure gradient to porous medium 404 . The pressure gradient results in the production of an aerosol having large droplets 422 and small droplets 420 . Large droplets 422 are impacted by sponge 402 which obstructs their path towards nozzle 412 .
[0164] Small droplets 420 , are lighter than large droplets 422 , and are mostly drifted away from impacting sponge 402 , thus they are not obstructed and may flow towards nozzle 412 . Large droplets 422 are impacted and obstructed by sponge 402 , advantageously resulting in a delivery of aerosol characterized with small diameter/size droplets.
[0165] The terms ‘droplet size’ and ‘mass median aerodynamic diameter’, also known as MMAD, as used herein are interchangeable. MMAD is commonly considered as the median particle diameter by mass.
[0166] According to some embodiments, control over droplet size and modality of generated aerosol is achieved by controlling physical properties of the porous medium. According to some embodiments, the physical properties of the porous medium are adjusted based on the desired droplet size. The physical properties of the porous medium, may include, but are not limited to, physical dimensions of the porous medium as a whole, pore count, pore density, pore distribution, pore shape, homogeneity of the aforementioned pore features, hydrophobicity of the porous material, and electromagnetic affinity among other properties. Each possibility is a separate embodiment of the invention.
[0167] The term “modality” as used herein refers to the modality of size distributions and includes, but is not limited to, uni-modal, bi-modal and tri-modal size distributions.
[0168] According to some embodiments, control over droplet size and modality of generated aerosol is achieved by controlling the physical properties of the liquid absorbing material.
[0169] According to some embodiments, control over droplet size and modality of generated aerosol is achieved by controlling the pressure gradient on the porous medium.
[0170] According to some embodiments, control over droplet size and modality of generated aerosol is achieved by controlling the properties of the medication and/or liquid and/or composition. The properties of the medication and/or liquid and/or composition which may be adjusted to achieve the desired aerosol, include, but are not limited to, viscosity, surface tension, pH, electrolyte concentration, solid content and polarity
[0171] According to some embodiments, control over droplet size and moadality of generated aerosol is achieved by introducing an impactor. According to some embodiments, the liquid absorbing material is configured to act as an impactor. According to some embodiments, the liquid absorbing material is the impactor. According to some embodiments, control over droplet size of generated aerosol is achieved by introducing a filter. According to some embodiments, the liquid absorbing material is configured to act as a filter. According to some embodiments, the liquid absorbing material is the filter. According to some embodiments, the impactor is an independent structure, different from the liquid absorbing material. According to some embodiments, the filter is an independent structure, different from the liquid absorbing material.
[0172] Reference is now made to FIG. 5 which schematically illustrates a nebulizer system 500 , according to some embodiments. Nebulizer system 500 comprises a gas pump 528 an actuator 530 a first deployment controller 524 , a second deployment controller 526 , a wetting mechanism 506 , a sponge 502 , a porous medium 504 , a gas channel 510 , a liquid container 514 , a medication container 516 and a nozzle 512 .
[0173] According to some embodiments, pump 528 is configured to deliver compressed gas to porous medium 504 via gas channel 510 . Actuator 530 is configured to control the movement and function of wetting mechanism 506 for pressing sponge 502 against porous medium 504 . First deployment controller 524 is configured to control the deployment of contained liquid in liquid container 514 to sponge 502 , and second deployment controller 526 is configured to control the deployment of medication in medication container 516 to sponge 502 .
[0174] According to some embodiments, the actuator is configured to control the pressure applied onto the liquid absorbing material. According to some embodiments, the actuator is configured to control the movement of the wetting mechanism. According to some embodiments, the actuator operates through mechanic, electro mechanic, electromagnetic, electro thermal, hydraulic, pneumatic or electronic mechanism. Each possibility is a separate embodiment of the invention.
[0175] There is provided, according to some embodiments, a method for producing aerosol comprising the steps of providing a liquid absorbing material, a porous medium having two sides in which the first side is facing the liquid absorbing material and further providing liquid, wetting the liquid absorbing material with the liquid, pressing liquid absorbing material against the porous medium, introducing pressure gradient to the porous medium and producing aerosol at the first side of the porous medium, the produced aerosol comprises droplets of the liquid.
[0176] According to some embodiments, the liquid is provided in a container. According to some embodiments, the method further comprises controlling the release of the liquid from the container into the liquid absorbing material. According to some embodiments, the method further comprises releasing the liquid in a slow and/or gradual release manner. According to some embodiments, the method further comprises deploying the medication or liquid from the container and into the liquid absorbing material.
[0177] According to some embodiments, the method further comprises providing a first container with a liquid and a second container with medication, and mixing the medication with the liquid to enable reconstitution of the medication, or dilution thereof, prior to aerosolization.
[0178] The term ‘wetting’ as used herein refers to homogenous or pseudo homogenous wetting of one side of the porous medium.
[0179] According to some embodiments, the method further comprises wetting the porous medium homogenously.
[0180] According to some embodiments, the method further comprises providing a pharmaceutical composition and mixing the pharmaceutical composition with the liquid, prior to wetting the liquid absorbing agent.
[0181] According to some embodiments, the liquid absorbing material already includes a pharmaceutical composition. The pharmaceutical composition within the liquid absorbing material may be in a solid form, e.g. a powder, or otherwise concentrated, such that upon wetting the liquid absorbing material, the pharmaceutical composition is reconstituted, or otherwise diluted, thereby resulting with the required pharmaceutically acceptable form suitable for inhalation following the conversion thereof into aerosols.
[0182] According to some embodiments, the liquid mixed with the pharmaceutical composition is a pharmaceutically acceptable carrier.
[0183] According to some embodiments, the pressing of the liquid absorbing material upon the porous medium is iterated a plurality of times. According to some embodiments, the pressing is executed while applying a non-constant pressing force/pressure across iterations. According to some embodiments, after deploying a content of liquid or medication container into the liquid absorbing material, a first pressing of the liquid absorbing material against the porous medium is carried out utilizing a first pressing force (pressure), a second pressing of the liquid absorbing material against the porous medium is executed utilizing a second pressing force, and so on. According to some embodiments, the first pressing force is lower than the second pressing force, advantageously resulting in a more unified wetting of the porous surface of the porous medium.
[0184] In some embodiments, a deployment of medication into the liquid absorbing material is performed, then the liquid absorbing material is pressed against the porous medium, wetting the porous surface of the porous medium for generating aerosol, and then a deployment of a liquid into the liquid absorbing material is performed. According to some embodiments, the liquid is sterile. According to some embodiments, the liquid is saline, water, carrier, cleansing liquid and the like, the deployment of which is performed for diluting the medication content in the liquid absorbing material. In some embodiment, the deployment of the liquid is performed for cleansing the liquid absorbing material and releasing the medication residues that may accumulate in the liquid absorbing material to achieve better delivery of medication to the subject, or for cleansing the liquid absorbing material, the porous medium or both.
[0185] According to some embodiments, by cleansing the liquid absorbing material, the porous medium or both, the components may be reused. Advantageously, the cleansing may prevent accumulation of medication residue in the nebulizer or some components thereof.
[0186] According to some embodiments, the droplets of the aerosol produced by the method and nebulizers disclosed herein are having an MMAD within the range of 0.3 to 7 microns. According to some embodiments, the MMAD is within the range of 2 to 10 microns. According to some embodiments, the MMAD is less than 5 microns.
[0187] According to some embodiments, the wetting mechanism includes a rotatable/displaceable elongated member, configured to be movably placed on the surface of the porous medium, or in close proximity thereto, or placed on the liquid absorbing material. According to some embodiments, the wetting mechanism includes a rotatable/displaceable elongated member (e.g. a spinning magnet) configured to be placed on the liquid absorbing material, such that liquid is extracted from the liquid absorbing material by the wetting mechanism. According to some embodiments, the rotatable elongated member is configured to move across the surface of the porous medium, thereby to homogeneously or semi-homogeneously spread the liquid on the surface of the porous medium.
[0188] According to some embodiments, the elongated member is axially movable. According to some embodiments, the elongated member is movable to cover the entire surface of the porous medium or substantial portions thereof. According to some embodiments, the wetting mechanism further includes an actuator, configured to displace/move or induce the displacement/movement of the elongated member.
[0189] The term “substantial portions” as used herein commonly refers to at least 30% coverage of the surface of the porous medium. According to some embodiments, the substantial portions include at least 50% coverage of the surface of the porous medium, at least 60% coverage of the surface of the porous medium, at least 70% coverage of the surface of the porous medium, at least 80% coverage of the surface of the porous medium or at least 90% coverage of the surface of the porous medium.
[0190] According to some embodiments, the elongated member may include a magnet, and the actuator may also include a magnet, magnetically associated with the magnet of the elongated member, such that by moving/displacing the magnet/electromagnet of the actuator, a moving/displacing of the elongated member may be induced.
[0191] According to some embodiments, one or more of the magnets includes an electromagnet. According to some embodiments, the actuator may include a motor configured to move/displace the actuating magnet.
[0192] According to some embodiments, the elongated member may be coated by a hydrophobic coating. According to some embodiments, the elongated member may be at least partially coated by a hydrophobic coating. According to some embodiments, the coating may be smooth, non-corrosive, non-toxic, non-evaporative or a combination thereof. According to some embodiments, the coating may include polytetrafluoroethylene (e.g. Teflon®).
[0193] The term “at least partially” as used herein may include at least 50 % coating of the elongated member, at least 60% coating of the elongated member, at least 70% coating of the elongated member, at least 80% coating of the elongated member or at least 90% coating of the elongated member.
[0194] According to some embodiments, the elongated member is an elongated tubular member. According to some embodiments, the elongated member may be movable by an actuator, mechanically connected thereto. According to some embodiments, the elongated member may be movable by an air-flow within the nebulizer and/or through the porous material.
[0195] According to some embodiments, the elongated member may be a roller. According to some embodiments, the elongated member may be a smearing device. According to some embodiments, the elongated member may be a spreading device. According to some embodiments, the elongated member may be configured to force at least portions of the liquid to at least some of the pores of the porous medium.
[0196] Reference is now made to FIG. 9 a , which schematically illustrates a side cross section of a nebulizer 900 with a rotatable wetting mechanism, according to some embodiments. According to some embodiments, the wetting mechanism of nebulizer 900 includes a rotatable elongated member, such as movable magnet 940 , which is placed on, or in close proximity to a surface of a porous medium, such as porous disc 904 , within a nebulizer housing, such as housing 902 . Movable magnet 940 is configured to rotate on porous disc 904 , thereby homogeneously or semi-homogeneously spread a liquid on porous disc 904 and/or at least partially force a liquid within the pores of porous disc 904 . According to some embodiments, nebulizer 900 further includes a liquid deploying mechanism, such as medication conduit 946 , configured to provide liquids and/or medication(s) to movable magnet 940 and/or porous disc 904 . According to some embodiments, nebulizer 900 further includes an actuator configured to directly or indirectly move or induce the displacement of movable magnet 940 . According to some embodiments, the actuator includes a motor 944 , mechanically or electromechanically connected to an actuator-magnet, such as motor-magnet 942 being associated with movable magnet 940 , such that a displacement of motor-magnet 942 induces a displacement of movable magnet 940 . Motor 944 is configured to axially rotate motor-magnet 942 , thereby induce an axial rotation of movable magnet 940 over/on the surface of porous medium 904 .
[0197] In operation, according to some embodiments, pressurized gas/air is provided to housing 902 , for example through pressurized-gas conduit 910 , and introduced to one side of porous disc 904 which interrupts the flow of gasses therethrough, thereby a pressure gradient occurs across porous disc 904 . Liquids may be provided through medication conduit 946 and introduced to the surface of porous disc 904 , and then movable magnet 940 spreads the liquid homogeneously or semi-homogeneously on the surface and at least partially forced through the pores of porous disc 904 by the axial rotation thereof, induced by the rotation of motor magnet 942 and motor 944 . According to some embodiments, the pressure gradient on porous disc 904 generates a mist of multiple droplets as the gas passes through the pores, the mist is then delivered through an outlet, such as mouthpiece 912 .
[0198] Reference is now made to FIG. 9 b , which schematically illustrates a top cross section view of a nebulizer 901 with a rotatable wetting mechanism, according to some embodiments. The rotatable wetting mechanism includes a displaceable/movable elongated member, such as a movable magnet 940 , which is placed on, or in close proximity to a surface of a porous medium, such as a porous disc 904 held within a nebulizer housing 902 . Movable magnet 940 is configured to be rotatable (arrows 950 ) and to spread/smear/distribute liquids on the surface of porous disc 904 , the liquids may be provided onto the surface of porous disc 904 , and According to some embodiments, the liquids may be provided to rotatable magnet 940 .
[0199] Reference is now made to FIG. 9 c , which schematically illustrates a side cross section of a nebulizer 900 with a rotatable wetting mechanism and a peripheral actuator, according to some embodiments. According to some embodiments, the wetting mechanism of nebulizer 900 includes a rotatable elongated member, such as movable magnet 940 , which is placed on, or in close proximity to a surface of a porous medium, such as porous disc 904 , within a nebulizer housing, such as housing 902 . Movable magnet 940 is configured to rotate on porous disc 904 , thereby homogeneously or semi-homogeneously spread a liquid on porous disc 904 and/or at least partially force a liquid into the pores of porous disc 904 . According to some embodiments, nebulizer 900 further includes a liquid deploying mechanism, such as medication conduit 946 , configured to provide liquids and/or medication(s) to movable magnet 940 and/or porous disc 904 . According to some embodiments, nebulizer 900 further includes a peripheral actuator configured to directly or indirectly move or induce the displacement of movable magnet 940 . According to some embodiments, the peripheral actuator included is configured to be placed over, or to surround, movable magnet 940 and to fluctuate the magnetic field flux near movable magnet 940 , thereby induce a mechanical movement thereof (rotation). According to some embodiments, the peripheral actuator may be a ring actuator such as controllable electromagnet-ring 960 which may include a plurality of controllable electro-magnets (not shown) which are electrically controlled for inducing a gradient in the electromagnetic field flux in the environment of movable magnet 940 , thereby induce an axial rotation of movable magnet 940 over/on the surface of porous medium 904 .
[0200] Reference is now made to FIG. 9 d , which schematically illustrates a top cross section view of a nebulizer 901 with a rotatable wetting mechanism, according to some embodiments. The rotatable wetting mechanism includes a displaceable/movable elongated member, such as a movable magnet 940 , which is placed on, or in close proximity to a surface of a porous medium, such as a porous disc 904 held within a nebulizer housing 902 . According to some embodiments, nebulizer 901 may also include a peripheral actuator configured to induce a change in the magnetic field flux in the environment of movable magnet 940 thereby induce a rotatable movement thereof 950 . According to some embodiments, peripheral actuator may be a ring actuator such as controllable electromagnet-ring 960 . According to some embodiments, movable magnet 940 is configured to be rotatable (arrows 950 ) and to spread/smear/distribute liquids on the surface of porous disc 904 , the liquids may be provided onto the surface of porous disc 904 , and According to some embodiments, the liquids may be provided to rotatable magnet 940 .
[0201] Reference is now made to FIG. 9 e , which schematically illustrates a side cross section of a nebulizer 900 with a rotatable wetting mechanism, according to some embodiments. According to some embodiments, nebulizer 900 is essentially similar to the nebulizer of FIG. 9 a , and further includes a flexible medication deploying end, such as flexible-conduit 948 which is connected to medication conduit 946 and is configured to provide/deploy medication on porous disc 904 According to some embodiments, flexible-conduit 948 is configured to reach near the surface of porous disc 904 , and to be flexibly movable by the rotation of movable magnet 940 for deploying medication at close proximity to the surface of porous disc 904 without obstructing the rotation/axial-movement thereof.
[0202] According to some embodiments, deploying medication near the surface of porous disc 904 via a flexible member, such as flexible-conduit 948 , may provide a homogeneous spreading of medication on the surface of porous disc 904 .
[0203] Reference is now made to FIG. 9 f , which schematically illustrates a top cross section view of a nebulizer 901 with a rotatable wetting mechanism, according to some embodiments. The rotatable wetting mechanism includes a displaceable/movable elongated member, such as a movable magnet 940 , which is placed on, or in close proximity to a surface of a porous medium, such as a porous disc 904 held within a nebulizer housing 902 . Movable magnet 940 is configured to be rotatable (arrows 950 ) and to spread/smear/distribute liquids on the surface of porous disc 904 , the liquids may be provided onto the surface of porous disc 904 , and According to some embodiments, the liquids may be provided to rotatable by a flexible medication deploying member, such as flexible-conduit 948 shown at a first location, and is flexibly movable (arrow 951 ) to a second location 949 by the rotation of movable magnet 940 .
[0204] Reference is now made to FIG. 9 g , which schematically illustrates a side cross section of a nebulizer 900 with a rotatable wetting mechanism, essentially as described in FIG. 9 a , according to some embodiments. According to some embodiments, nebulizer 900 further includes two spacers mounter/fastened on movable magnet 940 , such as a first Teflon™ ball 962 and second Teflon™ ball 964 , each being mechanically connected to one end of movable magnet 940 for elevating it from the surface of porous disc 904 and thereby improve the homogeneous spreading of the liquid and lead to production of controllable aerosol droplet size.
[0205] According to some embodiments, the two spacers may be integrally formed with the movable magnet. According to some embodiments, the two spacers are protrusions at the two ends of the movable magnet.
[0206] Reference is now made to FIG. 9 h , which schematically illustrates a top cross section of a nebulizer 900 with a rotatable wetting mechanism, essentially as described in FIG. 9 b , according to some embodiments. Depicted in FIG. 9 h are first Teflon™ ball 962 and second Teflon™ ball 964 , each being mechanically connected to one end of movable magnet 940 to prevent direct contact thereof with the surface of porous disc 904 .
[0207] Reference is now made to FIG. 9 i , which schematically illustrates a side cross section of a nebulizer 900 with a rotatable wetting mechanism, essentially as described in FIG. 9 a , according to some embodiments. According to some embodiments, nebulizer 900 further includes a spacer placed/mounted/integrated on the surface of porous disc 904 , such as a Teflon-ring 970 which is configured to elevate movable magnet 940 above the surface of porous medium 904 for providing spacing and preventing a direct contact therebetween. According to some embodiments, movable magnet 940 is tightened to Teflon-ring 970 , and is pulled towards porous disc by the magnetic field applied by motor magnet 942 . According to some embodiments, Teflon-ring 970 is configured to facilitate low-friction movement of movable magnet 940 thereon.
[0208] Reference is now made to FIG. 9 j , which schematically illustrates a top cross section of a nebulizer 900 with a rotatable wetting mechanism, essentially as described in FIG. 9 b , according to some embodiments. Depicted in FIG. 9 j is Teflon-ring 970 placed on the surface of porous disc 904 , to prevent direct contact thereof with the movable magnet 940 .
[0209] According to some embodiments, the spacing/distance/elevation between the surface of the porous medium and the movable magnet is approximately 100 micron (0.1 μm). According to some embodiments, the spacing/distance/elevation between the surface of the porous medium and the movable magnet is in the range of 50 micron (0.05 μm) to 150 micron (0.15 μm). According to some embodiments, the spacing/distance/elevation between the surface of the porous medium and the movable magnet is in the range of 20 micron (0.02 μm) to 200 micron (0.2 μm).
[0210] According to some embodiments, the term “approximately” may refer to the distance between the surface of the porous medium and the movable magnet, an thus may refer to values within the range of 20% or less from the value indicated. For example, a spacing/distance/elevation of approximately 100 micron (0.1 μm) includes values within the range of 80-100 micron.
[0211] Without being bound by any theory or mechanism of action, the distance between the surface of the porous medium and the movable magnet seems to result with advantageous droplet size distribution, possible due to an improved wetting mechanism.
[0212] Reference is now made to FIG. 10 , which schematically illustrates nebulizer 1000 with a rotatable wetting mechanism and a liquid deploying structure 1046 , according to some embodiments. Liquid deploying mechanism, such as liquid conduit 1046 is configured to deploy/provide liquids to the surface of a porous medium 1004 and a rotatable magnet 1040 is placed on the surface of porous medium 1004 and is configured to be movable thereon and to homogeneously or semi-homogeneously spread the liquids provided by liquid conduit 1046 on the surface of porous medium 1004 . The wetting mechanism further comprises an actuator having, according to some embodiments, a control-magnet 1042 magnetically/mechanically associated with rotatable magnet 1040 and rotated by a motor 1044 .
[0213] When a pressure gradient is applied on porous medium 1004 , a mist/aerosol of multiple droplets is released from the wetted/damped/moistened surface of porous medium 1004 .
[0214] According to some embodiments, motor 1044 may comprise a brushed or brushless DC motor, for example a steppe moto or the like. According to some embodiments, motor 1044 may comprise an AC motor, such as an induction motor or the like.
[0215] Reference is now made to FIG. 11 , which schematically illustrates a nebulizer 1100 with a rotatable wetting mechanism and a liquid absorbing material, such as sponge 1102 , according to some embodiments. Liquid absorbing material is placed on a surface of a porous medium 1104 and configured to reversibly contain/absorb liquids, and release the liquids with changed physical conditions such as pressing. A movable elongated spreader/presser, such as rotating rod 1140 , is placed on sponge 1102 and is configured to press at least some portions thereof against the surface of porous medium 1104 , thereby force the release of absorbed liquids from sponge 1102 . The moving of rotating rod 1140 is induced/caused by the rotating displacement of an actuator that is mechanically and/or magnetically associated with rotating rod 1140 . According to some embodiments, rotating rod 1140 may be movable/rotatable by inducing magnetic field changes in the environment thereof, and the actuator includes a magnetic-field inducer 1142 rotatable by a motor 1144 and configured to induce the rotation/displacement of rotating rod 1140 on sponge 1102 thereby pressing against various areas thereon and controllably releasing liquid to the surface of porous medium 1104 .
[0216] When a pressure gradient is applied on porous medium 1104 , a mist/aerosol of multiple droplets is released from the wetted/damped/moistened surface of porous medium 1104 .
[0217] Reference is now made to FIG. 12 , which schematically illustrates a side cross section of a nebulizer assembly 1300 with a rotatable wetting mechanism, according to some embodiments. Nebulizer 1300 includes a housing 1302 with an inlet orifice 1310 , an outlet orifice 1312 , a liquid conduit 1346 and a pressure-sensor conduit 1348 . Nebulizer 1300 further includes a rotatable spreading mechanism, such as spreading elongated magnet 1340 placed on a surface of a porous disc 1304 for spreading liquids thereon, an actuator within housing 1302 is associated with spreading elongated magnet 1340 , the actuator includes a motor 1344 mechanically connected to a motor-magnet 1342 and is configured to rotate spreading elongated magnet 1340 for spreading liquids on the surface and/or through the pores of porous disc 1304 . According to some embodiments, liquid conduit 1346 is configured to provide liquids to a central section of spreading elongated magnet 1340 .
[0218] Reference is now made to FIG. 13 , which schematically illustrates a nebulizer system assembly 1700 with a rotatable wetting mechanism, according to some embodiments. Nebulizer system assembly 1700 includes various functional, control and/or indicatory components. For exemplary purposes, system assembly 1700 includes a nebulizer, a gas pump for providing pressurized gas to the nebulizer, a pressure sensor, control gauges and buttons and others.
[0219] The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting. As used herein, the singular forms “a”, “an” and “the” are intended to include the plural forms as well, unless the context clearly indicates otherwise. It will be further understood that the terms “comprises” or “comprising,” when used in this specification, specify the presence of stated features, integers, steps, operations, elements, or components, but do not preclude or rule out the presence or addition of one or more other features, integers, steps, operations, elements, components, or groups thereof.
[0220] While a number of exemplary aspects and embodiments have been discussed above, those of skill in the art will recognize certain modifications, additions and sub-combinations thereof. It is therefore intended that the following appended claims and claims hereafter introduced be interpreted to include all such modifications, additions and sub-combinations as are within their true spirit and scope.
EXAMPLES
Example 1
Measurements of Water Aerosol Droplet Diameter
[0221] The cumulative droplet size distribution of an aerosolized aqueous solution of a water soluble dye produced using a nebulizer according to some embodiments, in the absence or presence of a sponge was tested. The results, presented in FIG. 6 (square—with a sponge; triangle—without a sponge) indicate that in the presence of a liquid absorbing material about 100% of the droplets have diameters of less than 5 microns, wherein 80% of the droplets have diameter of less than 1 micron. However, in the absence of a liquid absorbing material, only about 70% of the droplets have a diameter of less than 5 microns.
Example 2
Measurements of Viscous Water Aerosol Droplet Diameter
[0222] The cumulative droplet size distribution of an aerosolized aqueous solution of a water soluble dye containing glycerol (5%) produced using a nebulizer according to some embodiments, in the absence or presence of a sponge was tested. The results, presented in FIG. 7 (square—with a sponge; triangle—without a sponge) indicate that in the presence of a liquid absorbing material about 95% of the droplets have a diameter of less than 5 microns, wherein 85% of the droplets have a diameter of less than about 2 micron. However, in the absence of a liquid absorbing material, only about than 60% of the droplets have a diameter of less than 5 microns.
Example 3
Measurements of Aerosol Droplet Diameter of a Pharmaceutical Composition
[0223] The cumulative droplet size distribution of commercial Ventolin® (5 mg/ml albuterol) aerosol produced using a nebulizer according to some embodiments, in the presence of a sponge was tested. The results, presented in FIG. 8 indicate that about 90% of the droplets have a diameter of less than 9 microns, wherein 80% of the droplets have a diameter less than 5 microns.
Example 4
Measurements of Aerosol Droplet Diameter Produced by a Nebulizer Having a Wetting Mechanism and a Liquid Absorbing Material
[0224] The cumulative droplet size distributions for different aqueous formulations of a water soluble dye (Formulations 1-7), Ventolin™ and insulin was measured ( FIG. 14 )—Droplet size distributions were obtained using a cooled next generation impactor (NGI) operated at a flow rate of 15 liters/min. The results indicate that the values of mass median aerodynamic diameter (MMAD) and Geometric Standard Diameter (GSD) vary within the range of about 0.4-7 μm and about 2-5 (two to five) μm, respectively.
[0225] The fine (below 5 μm) and extra fine (below 3 μm) particle fractions obtained for the different formulations are presented in FIG. 15 .
Example 5
Analysis of Aerosol Droplet Diameter
[0226] Distribution of mass on Next generation impactor (NGI) plates for various aqueous formulations (2, 5 and 6) containing a soluble dye tracer having different physiochemical properties is presented in FIG. 16 . Formulations 2, 5 and 6 were selected for the following reasons: formulation 2 provides very small droplets suitable for systemic delivery, formulation 6 gives droplets at a size suitable for delivery to the central airways, and formulation 5 gives large droplets suitable for nasal delivery. The results highlight the advantage of the nebulizers disclosed herein: the aerosols obtained using the nebulizers may be used for targeting pharmaceutical compositions to various areas of the respiratory system.
[0227] An additional important aspect presented in FIG. 16 is the modality of the size distribution. By designing the formulation with proper liquid spreading, the modality may be controlled. For example, using an appropriate formulation, the modality may be changed from uni-modal to bi-modal and even tri-modal.
Example 6
Analysis of Aerosol Droplet Delivery
[0228] Cumulative size distribution plots, for formulations of Ventolin™ and insulin, was measured using NGI ( FIG. 17 ). As shown in the figure, the MMAD obtained for Ventolin™ is around 2.5 microns, which is conducive for the delivery of bronchodilators to the central airways. On the other hand, the MMAD for insulin is lower than 1 micron, which is conducive for delivery into the deep lung and hence for systemic uptake.
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The present disclosure generally relates to the field of nebulizers for aerosol generation and methods of using same for treating diseases and disorders.
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PRIORITY
[0001] This application is a continuation of U.S. Utility patent application Ser. No. 11/730,250 filed Mar. 30, 2007 and issued as U.S. Pat. No. 7,735,573 on Jun. 15, 2010, which, in turn, claims the benefit of U.S. Provisional Application Ser. No. 60/789,368 filed Apr. 5, 2006, the respective contents of which are incorporated by reference herein in their entirety.
TECHNICAL FIELD OF THE INVENTION
[0002] The present invention relates generally to a tool for perforating lawn and garden areas in preparation for seed applications. More particularly, the invention relates to a lawn perforating tool and method of using same to prepare new lawn or garden areas or distressed regions of existing lawns or gardens for the planting of new seed, for example grass seed, clover seed, wildflower seed, and the like.
BACKGROUND OF THE INVENTION
[0003] Diseases, pests, irrigation difficulties and other factors can create regions of dead and/or dying grass and/or bare soil in existing lawns. Prior to sowing seed in these regions, so as to restore the lawn, one must first prepare the ground for planting. To that end, it is necessary to produce indentations or holes (also referred to herein as “perforations”) in the lawn, preferably of a depth and size that maximizes seed-to-soil contact and is suitable for the germination of seed placed therein. The distribution of the holes must have density sufficient to allow the resulting plant growth to form a continuous grassy surface. In addition, it is desirable to provide spacing between the holes, and to the pattern the holes in a non-uniform manner to thereby prevent the resulting grass from having a visually objectionable pattern. A tool optimized for this utility should also be capable of tilling or plowing the neighboring earth; in particular, it is desirable to push up and loosen the soil around the hole so as to create a soft mound of soil that will readily crumble around the seed after watering. Finally, it is further desirable to configure the tool to minimize operator fatigue and muscle strain or, alternatively, to work in conjunction with a powered implement, such as a tractor or small engine.
[0004] There are a number of commercially available tools designed to loosen, cut, crumble and/or cultivate garden soil or the like. For example, U.S. Pat. Nos. 3,605,907 (Schuring et al.), 4,424,869 (vom Braucke et al.), and 4,678,043 (vom Braucke et al.) disclose various small hand tools specifically designed for such purposes. In addition, a variety of manual and automated lawn seeding machines are known in the art. However, none of the presently available options are capable of producing the optimized lawn perforations as described above while at the same time maximizing efficiency and minimizing operator fatigue. Thus, there remains a clear need in the art for a lawn tool capable of efficiently and effectively preparing a damaged area of lawn for reseeding. The present invention is directed to such a need.
SUMMARY OF THE INVENTION
[0005] In view of the foregoing, it is a primary object of the present invention to provide an improved lawn perforating tool which allows a user to prepare a new lawn area or damaged area of lawn for seeding. To that end, the present invention provides a unique lawn perforating tool having working head composed of a series of intersecting, non-planar, wheel-like perforating plates that freely rotate about a working head axle, each of the perforating plates provided with two or more angled radial arms particularly configured to not only penetrate soil to a desired depth but also produce a non-uniform pattern of perforations optimal for new growth.
[0006] It will be understood by those skilled in the art that one or more aspects of this invention can meet certain objectives, while one or more other aspects can meet certain other objectives. Each objective may not apply equally, in all its respects, to every aspect of this invention. As such, the following objects can be viewed in the alternative with respect to any one aspect of this invention.
[0007] It is, accordingly, an object of this invention to provide a lawn perforating tool which allows a user to prepare a lawn, particularly one or more damaged lawn areas, for seeding (or reseeding).
[0008] It is also an object of this invention to provide a lawn perforating tool which produces indentations or holes having non-uniform, irregular spacing and a controlled depth in areas of soil and dead grass.
[0009] It is further an object of the present invention to provide a lawn perforating tool that penetrates the soil in a sideways direction, creating an optimally sized, shaped, and positioned hole that can readily receive seed. In a preferred embodiment, this sideways action provides the tool with a tilling or plowing action, by loosening, and/or softening neighboring soil and creating soft mounds of soil that will readily crumble around a seed after watering.
[0010] It is further an object of this invention to provide a lawn perforating tool that prepares lawn areas for seeding while minimizing operator fatigue. To that end, in a preferred embodiment, it may be desirable to include an adjustable handle portion, for example utilizing telescoping shafts or tubes, and/or one or more ergonomic, elastomeric hand grips. In another embodiment, the lawn perforating tool may be coupled to powered implement such as a tractor of small engine.
[0011] These and other objects and features of the invention will become more fully apparent when the following detailed description is read in conjunction with the accompanying figures and examples. However, it is to be understood that both the foregoing summary of the invention and the following detailed description are of a preferred embodiment, and not restrictive of the invention or other alternate embodiments of the invention. In particular, while the invention is described herein with reference to a number of specific embodiments, it will be appreciated that the description is illustrative of the invention and is not constructed as limiting of the invention. Various modifications and applications may occur to those who are skilled in the art, without departing from the spirit and the scope of the invention, as described by the appended claims.
[0012] Likewise, other objects, features, benefits and advantages of the present invention will be apparent from this summary and certain embodiments described below, and will be readily apparent to those skilled in the art. Such objects, features, benefits and advantages will be apparent from the above as taken into conjunction with the accompanying examples, data, figures and all reasonable inferences to be drawn therefrom, alone or with consideration of the references incorporated herein.
BRIEF DESCRIPTION OF THE DRAWINGS
[0013] Various aspects and applications of the present invention will become apparent to the skilled artisan upon consideration of the brief description of the figures and the detailed description of the present invention and its preferred embodiments which follows:
[0014] FIG. 1 depicts a single shaft embodiment of a lawn perforating tool designed in accordance with the principles of the present invention.
[0015] FIG. 2 depicts a double shaft embodiment of a lawn perforating tool designed in accordance with the principles of the present invention.
[0016] FIG. 3A depicts a portion of a lawn having dead and dying grass, and bare soil following preparation for planting with seed using a lawn perforating tool designed in accordance with the principles of the present invention. FIG. 3B depicts a hole created in soil by a lawn perforating tool designed in accordance with the principles of the present invention, more particularly a plurality seeds filling the hole. The mouth of the hole is sufficiently wide so as to readily accept seeds. The hole then tapers to a small niche, the taper funneling seeds down to contact the soil, enhancing seed-to-soil contact which is critical to germination.
[0017] FIGS. 4A and 4B present perspective and front elevational views, respectively, of a first embodiment of the perforating plates of the present invention.
[0018] FIG. 5 is a perspective view of the perforating plates of FIG. 4 assembled in coordinating arrangement as rotatable subassemblies.
[0019] FIG. 6 is a front elevational sectional view of the objects of FIG. 5 .
[0020] FIG. 7 is an exploded view of the perforating plates of a second embodiment, prior to assembly as facing pairs.
[0021] FIG. 8 is a perspective view of the facing pair of the perforating plates of FIG. 7 in mating engagement.
[0022] FIG. 9 is an exploded perspective view depicting the engagement between opposing spikes and spike supports of the engaged pair of perforating plates of FIG. 8 .
[0023] FIG. 10 is a front elevational sectional view depicting the engagement between opposing spikes and spike supports of the engaged facing perforating plates of FIG. 8 as well as the inclusion of the intervening spacer element.
[0024] FIG. 11 is a perspective view of exemplary telescoping handles that may be used in accordance with a lawn perforating tool of the present invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0025] Although any methods and materials similar or equivalent to those described herein can be used in the practice or testing of embodiments of the present invention, the preferred methods, devices, and materials are now described. However, before the present materials and methods are described, it is to be understood that this invention is not limited to the particular sizes, shapes, dimensions, materials, methodologies, protocols, etc. described herein, as these may vary in accordance with routine experimentation and optimization. It is also to be understood that the terminology used in the description is for the purpose of describing the particular versions or embodiments only, and is not intended to limit the scope of the present invention which will be limited only by the appended claims.
[0026] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. However, in case of conflict, the present specification, including definitions, will control.
[0027] In the context of the present invention, the following definitions apply:
[0028] The words “a”, “an” and “the” as used herein mean “at least one” unless otherwise specifically indicated. Thus, for example, reference to a “rotatable plate” is a reference to one or more such plates and equivalents thereof known to those skilled in the art, and so forth.
[0029] The term “proximal” as used herein refers to that end or portion which is situated closest to the user of the device, farthest away from the working head and earthen area being treated. In the context of the present invention, the proximal end of the inventive device includes the handle portion.
[0030] The term “distal” as used herein refers to that end or portion situated farthest away from the user of the device, closest to the earthen site. In the context of the present invention, the distal end of the inventive device includes the working head and plurality of rotatable perforating plates.
[0031] The term “rotational” is used herein to refer to the revolutionary movement of the perforating plates, more particularly paired plate assemblies, about the axle. In the context of the present invention, rotation of the paired plate assemblies results in the production holes or indentations (i.e., perforations) in the soil, such perforations having size and shape optimized for receiving grass seed and present in a random or non-uniform pattern of perforations therein.
[0032] The term “axial” as used herein refers to the direction relating to or parallel with the longitudinal axis of the device. In the context of the present invention, the application of axial force to the device by the user, for example by pushing the handle portion and/or pressing the optional foot bar, results in both a downward pressure that drives the sharpened tines (i.e., spikes) of the perforating plates into the soil so as to produce one or more holes or indentations (i.e., perforations) in the soil suitable for receiving seeds, for example grass seeds, and a forward pressure that drives the rotation of the paired plate assemblies, which, in turn, results a random pattern of perforations in the soil.
[0033] As used herein, the term “tapered” refers to a gradual decrease in size toward a sharp point or tip. Likewise, the term “beveled” is used herein to refer to a surface or end that is slanted or inclined, at an angle other than 90 degrees. In the context of the present invention, each perforating plate is comprised of a plurality of radially projecting arms. In one embodiment, the free ends of the arms may be tapered spikes or tines, each of which is provided with a sharp knife-like edge. In another embodiment, the free arm ends are alternately tapered or beveled. The tapered arms are referred to herein as spikes or tines while the beveled arms are referred to as spike supports. In either embodiment, the spikes should be sufficiently sharp, provided with one or more cutting edges capable of slicing grass and puncturing soil, thereby creating holes or indentations (“perforations”) sized and shaped to readily receive grass seed and allow it to germinate and grow. More particularly, each spike is preferably sized and shaped to yield a perforation the can receive 1 to 5 seeds, more preferably 2 to 4 seeds, thereby avoiding the problems of overlapping and crowding of grass seed which, in turn, can result in dampening off or seed rot. To that end, the length of each spike is preferably 1 to 4 inches, more preferably about 3 inches.
[0034] As used herein, the term “acute” refers to an angle that is less than 90 degrees. Conversely, the term “obtuse” refers to an angle that is more than 90 degrees.
[0035] As used herein, the term “convex” refers to a surface or boundary that curves or bulges outward, as the exterior of a sphere. Conversely, the term “concave” refers to surface or boundary that curves inward, as the inner surface of a sphere. The perforating plates of the present invention have overall non-planar configuration that may be described as “convex” or “concave”, depending upon the point of reference. This configuration results from the fact that at least one of the radially projecting arms of each penetrating plate is disposed at an angle relative to a central bore axis. This angled arrangement allows one or more of the radial arms to penetrate the soil in a sideways direction, thereby creating holes of optimized size, shape, depth, and density.
[0036] As discussed above, the lawn perforating tool of the present invention is composed of a handle portion and a working portion. The handle portion preferably includes one or more drive shafts. It is desirable for each drive shaft to be “fitted” to the intended user or application, for example through the use of telescoping tubes that allow the overall length of the drive shaft to be adjusted as needed. In addition, depending upon the application, each drive shaft may be relatively straight or bent, at a fixed or adjustable angle. Each drive shaft is preferably formed from a suitably rigid and durable material capable of withstanding without bending. Examples of such materials include metals, particularly steel, iron and aluminum, and rigid plastics such as thermoset polyurethane, polycarbonates, and PVC. Materials with a tensile strength of at least 7,000 Psi, more preferably at least 10,000 Psi, even more preferably 12,000 Psi or higher are most suitable. The selected material be initially fabricated and subsequently formed into one or more tool components using any conventional process, for example through casting, molding or extrusion processes.
[0037] When designed for human powering, each drive shaft is preferably provided with one or more hand grips. The one or more hand grips are preferably formed from a soft elastomeric material, such as rubber, thermoplastic polyolefins, and polyethylenes. In one preferred embodiment, the hand grips are slidably disposed about the proximal end of the drive shafts and provided with one or more finger recesses. In a preferred embodiment, the hand grips extend from the drive shaft in a relatively transverse fashion. In certain preferred embodiments, the relative angle between each hand grip and drive shaft may be adjusted to suit the individual user or intended use.
[0038] When designed for use with a powered or motorized implement, such as tractor or small engine, the drive shaft(s) may be provided with a connecting means, for example a cupped element designed to engage a standard trailer hitch.
[0039] In contrast to conventional tools for loosening, cutting or crumbling garden soil, most of which are hand tools, the lawn perforating device of the present invention is in one embodiment designed to be powered by a user's leg or foot, with the user's hands serving to hold the device upright and guide it along its intended path. By placing one's foot on the working head end, foot pressure combine with human weight to drive the wheels in a downward direction, forcing the spikes to the requisite depth for seed germination (typically about 1 to 2 inches). Furthermore, moving the working head over grass areas in a back and forth fashion with one's leg or foot results in a random pattern of holes or indentations. This non-uniform hole pattern provides the best possible opportunity for seed to knit together to, in turn, create a uniform lawn. In contrast, conventional seeding tools typically plant seeds in rows, leaving obvious areas of bare soil.
[0040] In the context of the present invention, the working portion or working head of the lawn perforating tool of the present invention is mounted to the distal end of the handle portion, in a generally transverse direction. At a minimum, the working head is comprised of one or more non-planar perforating plates rotatably disposed about one or more axles. Although the number of perforating plates is not critical, for optimal performance it is preferable to utilize an even number of plates arranged in paired assemblies as discussed in detail below. In a preferred embodiment, the working head is provided with two to twenty plates, more preferably four to eighteen, even more preferably eight to sixteen. In that it is preferable to arrange the perforating plates along the axle in coordinating pairs, it is desirable to provide the working head with an even number of plates. To that end, the present invention contemplates a small version, comprised of about 2 to 6 plate pairs, as well as a larger version comprised of about 6 to 16 plate pairs. In addition, the present invention contemplates a working head composed of multiple axles, such an embodiment being particularly suited for use in conjunction with a motorized implement or engine or for being towed behind a tractor or the like.
[0041] The working head may also include a frame member, optimally composed of a foot bar mounted above and parallel to one or more axles, said foot bar and axle(s) connected at either end by a pair of side arms. The foot bar may optionally be fitted with a non-slip surface or coating, for example a grip tape layer or knurled metal surface. Each axle preferably comprises a straight shaft that distributes energy evenly across the perforating plates so as to allow for the application of a force sufficient to accomplish the creation of holes at the correct depth.
[0042] Each perforating plate is comprised of a central bore, sized to allow the working head axle to slide therethrough, and a plurality of radially projecting arms extending therefrom. Although the number of radial arms is not critical to the present invention, in a preferred embodiment each perforating plate is provided with two to twelve arms, more preferably four to ten, even more preferably four to eight. As noted above, over, one or more of the radial arms disposed at an angle relative to the axle, thereby affording each plate with a non-planar appearance, optimally a concave or convex configuration, depending upon the point of reference. The angled disposition of the radial arms provides the tool with a sideways “plowing” action that yields optimized indentations in the soil. Although the invention is not limited to a particular configuration, in order to achieve the sideways plowing action, it is preferable that the angle formed by each plate arm relative to a plane that includes the central bore axis of the plate ranges from 5 to 45 degrees, more preferably 10 to 30 degrees, even more preferably 10 to 20 degrees.
[0043] In a preferred embodiment, the perforating plates are arranged about the axle is coordinating pairs, referred to herein a rotatable subassemblies. In assembly, first and second concave plates are arranged in an offset facing relationship, such that the radially projecting spikes of the first plate interlace with those of the second plate. More particularly, in one preferred embodiment, each tapered arm (or spike) of the first plate extends between two opposing tapered arms (or spikes) of the second plate and vice versa. When the beveled spike supports are utilized, it is preferable that the beveled ends of each spike support of the first plate rests snugly against the surface of an opposing spike on the second plate and vice versa. This arrangement of opposing arms not only affords support to the spikes when penetrating soil, thereby allowing user to apply more pressure so as to reach a depth critical for seed germination, but also enhances the overall shape of the hole that each spike creates. In particular, the hole narrows from a wide mouth to a small niche hole. The wide opening is more accepting of seed spread across it (i.e., catches seeds more easily) and the narrowing furrow funnels the seed down to contact the soil, enhancing the soil to seed contact which is important for seed germination. The spike support also creates more of a plowing action. In use, it pushes up and loosens soil around the hole. The sideways puncture and the enhanced plowing together yield a soft mound of soil that will readily crumble around the seed after watering, causing increased soil to seed contact.
[0044] To maintain the coordinating relationship between paired plates, it is desirable to affix the plates to the axle, for example by means of brazing or welding, or alternatively to affix each plate to the other, for example by means of a spacer mechanism. The spacer should not only provide the requisite fixed axial separation between paired plates but also maintain correct alignment of neighboring radial arms and prevent relative movement between paired plates, thereby allowing the paired plates to form single rotatable subassembly. In that the spacer may also be slidably received about the axle, it too may be afforded with a central bore. Thus, in one preferred embodiment, the spacer takes the form of a tubular sleeve. To maintain the paired plates and intermediately disposed spacer as a fixed assembly, it may be desirable to provide each with engaging elements, for example screws and mating screw threads. Alternatively, the spacer sleeve may be provided with a plurality of splines that engage a keyway disposed in the central bore of one or more plates. Other fastening mechanisms are contemplated, including more permanent fastening means such as welding and brazing. In other embodiments, the rotatable paired plate subassemblies may be fabricated as a single unit, thereby avoiding the need to maintain axial separation and alignment.
[0045] In addition to providing a spacer element between facing plates, it may also be desirable to include a second spacer element to separate adjacent paired assemblies. Like the first spacer element(s), the second spacer element(s) may be permanently or removably affixed to its neighboring plates. Alternatively, the spacers may simply slide freely along the axle plate pairs.
[0046] The lawn perforating device of the present invention is designed to slice through dead grass then puncture the lawn soil, which is often quite hard. Furthermore, in order to achieve germination, it is important that the holes in the soil extend to a sufficient depth. Although seeds may be capable of germinating at depths of less than one inch or greater than two inches, for optimal germination it is preferable to utilize a depth of about 1 to 2 inches. Thus, it is clear that a certain amount of user strength and device integrity is required. The cupped and interlaced perforating plates of the lawn perforating tool of the present invention provide the needed rigidity to apply sufficient force to accomplish the creation of the holes at the necessary depth, typically about 1 to 2 inches. Bending of the spikes will cause the wheels to rotate and roll in a rough and uneven manner which, in turn, results in poor performance or failure of the device. As discussed above, the interlacing of the radial arms gain support from each other, thus preventing bending from applied force. Nevertheless, it is still desirable to construct the perforating plates and their radial arms of high tensile strength material sufficient to accomplish the creation of holes at the necessary depth without bending. Illustrative examples of such materials include, but are not limited to, stamped aluminum, laser cut aluminum, or other cast or cut metals, as well as certain hard plastics.
[0047] Hereinafter, the present invention is described in more detail by reference to Figures and Examples. However, the following materials, methods, figures, and examples only illustrate aspects of the invention and are in no way intended to limit the scope of the present invention. As such, methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention.
[0048] Multiple embodiments of the lawn perforating device of the present invention are contemplated herein. FIG. 1 depicts one embodiment of the lawn perforating tool of the present invention, tool 100 having an elongated proximal portion 104 forming a handle having a proximal portion 104 and a distal portion 106 . In a preferred embodiment, proximal portion 104 is offset from distal portion 104 at an angle 112 . Proximal portion 104 has at its proximal end single hand grip 108 , and at its distal end transverse element 110 from which extend a pair of hand grips 111 A and 111 B, grips 108 , 111 A, and 111 B being formed from a suitable flexible and/or elastomeric material. Distal portion 106 has at its distal end and mounted thereto transverse assembly 114 having a rigidly mounted frame portion 116 , and paired plate subassemblies 118 rotatably mounted to portion 116 .
[0049] Depending on the size of the damaged lawn area, one may opt for a smaller version ( FIG. 1 ) or larger version ( FIG. 2 ). For example, insect infestation, drought and disease situations typically result in large areas of damaged lawn. Accordingly, a larger model would be preferred. As shown in FIG. 2 , in addition to a pair of longer shafts ( 204 , 206 ), each of which is provided with hand grips ( 211 A, 211 B formed from a suitable flexible and/or elastomeric material, the larger version ( 200 ) is further provided with additional paired plate subassemblies 218 rotatably mounted to portion 216 to allow coverage of a large area in less time and with less effort. Conversely, pets spot areas and areas along curbs tend to be smaller, more confined, and thus are more suited for treatment with the smaller model of FIG. 1 . As shown in FIG. 1 , the smaller model is provided with more concentrated spiking so as to confine perforating to the target damaged area and avoid puncturing healthy areas of the lawn. This concentrated effort maximizes efficiency while minimizing user fatigue. In either embodiment, the handle portion may be straight or optionally bent, for example at the midpoint, to maximize downward pressure and concentrate effort.
[0050] FIG. 3A depicts a portion of a lawn having dead and dying grass, and bare soil following preparation for planting with seed using a lawn perforating tool designed in accordance with the principles of the present invention. Specifically, lawn portion 2 has regions 4 of live grass, regions of dead grass 6 , and regions 8 with no grass. Perforations 10 formed by an implement formed in accordance with the principles of this invention, are of a size and depth suitable for the germination of grass seed placed therein. Perforations 10 occur in regions 6 of dead grass and regions 8 of bare soil. The pattern of perforations 10 when viewed in plan view as in FIG. 3A , have an irregular spacing formed by a unique mechanism of the implement and method herein disclosed.
[0051] FIG. 3B depicts a hole 20 created in soil 21 by a lawn perforating tool designed in accordance with the principles of the present invention, more particularly a plurality seeds 22 filling the hole. As depicted, the mouth 23 of the hole is sufficiently wide so as to readily accept one or more seeds, preferably one to five seeds. The hole then tapers to a small niche 24 , the taper funneling seeds down to contact the soil, enhancing seed-to-soil contact which is critical to germination.
[0052] FIGS. 4A , 4 B, and 5 provide front elevational and perspective views of a first embodiment of the perforating plates of the present invention. FIG. 6 is a front elevational sectional view of the objects of FIG. 5 . Each subassembly 118 is composed of first perforating plate 120 , second perforating plate 122 , and spacer 124 , plates 120 and 122 being optionally secured to spacer 124 by welding, brazing or other suitable mechanical fastening means. In one preferred embodiment, plates 120 and 122 are secured to spacer 124 by welding. Perforating plates 120 and 122 are each provided with a plurality of radial arms 126 of width 128 , angularly spaced by angle 130 to create angular spaces 131 therebetween. Arms 126 terminate in tapered portions 132 forming knife edges 134 , herein referred to as “spikes”. Spikes 126 are formed to angle 136 with a plane normal to axis 138 of spacer 124 . Assembly 118 has a central bore or hole 142 of diameter 140 formed therethrough.
[0053] Multiple subassemblies are aligned for assembly onto an axle through axial holes 142 . As seen in FIG. 5 , first subassembly 250 is separated from second subassembly 252 by second spacer 254 , which is preferably not affixed to either subassembly. Radial arms 126 (designated 226 ) of first subassembly 250 adjacent to second subassembly 252 are positioned within angular spaces 131 (designated 231 in FIGS. 5 and 6 ) of second subassembly 252 . Arms 126 (designated 326 in FIGS. 5 and 6 ) of second subassembly 252 are positioned within angular spaces 131 (designated 331 in FIGS. 5 and 6 ) of first subassembly 250 . This relative positioning and loose meshing of arms 226 and 326 of adjacent subassemblies 118 allows first subassembly 250 to be angularly displaced (i.e., offset) relative to second subassembly 252 , the maximum amount of relative displacement being determined by width 128 of spikes 126 , and the angular spacing 130 between arms 126 . Arms 126 of subassemblies 250 and 252 together form a wedge having an included angle 156 equal to twice angle 136 .
[0054] FIGS. 7-10 depict an alternate embodiment of perforating plate and assembled plate pairs. Like the above-described embodiments, each subassembly 718 is composed of first perforating plate 720 , second perforating plate 722 , and spacer 724 . Assembly 718 has a central bore or hole 742 of diameter 740 formed therethrough. Plate 720 may be optionally secured to plate 722 via spacer 724 . In the embodiment depicted, the spacer is attached to first plate 720 and provided at its distal end with a series of splines 50 that interlock with the mating keyway 51 provided in the axial hole 742 of opposing plate 722 . Perforating plates 720 and 722 are each provided with a plurality of angularly spaced radial arms 726 .
[0055] Unlike the previous embodiment, the herein depicted alternate embodiment utilizes plates comprised of alternating tapered spikes 727 and spike supports 728 . Spikes 727 terminate in tapered portions 732 forming knife edges 734 . Both spikes and spike supports are preferably disposed at an angle 736 with a plane normal to axis 738 of spacer 724 . As best shown in FIG. 9 , when assembled in coordinating facing pairs 718 , the beveled ends 729 of each spike support 728 of a first plate rests snugly against a side surface 730 of an opposing spike 727 on a second plate and vice versa.
[0056] This offset arrangement of opposing arms not only affords support to the spikes when penetrating soil, thereby allowing user to apply more pressure so as to reach a depth critical for seed germination, but also enhances the overall shape of the hole that each spike creates. In particular, the hole narrows from a wide mouth to a small niche hole. The wide opening is more accepting of seed spread across it (i.e., catches seeds more easily) and the narrowing furrow funnels the seed down to contact the soil, enhancing the soil to seed contact which is important for seed germination. The spike support also creates more of a plowing action. In use, it pushes up and loosens soil around the hole. The sideways puncture and the enhanced plowing together yield a soft mound of soil that will readily crumble around the seed after watering, causing increased soil to seed contact.
[0057] When assembled, the working head comprises a plurality of subassemblies 718 , the arms 726 of adjacent subassemblies loosely meshing so as to allows angular displacement between adjacent subassemblies 718 . Subassemblies 718 and spacers are designed to rotate freely on axle.
[0058] During use, downward force is applied to distal assembly 114 using handle 102 such that protrusions 126 are forced into the soil as assembly 114 is traversed over a region of dead grass and soil. Because subassemblies 118 and 718 are able to angularly displace from each other during rotation, the pattern of holes produced is non-uniform in spacing. The depth of the holes is determined by the downward force applied to the workhead and the wedge angle between angled arms 126 and 726 . Holes produced in this manner are optimal for the germination of seed placed therein.
[0059] In preferred embodiments, subassemblies 118 and 718 are formed from a suitably durable, high tensile strength material, for example a metallic material, polymeric material, or composite material.
[0060] In the embodiments herein described subassemblies 118 and 718 rotate on an axle mounted at its end to endplates. In other embodiments distal end 106 of elongated portion 102 is affixed to the center point of an axle and subassemblies 118 and 718 rotate on lateral portions of the axle.
[0061] Arms 126 and spikes 727 of the embodiments herein described are radial, of a constant width, and have a tapered end terminating in a knife-edge. Other embodiments are anticipated in which arms 126 have other, more complex shapes. For instance, the arms may be tapered over their entire length, and/or may terminate in a blunt end (e.g., spike support 728 ). Similarly, the arms may be disposed at an angle relative to a radial line when viewed in plan view. The number of protrusions on each plate may be increased or decreased.
[0062] Any embodiment of the lawn perforating tool of the present may be equipped with telescoping handles to ergonomically fit any body type. It is important that the tool be adjusted proportionately to the person using it as the action of the working head with leg/foot/arm requires the correct handle length to work comfortably and effectively. Furthermore, through correct adjustment of the telescoping handle, one can maximize the efficiency of energy transfer needed for effective use, i.e., to drive the spikes to the requisite 1 to 2 inch depth of soil penetration. An exemplary embodiment of telescoping handles, including relatively slidable proximal and distal shafts 304 and 306 ) is depicted in FIG. 11 . Handles 311 A and 331 B may optionally be fitted with elastomeric covers (not shown) as desired.
INDUSTRIAL APPLICABILITY
[0063] The lawn perforating tool of the present invention is ideally suited to repairing damaged areas of existing lawn and preparing such for reseeding.
[0064] All patents and publications mentioned herein are incorporated by reference in their entirety. Nothing herein is to be construed as an admission that the invention is not entitled to antedate such disclosure by virtue of prior invention.
[0065] While the invention has been described in detail and with reference to specific embodiments thereof, it is to be understood that the foregoing description is exemplary and explanatory in nature and is intended to illustrate the invention and its preferred embodiments. Through routine experimentation, one skilled in the art will readily recognize that various changes and modifications can be made therein without departing from the spirit and scope of the invention. For example, the invention disclosed could be provided with, for example, a larger or smaller handle, a motor and/or other attachments without departure from the spirit of the invention.
[0066] Other advantages and features will become apparent from the claims filed hereafter, with the scope of such claims to be determined by their reasonable equivalents, as would be understood by those skilled in the art. Thus, it should be understood that the invention is not intended to be defined by the foregoing description, but rather by the appended claims and their equivalents.
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Disclosed herein is a lawn perforating tool and method of using same to prepare new lawn or garden areas or distressed regions of existing lawns or gardens for the planting of seed, example of which include, but are not limited to, grass seed, clover seed, wildflower seed, and the like. The lawn perforating tool of the present invention is particularly configured to provide in the soil and dead grass holes or indentations of a size, shape, and depth that is optimal for receiving and germinating new grass seed and of a density and distribution suitable to provide the resulting grass with a visually desirable pattern, rendering new growth indistinguishable from old growth.
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STATEMENT OF GOVERNMENT INTEREST
The invention described herein may be manufactured and used by or for the Government for governmental purposes without the payment of any royalty thereon.
BACKGROUND OF THE INVENTION
The present invention relates generally to a sensing surface, or focal plane, for an infrared camera. More particularly, the present invention relates to a hybrid focal plane array formed of densely packed, self guarded Schottky infrared internal emission photodiodes.
In U.S. Pat. No. 3,902,066, issued Aug. 26, 1975 to Roosild et al, there is described a monolithic Schottky barrier array for detecting the infrared portion of the electromagnetic spectrum. Individual Schottky electrodes within the array are connected through enhancement mode field effect transistors to charge coupled devices for providing signals to an infrared vidicon camera. The performance of this array has proven to be limited by aliasing and drop-out effects which are related to the low percentage active area of the array. Space is required within the focal plane for multiplexing the signals derived from the individual Schottky electrodes, and also for the guard rings which are provided about each individual Schottky electrode. In such an array, the charge coupled device signal readout circuitry occupies up to 50% of the focal plane area. Add to this the losses of sensing area because of guard rings and channel stops and the active area of the array is reduced to approximately 30 to 45 percent of the total area of the array.
An improvement has been made upon the aforementioned prior art array by Charlotte E. Ludington, a coinventor in the present patent application, and a separate patent application entitled "Hybrid Schottky Infrared Focal Plane Array," bearing Ser. No. 455,715, has been filed thereon. The Ludington patent application discloses a design for an infrared internal emission Schottky array that is compatible with hybrid bump bonding techniques as known in the prior art and shown, for example, in U.S. Pat. No. 3,808,435 issued to Robert T. Bate et al. This structure increases the active area of the array to about 70% of the total area but still leaves blind spots in the array because of the areas occupied by the guard rings which surround the individual Schottky cells.
SUMMARY OF THE INVENTION
In accordance with the present invention, it has been found that an infrared focal plane mosaic having near 100% active area as well as good electrical and sensing properties can be realized by fabrication of a densely packed two-dimensional array of Schottky metal photoemission electrodes on a semiconductor focal plane substrate. The Schottky electrodes are spaced close enough for their depletion regions to overlap. This close spacing reduces the electric field intensity at the edge of the electrodes and eliminates the need for conventional guard rings in the focal plane, thus eliminating a major active area loss factor. Depletion field merger cannot be exploited in conventional infrared detector arrays, which sense radiation in the semiconductor rather than the metal, because such merger would erase the image information. The perimeter of the array can be similiarly guarded with a closely spaced picture frame Schottky electrode. Signal multiplexing and readout is accomplished by the use of a second semiconductor substrate, as known in the prior art for detector arrays which sense infrared radiation in the semiconductor such as HgCdTe. The use of self-guarding simplifies the mosaic architecture and reduces the number of fabrication steps and lithographic masks required; thus, both increased production yield and reduced costs are realized.
Accordingly, the primary object of this invention is to provide an improved Schottky barrier focal plane array.
A further object of this invention is to provide a Schottky barrier focal plane array with an increased active sensing area.
Another object of this invention is to provide simplified array fabrication and reduced array cost through use of self guarding wherein metal electrode Schottky devices are placed close enough to each other to suppress high fields and edge breakdown effects.
Still another object of this invention is to provide mosaic perimeter edge breakdown protection by means of a picture frame Schottky electrode close enough to the photodiode array to provide mutual self-guarding.
These and other advantages, features and objects of this invention will become more apparent from the following description when taken in connection with the illustrative embodiments in the accompanying drawings.
DESCRIPTION OF THE DRAWINGS
FIG. 1 is a pictorial representation of the basic elements of an infrared camera system.
FIG. 2 is a diagrammatic representation of prior art Schottky infrared focal plane array.
FIG. 3 is a diagrammatic representation of a hybrid focal plane array.
FIG. 4 is a diagrammatic representation of a basic Schottky photodiode without a guard ring.
FIG. 5 is a diagrammatic representation of prior art Schottky photodiodes having guard rings.
FIG. 6 is a diagrammatic representation of Schottky photodiodes having the self-guarding feature of the present invention.
FIG. 7 is a diagrammatic representation of a portion of a self-guarded Schottky focal plane array.
DESCRIPTION OF THE PREFERRED EMBODIMENT
Referring now to FIG. 1 of the drawings, there is shown a pictorial representation of the basic elements of a camera for infrared imaging wherein an infrared scene 2 is projected onto a semiconductor focal plane 4 by means of optics 6. Focal plane 4 includes an array of infrared sensitive photodiodes 8 in a two dimensional mosaic pattern. During an exposure or frame time a charge image is built up on the mosaic that is a replica of the observed scene. At the end of the frame, the charge image is read out as a video signal by means well known in the art.
FIG. 2 represents the component layout configuration of a prior art Schottky infrared focal plane array 10 such as that shown in U.S. Pat. No. 3,902,066 mentioned above. This is a monolithic device in which both sensing and multiplexing takes place within the focal plane. The array includes a number of infrared detectors 12, each having a guard ring 14 thereabout to minimize edge breakdown leakage. Channel stops 16 are used to isolate individual photodiodes from each other and from the charge coupled multiplexer network 18 which is used for signal readout. In such prior art devices, the charge coupled devices alone utilize up to 50% of the focal plane area. In addition, the guard rings and channel stops further reduce the useable area of the array to approximately 35 percent.
FIG. 3 represents a hybrid focal plane array assembly 20 in which a simple Schottky focal plane array 22 is bump-bonded to a separate multiplexer chip 24. An array having this structure is described in the Ludington patent application mentioned above. Methods of making suitable bump bonds 26 to the Schottky photodiodes 28 are known in the art.
FIG. 4 represents the schematic of a basic Schottky photodiode 30 including a substrate semiconductor 32, a Schottky metal photoelectrode 34 and an insulator 36. When the photodiode is fabricated, the differences in chemical potential between the metal and the semiconductor causes free charge to be swept from the semiconductor region that is immediately adjacent to the electrode. This process creates both the Schottky potential barrier at the metal-semiconductor interface and a high field depletion region 38 in the semiconductor. Electric field strengths at the edge of the Schottky electrode 40 can be extremely high and it is in this region where most device limiting dark currents and breakdown effects occur.
FIG. 5 illustrates the conventional means for eliminating edge related dark currents. Guard rings 42 are formed by means of impurity diffusion or ion implantation at the edges of the photoelectrodes. Further, to prevent short circuiting between adjacent electrodes, a space or channel stop 44 is provided between guard rings. The depletion region is now confined to the area 46. As illustrated in FIG. 5, for a detector active area having dimension d, a guard ring width g, and a channel stop width c, the mosaic percent active area will be:
100×d.sup.2 /(d+2g+c).sup.2
It can therefore be seen that the use of guard rings greatly restricts the focal plane percent active area, particularly where the center to center distances of detectors is small.
In FIG. 6, the self guarding technique of the present invention is illustrated. Here the individual Schottky electrodes 48 are placed so close that their individual depletion regions 50 merge. The combined depletion field 52 becomes continuous and edges of individual depletion regions no longer come to the surface between adjacent electrodes 48. The electric field at the inner electrode edges 54 is thereby reduced. As a result, leakage currents at electrode edges are eliminated and mosaics can be operated at useful voltages (10 to 30 volts) without exhibiting breakdown. There is no loss of image when the depletion regions merge because, in the case of Schottky internal emission sensors, the signal is entirely on the metal electrodes 48. Electrodes spacing of less than 5 micrometers has been found effective for such self-guarding. By eliminating guard rings, the percent active area becomes:
100×d.sup.2 /(d+c).sup.2
It can be seen that this self-guarding technique is substantially more area efficient than the conventional guard ring technique shown in FIG. 5. A second advantage of self guarding is the simplification of focal plane fabrication. The conventional guard ring architecture requires both additional photolithographic masks and additional processing steps. Also, greater processing precision is required in the prior art designs in order to align the Schottky electrode edges with the center of the guard ring. No alignment is required in the present invention illustrated in FIG. 6.
The preferred embodiment of a portion of a self guarded Schottky hybrid focal plane array is shown in FIG. 7. Here, the outer Schottky electrodes are surrounded by a picture frame perimeter Schottky electrode 58 which is separated from the array by 1 to 5 micrometers. Self-guarding will now occur at the array perimeter 60. It should be noted that leakage is possible at the outer edge 62 of the perimeter Schottky electrode. This leakage can be diverted to the substrate and will not impact imaging performance. Alternately, such leakage can be eliminated by use of a conventional guard ring along the outer edge 62 of the Schottky perimeter electrode 58 without degrading focal plane area coverage. Schottky photoelectrodes 64 are separated by very narrow gaps 66 on the order of 1 to 5 micrometers. The Schottky electrode array and the perimeter electrode 58 each provide mutual self-guarding action by overlap of their depletion fields. Both the array and picture frame electrode can be fabricated with one metal evaporation. To complete focal plane fabrication, oxide feedthroughs 68 connect to bump landing pads 70 and substrate ohmic contacts are added by means well known in the semiconductor art. A second semiconductor substrate containing multiplexing circuitry is then bonded to each of the bump landing pads 70. The semiconductor base material of the present invention is preferably silicon while the Schottky electrodes are preferably formed of platinum silicide or other metallic silicides.
Although the invention has been described with reference to a particular embodiment, it will be understood to those skilled in the art that the invention is capable of a variety of alternative embodiments within the spirit and scope of the appended claims.
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A two dimensional focal plane array of Schottky photodiodes on a silicon substrate for infrared imaging. The array is designed for mating with multiplexing circuitry and has a self-guarding feature wherein adjacent Schottky electrodes act as guard electrodes. This feature allows a substantial increase of the focal plane area coverage ratio.
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BACKGROUND OF THE INVENTION
This invention relates to a polish formulation including a zwitterionic aminofunctional siloxane which imparts to the surface containing the polish a film forming capacity which functions to sheet water coming into contact with the surface rather than to bead the water as has been the case with prior formulations.
Polishes are used to produce a glossy finish on a surface as well as to prolong the useful life of the surface. The gloss provided by the polish is the result of components in the polish which leave a coating and that function to smooth and clean the surface. Floor polish, furniture polish, and shoe polish, rely upon a deposited film. Car and boat polish formulations result in a glossy and protective film and contain abrasives for removing weathered paint and soil as well as old built-up polish. Metal polish contains ingredients for abrasive smoothing of the surface being treated and for surface cleaning, as well as components that function to remove and retard the build-up of tarnish.
Motor vehicle polish is formulated in order to remove road film and oxidized paint, and to provide a continuous glossy film which resists water and its removal by water and car wash detergents. Such vehicle polishes contain several major functional ingredients including an abrasive. The abrasive, however, must be mild enough to avoid scratching of the painted surface, and representative of such mild acting material are, for example, fine grades of aluminum silicate, diatomaceous earth, and various silicas. Straight and branched chain aliphatic hydrocarbons are employed to facilitate the detergency of the polish against oil based traffic soils and debris, and provide the solvency characteristics necessary in the production of a stable formulation. These hydrocarbons also control the drying rate of the formulation. Wax constitutes another polish ingredient and is one of the two film forming materials in the polish. The wax is spread and leveled and produces a high luster following buffing of the surface. Blends of soft and hard wax are often employed in order to facilitate ease of buffing and the durability of the polish against environmental antagonists. Exemplary waxes are paraffin wax, microcrystalline petroleum wax, carnauba wax, candelilla vegetable wax, montan coal derived wax, and synthetic polymeric waxes such as oxidized polyethylene.
Silicone materials are included in polishes as the other film forming ingredient. Such silicone materials also function as lubricants for easing the application of the polish as well as its buffing, and act as release agents for dried abrasive. The silicone materials spread easily and provide a uniform high gloss and with it water repellency. Such materials typically are dimethylsilicones, however, aminofunctional silicone products are becoming more prevalent. The aminofunctional products result in films having increased resistance to removal from the surface by detergents and the environment believed to be the result of their ability to plate out on a painted surface and to crosslink and bond to that surface.
A car polish may also contain an emulsifier, a thickener, and a stabilizer, for the production of a homogeneous stable product of desired consistency. Such polishes may be solid in form, semisolid, presoftened, or liquid. The polish, for example, can be solvent based or an emulsion, and in either case is a liquid, semi-solid, or solid in constitution. Typically, liquid emulsions include ten to fifteen weight percent of an abrasive, ten to thirty weight percent of solvent, two to fifteen weight percent of a silicone material, and up to about four weight percent wax. In an emulsion paste formulation, the wax ingredient is increased in level from three to twenty-five weight percent.
In U.S. Pat. No. 3,956,353, issued May 11, 1976, there is disclosed the reaction product of an aminofunctional silane and a cyclic acid anhydride. These products are limited, however, to vinyl benzyl functional amines whereas the materials of the present invention differ in the amine group, and do not require such a substitution. Such products further are not disclosed to be useable in a polish formulation as such, but are aqueous or alcohol coupling agent compositions, in contrast to the polish compositions disclosed in the present invention. Polishes, it should be noted, require polymers with significant dimethyl character for solubility, as are the aminofunctional siloxane zwitterions of the present invention. The reaction products in U.S. Pat. No. 3,956,353, however, are low molecular weight monomer materials. Polish formulations containing silicone materials are disclosed in U.S. Pat. No. 3,508,933, issued Apr. 28, 1970, in U.S. Pat. No. 3,836,371, issued Sept. 17, 1974, and in U.S. Pat. No. 3,890,271, issued Jun. 17, 1975. While these silicone materials are characterized as being aminofunctional siloxanes, they are not zwitterionomers as are the compositions of the present invention, and it is not believed to be known to employ zwitterionomers in polish formulations. What appears to be a zwitterion in a polish in Japanese Publication No. 8029/80 is actually an amido acid. Such acids are low molecular weight hard solids in contrast to the high molecular weight fluids of the present invention. Further, the function of such amido acids is to increase the luster or shine of a polish, rather than to cause water to sheet as in the present invention. Zwitterionomers are not new as exemplified by U.S. Pat. No. 4,525,567, issued Jun. 25, 1985, to Campbell et al, however, the zwitterionomers of Campbell et al are characterized as being sultone based zwitterionomers whereas the zwitterionomers of the present invention are sulfur free amine cyclic-anhydride based zwitterionomers in contrast thereto. Further, the zwitterionomers of the present invention are lactone free in contrast to Campbell et al. A further distinction exists between the instant invention and that of Campbell et al, in that in Campbell et al, there is disclosed a low cost process of making the zwitterions by combining OH endblocked polydimethylsiloxane, a functional silane, and an acid catalyst. In the present invention, however, the zwitterionomers can be prepared from fully-premade aminofunctional siloxane polymers which are not silicon functional. As such, the compositions of the present invention provide new and unique advantages over typical prior art polish formulations which will become apparent hereinafter.
SUMMARY OF THE INVENTION
This invention relates to a polish formulation containing as components thereof at least one member selected from the group consisting of waxes, solvents, surfactants, thickening agents, abrasives, dyes, odorants, and other ingredients normally used in making polishes. The improvement includes incorporating therein a composition which is the reaction product of a cyclic acid anhydride and an aminofunctional siloxane selected from the group consisting of (A) a blend or reaction product of a hydroxyl endblocked polydimethylsiloxane having a viscosity in the range of about 10 to 15,000 cs at twenty-five degrees centigrade, and a silane selected from the group consisting of those having the general formulae R" n (R'O) 3-n Si(CH 2 ) 3 NHR'" and R" n (R'O) 3-n SiRNHCH 2 CH 2 NH 2 wherein R'" is a hydrogen atom or a methyl radical, R" is a monovalent hydrocarbon radical free of aliphatic unsaturation and contains from one to six carbon atoms, n has a value of from zero to two, R' is an alkyl radical containing from one to four carbon atoms, and R is a divalent hydrocarbon radical free of aliphatic unsaturation and contains three to four carbon atoms, (B) a blend or reaction product of a hydroxyl endblocked polydimethylsiloxane having a viscosity in the range of about 10 to 15,000 cs at twenty-five degrees centigrade, a silane selected from the group consisting of those having the general formulae (R 1 O) 3 --SiR 2 NHR 3 and (R 1 O) 3 --SiR 2 NHCH 2 CH 2 NH 2 wherein R 1 is an alkyl radical containing from one to four carbon atoms, R 2 is a divalent hydrocarbon radical free of aliphatic unsaturation and contains from three to four carbon atoms, and R 3 is selected from the group consisting of the hydrogen atom and the methyl radical, and a silane having the general formula X 3 SiZ wherein X is selected from the group consisting of alkoxy and acyloxy radicals containing from one to four carbon atoms, and Z is a nonhydrolyzable radical selected from the group consisting of hydrocarbon radicals, halogenated hydrocarbon radicals, and radicals composed of carbon, hydrogen, and oxygen atoms, wherein the oxygen atoms are present in hydroxyl groups, ester groups, or ether linkages, there being from one to ten carbon atoms in the Z radical, and (C) a blend or reaction product of a polydimethylsiloxane having a viscosity in the range of about one to 15,000 cs at twenty-five degrees centigrade, and a silane selected from the group consisting of those having the general formulae R" n (R'O) 3-n Si(CH 2 ) 3 NHR'" and R" n (R'O) 3-n SiRNHCH 2 CH 2 NH 2 wherein R'" is a hydrogen atom or a methyl radical, R" is a monovalent hydrocarbon radical free of aliphatic unsaturation and contains from one to six carbon atoms, n has a value of from zero to two, R' is an alkyl radical containing from one to four carbon atoms, and R is a divalent hydrocarbon radical free of aliphatic unsaturation and contains three to four carbon atoms. (C) above is a specific species and a trimethylsilyl endblocked aminofunctional siloxane produced by incorporating conventional trimethylsilyl functional silanes or siloxanes into the aminofunctional siloxanes.
In a specific embodiment of the present invention, the acid anhydride is selected from the group consisting of succinic anhydride, maleic anhydride, phthalic anhydride, and carbon dioxide. The reaction product is an aminofunctional siloxane zwitterion having the structural formula: R2 ? ? ##STR1## where Me is methyl, x is an integer of from about forty to about four hundred, y is an integer of from about one to about twenty, and R 4 is ethylene, vinylidene, or phenylene. x is preferably 188 and y is ten.
The zwitterionic aminofunctional siloxane can, if desired, be further reacted with a strong acid resulting in an equilibrium of the zwitterion and a conjugate acid base pair of the zwitterion and the acid; for which the extent of conjugate acid base pair formation depends upon the pKa of the strong acid and the dielectric strength of the solvent. In such case, the strong acid is selected from the group consisting of hydrochloric, hydrobromic, hydriodic, nitric, perchloric, phosphoric, and organic acids. The organic acid is selected from the group consisting of acetic, propionic, butyric, valeric, caproic, benzoic, halo-substituted benzoic, and nitro-substituted benzoic. The conjugate acid base pair of the zwitterion and the strong acid has the structural formula: ##STR2## where Me is methyl, x is an integer of from about forty to about four hundred, y is an integer of from about one to about twenty, A is an anion and the conjugate base of the strong acid, and R 4 is ethylene, vinylidene, or phenylene. x again is preferably 188 and y is ten.
The invention is further directed to a method of sheeting water on a surface in which there is applied to the surface before the surface is exposed to water a polish formulation containing as components thereof the ingredients enumerated above.
The invention is also directed to a method of making an aminofunctional siloxane zwitterionomer comprising reacting an acid anhydride with an aminofunctional siloxane selected from the group consisting of (A) and (B) as set forth and detailed above.
Still further, the present invention relates to an aminofunctional zwitterionomeric siloxane compound which is a reaction product of an acid anhydride with an aminofunctional siloxane selected from the group consisting of (A) and (B) again as defined hereinabove.
It is therefore an object of the present invention to provide a new and novel type of polish formulation particularly adapted for use on motor vehicles in which water coming into contact with such surfaces is sheeted and drained away rather than being beaded and repelled as has been the practice of prior art formulations in the past. A particular advantage to this approach is that vehicles need not be washed following every period of rain as has been the case due to spots caused by the beads. Instead, with the sheeting action of the compositions of the present invention, this disadvantage is overcome, and rain is sheeted away from vehicle surfaces without leaving behind the unaesthetic appearance of rings containing debris.
These and other features, objects, and advantages, of the herein described instant invention, should become more apparent when taken in conjunction with the following detailed description thereof.
DETAILED DESCRIPTION OF THE INVENTION
A surfactant is a compound that reduces surface tension when dissolved in a liquid. Surfactants exhibit combinations of cleaning, detergency, foaming, wetting, emulsifying, solubilizing, and dispersing properties. They are classified depending upon the charge of the surface active moiety. In anionic surfactants, the moiety carries a negative charge as in soap. In cationic surfactants, the charge is positive. In non-ionic surfactants, there is no charge on the molecule, and in amphoteric surfactants, solubilization is provided by the presence of positive and negative charges linked together in the molecule. A zwitterion is a special category and is a molecule that exists as a dipolar ion rather than in the un-ionized form. The molecule is neutral overall but has a large charge separation like an amino acid. Zwitterions are also known as hybrid ions, and internal or intramolecular salts. In the case of amino acids, they are electrolytes having separated weakly acidic and weakly basic groups. For example, while shown as H 2 N--R--COOH, in aqueous solution ⊕H 3 N--R--COO - is the actual species where an internal proton transfer from the acidic carboxyl to the basic amino site is complete. The uncharged species has separate cationic and anionic sites but the positive and the negative ions are not free to migrate. Thus, it is a complex ion that is both positively and negatively charged. Alkyl betaines are also representative of zwitterions and are a special class of zwitterion where there is no hydrogen atom bonded to the cationic site. Some silicones are also zwitterions and it is this special category of silicone zwitterion to which the present invention relates.
The zwitterionomeric aminofunctional siloxane compositions of the present invention may be prepared in accordance with the following schematic: s ##STR3##
It should be noted in the above schematic that formula (I) denotes an aminofunctional siloxane, formula (II) denotes the zwitterionomer of the present invention, and formula (III) indicates the conjugate acid base pair of the zwitterionomer and the strong acid (HA). Formula (I) is generically described as an aminofunctional siloxane selected from the group consisting of reaction products of (A) a blend or reaction product of a hydroxyl endblocked polydimethylsiloxane having a viscosity in the range of about 10 to 15,000 cs at twenty-five degrees centigrade, and a silane selected from the group consisting of those having the general formulae R" n (R'O) 3-n Si(CH 2 ) 3 NHR'" and R" n (R'O) 3-n SiRNHCH 2 CH 2 NH 2 wherein R'" is a hydrogen atom or a methyl radical, R" is a monovalent hydrocarbon radical free of aliphatic unsaturation and contains from one to six carbon atoms, n has a value of from zero to two, R' is an alkyl radical containing from one to four carbon atoms, and R is a divalent hydrocarbon radical free of aliphatic unsaturation and contains three to four carbon atoms, (B) a blend or reaction product of a hydroxyl endblocked polydimethylsiloxane having a viscosity in the range of about 10 to 15,000 cs at twenty-five degrees centigrade, a silane selected from the group consisting of those having the general formulae (R 1 O) 3 --SiR 2 NHR 3 and (R 1 O) 3 --SiR 2 NHCH 2 CH 2 NH 2 wherein R 1 is an alkyl radical containing from one to four carbon atoms, R 2 is a divalent hydrocarbon radical free of aliphatic unsaturation and contains from three to four carbon atoms, and R 3 is selected from the group consisting of the hydrogen atom and the methyl radical, and a silane having the general formula X 3 SiZ wherein X is selected from the group consisting of alkoxy and acyloxy radicals containing from one to four carbon atoms, and Z is a nonhydrolyzable radical selected from the group consisting of hydrocarbon radicals, halogenated hydrocarbon radicals, and radicals composed of carbon, hydrogen, and oxygen atoms, wherein the oxygen atoms are present in hydroxyl groups, ester groups, or ether linkages, there being from one to ten carbon atoms in the Z radical, and (C) a blend or reaction product of a polydimethylsiloxane having a viscosity in the range of about one to 15,000 cs at twenty-five degrees centigrade, and a silane selected from the group consisting of those having the general formulae R" n (R'O) 3-n Si(CH 2 ) 3 NHR'" and R" n (R'O) 3-n SiRNHCH 2 CH 2 NH 2 wherein R'" is a hydrogen atom or a methyl radical, R" is a monovalent hydrocarbon radical free of aliphatic unsaturation and contains from one to six carbon atoms, n has a value of from zero to two, R' is an alkyl radical containing from one to four carbon atoms, and R is a divalent hydrocarbon radical free of aliphatic unsaturation and contains three to four carbon atoms. Such compositions are described in more or less detail in U.S. Pat. No. 3,508,933, issued Apr. 28, 1970, in U.S. Pat. No. 3,836,371, issued Sept. 17, 1974, and in U.S. Pat. No. 3,890,271, issued Jun. 17, 1975. The preparation of these compositions and their use in polishes is also detailed in the aforementioned patents, the disclosures of which are incorporated herein by reference thereto. Particular of such compositions prepared and falling within the scope of the present invention is set forth in Table I.
TABLE I______________________________________Compound (I) x y______________________________________A 45.75 2.25B 69.25 3.75C 96 2D 188 10E 295.9 2.1F 400 8______________________________________
In the above schematic, the acid anhydride which is reacted with compositions of formula (I) is selected from the group consisting of succinic anhydride, maleic anhydride, phthalic anhydride, itaconic anhydride, or other cyclic anhydrides, and carbon dioxide, with the first named anhydride being the preferred material for use herein.
The resulting reaction product indicated by formula (II) in the foregoing schematic is an aminofunctional siloxane zwitterionomer having the structural formula: ##STR4## where Me is methyl, x is an integer of from about forty to about four hundred, y is an integer of from about one to about twenty, and R 4 is ethylene, vinylidene, or phenylene. x is preferably 188 and y is ten. The zwitterionic aminofunctional siloxane of formula (II) is further reacted with a strong acid (HA) resulting in an equilibrium of the zwitterion (II) and a conjugate acid base pair indicated by formula (III) of the zwitterion (II) and the acid (HA) which depends upon the pKa of the strong acid and the dielectric strength of the polish solvent. The strong acid (HA) is selected from the group consisting of hydrochloric, hydrobromic, hydriodic, nitric, perchloric, phosphoric, and organic acids, wherein the organic acid may be one of the group consisting of acetic, propionic, butyric, valeric, caproic, benzoic, halo-substituted benzoic, and nitro-substituted benzoic. The resulting formula (III) as shown above of the conjugate acid base pair of the zwitterion (II) and the strong acid (HA) has the structural formula: ##STR5## where again Me is methyl, x is an integer of from about forty to about four hundred, y is an integer of from about one to about twenty, A is an anion, and R 4 is ethylene, vinylidene, or phenylene. x is preferably 188 and y is ten. This is a specific embodiment of the present invention, and is not a requirement that the conjugate composition (III) be formed in every instance. However, it should be noted that where the conjugate (III) is formed, it necessitates the presence in the formulation of an acid. The equilibrium reached between the zwitterionomer (II) and the conjugate (III) depends on the strength of the acid. Where the acid is strong, the conjugate (III) predominates. Where the acid is weaker, the zwitterionomer predominates. As noted hereinbefore, such equilibrium depends upon the pKa of the strong acid and the dielectric strength of the solvent. Preferred solvents in accordance with the present invention are ethanol and toluene, for example.
The zwitterionic aminofunctional siloxane of formula (II) can also be further reacted with a basic compound resulting in an equilibrium of the zwitterion (II) and a conjugate acid base pair indicated by formula (IV) of the zwitterion (II) and the basic compound which depends upon the relative pKa's of the base B and the basic sites of the zwitterion, and the dielectric strength of the medium. The strong base is selected from the group consisting of organic amines, hydroxides, and lewis bases. The resulting formula (IV) as shown below of the conjugate acid base pair of the zwitterion (II) and the basic compound has the structural formula: ##STR6## where again Me is methyl, x is an integer of from about forty to about four hundred, y is an integer of from about one to about twenty, BH is a cation and a protonated base, and R 4 is ethylene, vinylidene, or phenylene. x is preferably 188 and y is ten. This is a specific embodiment of the present invention, and is not a requirement that the conjugate composition (IV) be formed in every instance. However, it should be noted that where the conjugate (IV) is formed, it necessitates the presence in the formulation of a basic compound such as dibutyl amine. The equilibrium reached between the zwitterionomer (II) and the conjugate (IV) depends on the strength of the base. Where the base is strong, the conjugate (IV) predominates. Where the base is weaker, the zwitterionomer predominates. As noted hereinbefore, such equilibrium depends upon the relative pKa's of the strong base and zwitterion, and the dielectric strength of the solvent.
The aminofunctional siloxanes of the formula (I) type may also be prepared by an alternate method from that set forth in U.S. Pat. No. 3,508,993, U.S. Pat. No. 3,836,371, and U.S. Pat. No. 3,890,271, aforementioned. In the alternate method, the starting material is methyldimethoxy ethylenediaminoisobutyl silane of the formula:
CH.sub.3 (CH.sub.3 O).sub.2 SiCH.sub.2 CH(CH.sub.3)CH.sub.2 NHCH.sub.2 CH.sub.2 NH.sub.2
This aminofunctional silane is distilled to an active concentration of between about 95-99%. The silane is hydrolyzed with three moles of water added to one mole of the silane. The material is batch distilled at atmospheric pressure and at a temperature of about one hundred and thirty degrees centigrade. Methanol and residual water are then removed by vacuum stripping to yield an aminofunctional hydrolyzate. The aminofunctional hydrolyzate is added to a mixture of polydimethylsiloxane of viscosity of 1.5 centistokes, a dimethylcyclic of the formula (Me 2 SiO) n where n is three, four, or five, and a catalyst such as potassium hydroxide or potassium silanolate. This mixture is equilibriated to a polymer by agitation and heat at about one hundred-fifty degrees centigrade. The mixture is cooled to about 80-90 degrees centigrade or lower and the catalyst is neutralized by the addition of acetic acid accompanied with mixing. The non-volatile content is increased by stripping of the volatiles under vacuum, followed by filtration of the material in a pre-coated plate and frame filter for the purpose of removing any haze in order to obtain a clarified product. A typical example of this procedure is set forth below.
EXAMPLE I
Into a round bottom flask was added 3,482.8 grams of a dimethylcyclic, 439.2 grams of hydrolyzate, 78.4 grams of polydimethylsiloxane of viscosity of 1.5 cs, and 38.3 grams of potassium silanolate catalyst. The contents of the flask were mixed under a nitrogen atmosphere for twenty minutes. Heat was applied to the flask and the contents were maintained at one hundred-fifty degrees centigrade for four hours. The mixture was cooled to thirty-three degrees centigrade. The catalyst was neutralized by the addition to the flask of 2.14 grams of acetic acid. The fluid was stirred overnight and filtered. The resulting product was water clear and had a viscosity of 354 cs. The product contained five mol percent amine and was identified as the material set forth in Table I where x=188 and y=10.
EXAMPLE II
Example I was repeated in order to produce an aminofunctional siloxane of the formula (I) type. Zwitterionic aminofunctional siloxanes materials of the formula (II) type were obtained by separately dissolving succinic anhydride in dimethoxyethane in order to provide a ten weight percent solution of the anhydride. The succinic anhydride was added from a dropping funnel to the contents of the flask containing the formula (I) type aminofunctional siloxane, and the solution was heated with stirring at about fifty-five degrees centigrade and under a nitrogen flow. The mixture was vacuum distilled at about twenty millimeters of mercury or less under a nitrogen atmosphere at one hundred-twenty degrees centigrade for about forty-five minutes or until the vapor reached about eighty degrees centigrade, to remove all of the dimethoxyethane and yielding the zwitterionomer. The resulting zwitterionomer was distilled to a solids content of about eighty-eight percent. This example was repeated producing zwitterionomers having amine mol percentages ranging from about 0.5 mol percent to about eight mol percent.
The zwitterionic aminofunctional siloxanes of the present invention, were formulated into polishes in place of the aminofunctional siloxanes employed in U.S. Pat. No. 3,508,933, U.S. Pat. No. 3,836,371, and U.S. Pat. No. 3,890,271, causing water coming into contact with the surface treated, to sheet rather than to bead, as is conventional with prior art polish formulations. The polishes so formulated were applied both to actual vehicle surfaces as well as test panels. Water contacting the treated surfaces sheeted water and was noted by visual observation. Thus, prior art polishes lay down a film, but the film is a water beading film, in contrast to the water sheeting film obtained when the zwitterionomeric compositions of the present invention are employed. In either case, a film is formed by applying the polish to the surface to be treated and by rubbing in the polish onto the surface and allowing the solvent to evaporate, leaving behind the film. Inclusion of the zwitterionomers of the present invention, however, sheets the water, whereas omission beads the water. A distinct advantage of a water sheeting film is that, in contrast to a film that beads the water, the water sheeting film will not collect dust and debris following a rain as do water beading films, which necessitate that the surface be washed once more in order to remove the spots and rings caused by the water beading type of film. The water sheeting films of the present invention are of general application including such surfaces as motor vehicles, boats and navigable crafts, wood surfaces, plastic surfaces, and fiber surfaces. The films produce a high gloss, are durable, and are easy to apply.
It will be apparent from the foregoing that many other variations and modifications may be made in the structures, compounds, compositions, and methods described herein without departing substantially from the essential features and concepts of the present invention. Accordingly, it should be clearly understood that the forms of the invention described herein are exemplary only and are not intended as limitations on the scope of the present invention.
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A polish formulation containing as components at least one member selected from the group consisting of waxes, solvents, surfactants, thickening agents, abrasives, dyes, odorants, and other ingredients normally used in making polishes, and as an improvement incorporating a composition which is the reaction product of an acid anhydride and an aminofunctional siloxane. The resulting zwitterionic aminofunctional siloxane can, if desired, be further reacted with a strong acid to provide an equilibrium of the zwitterion and a conjugate acid base pair of the zwitterion and the acid. The invention also includes a method of sheeting water on a surface with the polish, a method of making an aminofunctional siloxane zwitterionomer, and an aminofunctional zwitterionomeric siloxane compound which is the reaction product.
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BACKGROUND OF THE INVENTION
The present invention relates to a connection structure between a shield electric wire and a shield terminal and a connection method therebetween.
A shield connector that is disclosed in Japanese Patent Application Laid-Open No. 8-78071 has a shield electric wire, a terminal electrically connected to a core wire of the shield electric wire, a shield terminal electrically connected to a braided wire of the shield electric wire, a housing for accommodating these elements therein, and a cap mounted on a forward end of the shield terminal.
The shield terminal and the braided wire are connected to each other by the use of the following method. The method is first to peel an insulating outer covering at one end of the shield electric wire to thereby cause the braided wire to be exposed, to fold the exposed braided wire back onto the insulating outer covering to thereby superpose this braided wire upon the insulating outer covering, and then to peel an insulating inner covering to thereby cause the core wire to be exposed. Next, the method is to pass the insulating inner covering through a terminal-retaining portion of the terminal and to caulk the terminal-retaining portion to thereby electrically connect the core wire and the terminal. Finally, the method is to insert the shield electric wire into the housing to thereby connect the shield terminal and the braided wire to each other.
The connection between the shield terminal and the braided wire is achieved through the press contacting of the braided wire with respect to a plurality of blade spring pieces disposed within the shield terminal.
SUMMARY OF THE INVENTION
However, in the above-described conventional structure, it is necessary to perform the peeling of the insulating outer covering over a wide range to thereby expose the braided wire. Therefore, the operation of eliminating the insulating outer covering is troublesome. In addition, for the purpose of preventing the braided wire and the core wire from being short-circuited, the braided wire must be cut to a prescribed length. Because the blade spring pieces are needed to be disposed within the shield terminal, the structure of the shield terminal becomes complex. When causing an increase in the blade loading of the blade spring piece in order to make the contact between this spring piece and the braided wire reliable, there is the likelihood that the braided wire will become hard to insert between the blade spring pieces. Simultaneously, there is also the likelihood that the braided wire will be dragged up and so a defective contact will occur between the braided wire and the blade spring piece. In addition, the terminal end of the braided wire becomes likely to get frayed and so the connection thereof to the shield terminal becomes more and more difficult.
Thereupon, it is an object of the present invention to provide a highly reliable connection structure that makes it possible to reliably and easily perform an electric connection between the shield terminal and the braided wire.
To achieve the above object, in the structure according to the present invention, the shield electric wire has braided wires, an outer insulating portion for covering the braided wires, and a connecting portion formed using part of the braided wires. The connecting portion is formed by drawing up the braided wires extended and exposed from the end of the outer insulating portion and collecting them together to the end thereof, and has a rib-like configuration. The shield terminal is connected to the connecting portion.
According to this construction, the rib-like connecting portion that has been formed by the braided wires being drawn near and collected together is connected to the shield terminal. Therefore, between the shield terminal and the connecting portion, there is attained a state of surface contact where the contact area between the both has been sufficiently ensured. As a result, the braided wires and the shield terminal are directly connected together. Accordingly, a stable electrical connection is obtained with a simple structure and in addition the braided wires are prevented from getting frayed.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is an exploded perspective view illustrating a connection structure of a shield electric wire according to an embodiment of the present invention;
FIG. 2 is an enlarged perspective view illustrating a main part of a terminal processed portion of the electric wire according to the embodiment;
FIG. 3A is a front view illustrating a shield terminal in the connection structure of the shield electric wire according to the embodiment;
FIG. 3B is a sectional view taken along a line III—III of FIG. 3A;
FIG. 4 is an enlarged sectional view illustrating the connection structure of the shield electric wire according to the embodiment;
FIG. 5A is an enlarged view illustrating a main part of a step of mounting a terminal metal fitting in a shield-terminal connection method performed with respect to the shield electric wire according to the embodiment;
FIG. 5B is an enlarged view illustrating a main part of a step of performing outer-covering peeling of an insulating outer covering in the shield-terminal connection method performed with respect to the shield electric wire according to the embodiment;
FIG. 5C is an enlarged view illustrating a main part of a step of forming a rib-like connecting portion in the shield-terminal connection method performed with respect to the shield electric wire according to the embodiment;
FIG. 5D is an enlarged view illustrating a main part of a state of a separated outer covering being pressed against the rib-like connecting portion in the shield-terminal connection method performed with respect to the shield electric wire according to the embodiment;
FIG. 6 is an enlarged sectional view illustrating a connecting portion of the shield terminal and the rib-like connecting portion that have been connected by resistance welding; and
FIG. 7 is an enlarged sectional view illustrating the connection structure of the shield electric wire, the rib-like connecting portion of that has been formed using only braided wires alone with the peeled-off insulating outer covering thereof being taken away therefrom.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
A concrete embodiment, to which the present invention has been applied, will now be explained in detail with reference to the drawings.
First, a connection structure of a shield electric wire according to this embodiment will be explained.
As illustrated in FIGS. 1 to 4 , in the connection structure of a shield electric wire 1 , a shield terminal 4 is electrically connected to braided wires 3 that have been exposed by part of an insulating outer covering (outer insulating portion) 2 being peeled away. Being drawn up and collected to an end surface of the insulating outer covering 2 , the exposed braided wires 3 constitute a rib-like connecting portion 5 . The rib-like connecting portion 5 is connected to the shield terminal 4 .
As illustrated in FIGS. 1 and 2, the shield electric wire 1 has core wires 6 each consisting of a conductor, and an insulating inner covering (inner insulating portion) 7 that covers the core wires. The shield electric wire 1 also has braided wires 3 that have been disposed on an outer surface of the insulating inner covering 7 so as to cover this insulating inner covering 7 . Further, the shield electric wire 1 also has an insulating outer covering 2 that covers on an outer-peripheral surface of the braided wires 3 the core wires 6 , the insulating inner covering 7 , and the braided wires 3 and that is formed of insulating resin.
As illustrated in FIG. 2, on one end portion of the shield electric wire 1 there is provided the rib-like connecting portion 5 made up of the braided wires 3 . The rib-like connecting portion 5 is formed by drawing up an outer covering 2 a partly separated from the insulating outer covering 2 to the end surface of the insulating outer covering 2 together with the exposed braided wires 3 . The rib-like connecting portion 5 protrudes from the outer surface of the insulating outer covering 2 and so the area of contact thereof with the shield terminal 4 is sufficiently ensured. The amount of protrusion of the rib-like connecting portion 5 is adjusted by the distance (the length of the exposed braided wires 3 ) between the separated outer covering 2 a and the insulating outer covering 2 .
At one end portion of the shield electric wire 1 , as illustrated in FIGS. 1 and 2, there are exposed the core wires 6 by part of the insulating inner covering 7 being peeled away. As illustrated in FIG. 4, on the core wires 6 there is mounted a terminal metal fitting (terminal) 8 . The terminal metal fitting 8 , as illustrated in FIG. 1, is composed of a caulking connecting portion 9 that caulks the portions in the vicinity of forward ends of the core wires 6 and that is thereby electrically connected to these core wires 6 , and a contacting portion 10 connected to a mating terminal not illustrated.
As illustrated in FIG. 3, the shield terminal 4 has an outer hollow-cylinder 11 , an inner hollow-cylinder 13 situated within the outer hollow-cylinder 11 , and a connection portion 12 between the outer hollow-cylinder 11 and the inner hollow-cylinder 13 . The shield terminal 4 is thereby integrally formed as a whole. The inner hollow-cylinder 13 is disposed in the vicinity of an opening 4 a from which the shield electric wire 1 is inserted and has at least a size permitting the insertion therethrough of the shield electric wire 1 .
The connection portion 12 has a configuration that is like a circular annulus. The outer hollow-cylinder 11 has a diameter larger than the inner hollow-cylinder 13 in order to accommodate therein a terminal processed portion of the shield electric wire 1 equipped with the terminal metal fitting 8 .
As illustrated in FIG. 4, the shield electric wire 1 having the terminal metal fitting 8 mounted at the forward ends of the core wires 6 is inserted into the shield terminal 4 . The rib-like connecting portion 5 gets contacted with the connection portion 12 in the fashion of a surface contact and this connecting portion 5 is electrically connected thereto by the use of various joining means. As the joining means there are adopted various kinds of joining means such as resistance welding, ultrasonic welding, adhesion, etc. The forward end of the terminal metal fitting 8 is accommodated within the shield terminal 4 without being caused to externally protrude from the shield terminal 4 .
Next, the shield-terminal connection method with respect to the shield electric wire according to this embodiment will be explained.
First, as illustrated in FIG. 5A, the method is to peel the coverings of the terminal portion of the shield electric wire 1 to thereby expose the core wires 6 , insulating inner covering 7 , and braided wires 3 . Then it is also to caulk the portion in the vicinity of the forward ends of the core wires 6 by the terminal metal fitting 8 and connect this terminal metal fitting 8 to that portion.
Next, as illustrated in FIG. 5B, the method is to cut part of the insulating outer covering 2 by means of a cutter, etc. and separate it from the remaining portion thereof. Then it is to drag this cut part toward the terminal metal fitting 8 to thereby expose the braided wires 3 externally. The separated outer covering 2 a is not completely drawn away from the braided wires 3 and so the ends of the braided wires 3 remain within the separated outer covering 2 a.
Next, as illustrated in FIG. 5C, the method is to draw up the separated outer covering 2 a toward the end of the insulating outer covering 2 by a damper 15 , etc. As a result of this, the exposed braided wires 3 is externally loosened by degrees in correspondence with the movement of the separated outer covering 2 a . Eventually, the braided wires 3 are clamped between the separated outer covering 2 a and the insulating outer covering 2 to thereby form the rib-like connecting portion 5 having the shape of a circular disk. At this time, as shown in FIG. 5D, the terminal end portions 3 a of the braided wires 3 are drawn into the interior of the separated outer covering 2 a.
Next, as illustrated in FIG. 4, the shield terminal 4 is inserted over the terminal processed portion of the shield electric wire 1 , and this terminal 4 is forced in until the connection portion 12 contacts with the rib-like connecting portion 5 .
Next, one electrode 16 is inserted into a space formed between the outer hollow-cylinder 11 of the shield terminal 4 and the inner hollow-cylinder 13 while another electrode 17 is inserted into a space formed between the outer hollow-cylinder 11 and the shield electric wire 1 .
Finally, forward ends of the electrodes 16 and 17 are pressed against the connection portion 12 and the rib-like connecting portion 5 , respectively. In this condition, a prescribed voltage is applied from a power source portion 18 to between the electrodes 16 and 17 . As a result, the rib-like connecting portion 5 and the connection portion 12 are resistance-welded due to the heat generated by application of the voltage and are metal-joined together. As a result of this, the electrical-connection performance between the rib-like connecting portion 5 and the connection portion 12 is remarkably graded up.
In the above-constructed connection structure of the shield electric wire according to this embodiment, the shield terminal 4 is connected to the rib-like connecting portion 5 prepared by drawing up the exposed braided wires 3 to the end surface of the insulating outer covering 2 and collecting them together. Since the rib-like connecting portion 5 and the shield terminal 4 are joined to each other in the fashion of a surface contact, the reliability on the connection between these two elements 5 and 4 is greatly enhanced. Simultaneously, fraying of the terminal ends of the braided wires 3 is suppressed.
Also, because the rib-like connecting portion 5 and the core wires 6 are formed at their mutually separate positions, there is no need to cut the braided wires 3 for the purpose of preventing the occurrence of a short-circuiting.
Also, the outer covering 2 a that has been partly separated from the insulating outer covering 2 is used to prevent the fraying of the terminal end portions 3 a of the braided wires 3 without being taken away.
Further, because the shield terminal 4 is connected to the forward end of the shield electric wire 1 beforehand, the operation of mounting to the housing not illustrated becomes easy to perform.
In the shield-terminal connection method of the shield electric wire according to this embodiment, the braided wires 3 exposed from the insulating outer covering 2 are drawn up to the end surface of the insulating outer covering 2 and collected together. By doing so, the rib-like connecting portion 5 consisting of the braided wires 3 is formed. And to this rib-like connecting portion 5 is connected the shield terminal 4 . For this reason, the rib-like connecting portion 5 and the shield terminal 4 are joined together in the fashion of a surface contact. As a result of this, the reliability on the connection between these two elements 5 and 4 is greatly enhanced. Also, because there is no need to cut and remove the braided wires 3 for the sake of preventing short-circuiting, the working operation efficiency is excellent.
Also, as mentioned above, the separated outer covering 2 a is drawn up to the end surface of the insulating outer covering 2 together with the exposed braided wires 3 , and the rib-like connecting portion 5 consisting of the braided wires 3 is thereby formed. And to this rib-like connecting portion 5 is connected the shield terminal 4 . Therefore, the reliability on the connection between the rib-like connecting portion 5 and the shield terminal 4 is enhanced. In addition, the fraying of the terminal end portions of the braided wires 3 is prevented by the separated outer covering 2 a that is to be thrown away.
Although an explanation has been above given of the concrete embodiment to which the present invention has been applied, this invention is not limited thereto and permits various changes and modifications to be made.
In the above-described embodiment, the rib-like connecting portion 5 has been formed using the outer covering 2 a that has been partly separated from the insulating outer covering 2 . However, as illustrated in FIG. 7, the rib-like connecting portion 5 may be formed by eliminating the separated outer covering 2 a and drawing up the braided wires 3 to the side of the cut end surface manually or by means of a jig. In this case, even when there exists no separated outer covering 2 a , the connection portion 12 is connected to the rib-like connecting portion 5 in the fashion of a surface contact. Therefore, the fraying of the ends of the braided wires 3 is prevented.
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A shield electric wire includes braided wires, an outer insulating portion for covering the braided wires, and a rib-like connecting portion that is formed by part of the braided wires. A second outer insulating portion is provided that is formed by separating it from an end of the outer insulating portion and dragging it away from the end of the outer insulating portion to expose part of the braided wires. The second outer insulating portion remains on the braided wires to cover the ends of the braided wires. The second outer insulating portion is then drawn back towards the end of the outer insulating portion to draw up and collect the parts of the braided wires exposed between the outer insulating portion and the second outer insulating portion to thereby form the rib-like connecting portion. A shield terminal is connected to the connecting portion.
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CROSS-REFERENCE TO RELATED APPLICATIONS
This application is a continuation of U.S. patent application Ser. No. 11/557,587, filed Nov. 8, 2006, the disclosure of which is incorporated by reference herein in its entirety.
TRADEMARKS
IBM® is a registered trademark of International Business Machines Corporation, Armonk, N.Y., U.S.A. Other names used herein may be registered trademarks, trademarks or product names of International Business Machines Corporation or other companies.
BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention relates to computer systems and, more specifically, to a method and a system for maximizing the throughput of a computer system in the presence of one or more power constraints.
2. Description of Background
From small clusters of computers to large supercomputers, peak power consumption places a major constraint on the scalability of computer systems. For purposes of cost effectiveness, a computing system may initially comprise a small number of computing elements. At some point, it may be necessary to scale the computing system by adding additional computing elements so as to increase the overall processing capacity of the system. However, each of the components added to the system also increases the overall power consumption of the aggregate system. Energy constraints may prevent the use of computer systems which are capable of providing high throughput. In particular, peak power consumption is constrained such that computer processors are unable to operate at full computational capacity. What is needed is a control system that maximizes throughput in view of energy constraints.
SUMMARY OF THE INVENTION
Methods are provided for maximizing the throughput of a computer system in the presence of one or more power constraints by repeatedly or continuously optimizing task scheduling and assignment for each of a plurality of components of the computer system. The components include a plurality of central processing units (CPUs) each operating at a corresponding operating frequency. The components also include a plurality of disk drives. The corresponding operating frequencies of one or more CPUs of the plurality of CPUs are adjusted to maximize computer system throughput under one or more power constraints. Optimizing task scheduling and assignment, as well as adjusting the corresponding operating frequencies of one or more CPUs, are performed by solving a mathematical optimization problem using a first methodology over a first time interval and a second methodology over a second time interval longer than the first time interval. The first methodology comprises a short-term heuristic solver for adapting to computer system changes that occur over the first time interval. The second methodology comprises a long-term solver for adapting to computer system changes that occur over the second time interval, wherein the second methodology has greater accuracy and greater computational complexity than the first methodology.
Additional features and advantages are realized through the techniques of the present invention. Other embodiments and aspects of the invention are described in detail herein and are considered a part of the claimed invention. For a better understanding of the invention with advantages and features, refer to the description and to the drawings.
TECHNICAL EFFECTS
As a result of the summarized invention, technically we have achieved a solution wherein the components of a computer system are proactively controlled so as to limit power consumption with minimal degradation in computer system throughput. By limiting power consumption in this manner, these components may be packed more densely than what is currently practicable while still conforming to predetermined limits on power dissipation and power consumption.
BRIEF DESCRIPTION OF THE DRAWINGS
The subject matter, which is regarded as the invention is particularly pointed out and distinctly claimed in the claims at the conclusion of the specification. The foregoing and other objects, features, and advantages of the invention are apparent from the following detailed description taken in conjunction with the accompanying drawings in which:
FIG. 1 is a block diagram illustrating an exemplary embodiment of a system for maximizing the throughput of a computer system under peak power constraints.
FIG. 2 is a block diagram illustrating a further exemplary embodiment of a system for maximizing the throughput of a computer system under peak power constraints.
FIG. 3 is a flowchart illustrating an exemplary method for maximizing the throughput of a computer system under peak power constraints.
Like reference numerals are used to refer to like elements throughout the drawings. The detailed description explains the preferred embodiments of the invention, together with advantages and features, by way of example with reference to the drawings.
DETAILED DESCRIPTION OF THE INVENTION
The following description of systems and methods for maximizing the throughput of a computer system in the presence of power constraints utilizes the following terms:
“Workload” is defined as the amount of input/output (I/O) utilization, processor utilization, or any other performance metric of servers employed to process or transmit a data set.
“Throughput” is the amount of workload performed in a certain amount of time.
“Processing capacity” is the configuration-dependent maximum level of throughput.
“Frequency throttling” is an illustrative example of a technique for changing power consumption of a system by reducing or increasing the operational frequency of a system. For example, by reducing the operating frequency of a processor under light workload requirements, the processor (and system) employs a significantly less amount of power for operation, since power consumed is related to the power supply voltage and operating frequency. Although frequency throttling has been applied to central processing units (CPUs), the operational frequency or speed of system components other than CPUs may also be adjusted or controlled. As a general consideration, the operational frequency or speed of a component may be related to the energy consumption level of that component. Any of several techniques may be employed to adjust or control the frequency of a system component. These may, but need not, include changing the system supply voltage or controlling a clock gate to eliminate a portion or fraction of a clock signal. Changing the system supply voltage is an effective technique for adjusting the operational frequency of a system component, but a processing delay may occur until this voltage stabilizes. Controlling the clock gate will not cause a substantial processing delay. Illustratively, the embodiments disclosed herein may utilize any of a fixed set of operational frequencies available to a system component. The fixed set of operational frequencies is selected to provide energy efficient operation. Energy efficient operation often exhibits a non-linear dependence on processing speed, thus making system optimization more difficult. Accordingly, less efficient but readily available technologies may be used to provide system optimization, such as permitting a CPU to momentarily exceed its power budget.
FIG. 1 is a block diagram illustrating an exemplary embodiment of a system for maximizing the throughput of a computer system under peak power constraints. The system is capable of proactively managing and controlling large-scale computer systems ranging from small clusters to large data centers and supercomputers. Since these large-scale computer systems are to be managed and controlled, they are referred to hereinafter as a controlled system 101 .
In the illustrative example of FIG. 1 , controlled system 101 includes a first hardware component 103 and a second hardware component 105 . However, a typical controlled system 101 includes numerous hardware components such as computing devices, storage devices, I/O and network devices, cooling devices, and so forth. Each of these component categories could, but need not, be implemented using a plurality of virtually identical devices. A computing device could, for example, be implemented using a general purpose computer equipped with one or more central processing units (CPUs), random access memory (RAM), one or more hard disk drives, and a network adapter, and capable of executing an operating system such as Linux. The components could be organized in various architectures, e.g., flat (a group of standalone computers) or hierarchical (grouped into clusters of servers/cabinets/chassis in which peripherals are shared).
A controlling system 107 is employed to proactively manage and control controlled system 101 . Controlling system 107 is capable of interacting with a plurality of components of controlled system 101 . Illustratively, controlling system 107 is implemented using a software program running on a general-purpose computer referred to as a resource manager 109 . Resource manager 109 is capable of accessing a policy database 111 stored on a computer-readable storage medium. Controlling system 107 could, but need not, be a part of controlled system 101 . Controlling system 107 controls controlled system 101 by repeatedly or continuously receiving information from the hardware components of the controlled system (such as first hardware component 103 and second hardware component 105 ) related to the current configuration of the components, workload of the components, and performance of the components. Based upon this received information, controlling system 107 provides first and second hardware components 103 , 105 with electric power budgets and configuration changes. An electric power budget specifies an upper bound on power consumption for a component. Illustratively, a component may, but need not, be responsible for maintaining adherence to this electric power budget.
Controlling system 107 controls assignment of tasks to the hardware components such as, for example, migrating a task from first hardware component 103 to second hardware component 105 . Controlling system 107 maintains a set of power constraints while maximizing throughput of controlled system 101 . This functionality is implemented by controlling system 107 receiving one or more external inputs from external sources such as a first external sensor 113 and a second external sensor 115 . First external sensor 113 may represent a temperature sensor, an electric power controller, or another type of sensor. Similarly, second sensor 115 may represent a temperature sensor, an electric power sensor, or another type of sensor. Controlling system 107 also includes an input/output device 117 for accepting an input from a human operator and for providing an output to a human operator. In response to at least one of first external sensor 113 , second external sensor 115 , or input/output device 117 , resource manager 109 modifies power constraints and/or optimization parameters for controlled system 101 .
Controlling system 107 interacts with first and second external sensors 113 , 115 and first and second hardware components 103 , 105 to monitor controlled system 101 on a continuous or repeated basis. Typically, this monitoring is periodic and performed at fixed intervals such as every five seconds. Additionally or alternatively, this monitoring may include resource manager 109 sending a message to input/output device 117 in response to at least one of first external sensor 113 or second external sensor 115 sensing a predetermined event. During this monitoring process, controlling system 107 receives updated information from first hardware component 103 and second hardware component 105 pertaining to each component's current physical and logical configurations, as well as each component's current workload and performance.
Physical configuration data includes a component's installed hardware (such as RAM), the hardware's settings (e.g., CPU frequency and voltage), and available peripherals (e.g., active network and storage devices). Logical configuration data includes information regarding an operating system installed on the component, as well as any runtime parameters for the component. Workload data contains statistics regarding the task or tasks currently performed by the component. For example, if the component is a computing device, workload data includes a relative intensity for each of a plurality of tasks in terms of CPU, memory, disk space, or network access. If the component is a network or storage device, workload data includes the number and intensity of flows that traverse the component. Performance data includes information regarding the utilization of the component (such as a cache missed count), the progress of any task or tasks assigned to the component (such as the number of each task's instructions that have been executed), and the current physical conditions under which the component is operating (such as a device's power consumption and internal temperature).
Controlling system 107 outputs an electric power budget and configuration changes to each of a plurality of components, such as first hardware component 103 and second hardware component 105 . The power budget is a limit on the actual power consumption of the component. If controlling system 107 has control over an electric power supply, then the controlling system can physically enforce power budget limits for one or more components as, for example, by disconnecting power to components that violate the limit. Alternatively or additionally, each component is responsible for adhering to its power budget by routinely measuring its own power consumption and taking action in response thereto when measured power consumption exceeds the budget limit. If each component is responsible for adhering to its own power budget, this is helpful in situations where the response time of the component is shorter than the response time of controlling system 107 .
From time to time, controlling system 107 may receive an input from first external sensor 113 or second external sensor 115 and, in response thereto, modify one or more power constraints or configuration parameters. For example, overall power consumption may be severely constrained due to a power failure, or if a particular location exceeds a predetermined room temperature threshold, then all components proximate to that location might be constrained to a total power consumption which is considerably less than current (or recent) power consumption. By means of input/output device 117 , a human operator can manually place ad-hoc constraints or relax existing constraints, according to external considerations (i.e., short-term peak performance). Similarly, the operator may change various optimization parameters, for example, by modifying task priorities or by relaxing fairness requirements.
Controlling system 107 may instruct first hardware component 103 or second hardware component 105 to change its configuration. A configuration change includes any of: (a) shutting the component down or putting the component into a low-power consumption (standby) mode for a limited or indefinite time, (b) changing a component setting such as frequency and/or voltage, or (c) turning off some subcomponents of the component (like RAM, hard disks, or network adapters). Such changes may have a negative effect on component throughput, but one function of controlling system 107 is to assess controlled system 101 for the purpose of determining which change or changes will provide the least degradation of overall throughput.
Controlling system 107 controls assignment of tasks to first and second hardware components 103 , 105 . Controlling system 107 also controls migration of tasks from first hardware component 103 to second hardware component 105 , and from second hardware component 105 to first hardware component 103 . In order to implement these assignments and migrations, controlling system 107 may be provided with a list or set of permissible hardware components to which a given task or category of tasks may be assigned, a speed estimation algorithm for estimating execution speed of a task on every permissible hardware component, and a resource estimation algorithm for estimating time and bandwidth required for a potential migration. However, these estimation algorithms and task lists are greatly simplified if every single task is permissible on a set of substantially identical hardware components.
FIG. 2 is a block diagram illustrating a further exemplary embodiment of a system for maximizing the throughput of a computer system under peak power constraints. The embodiment of FIG. 2 is based upon the exemplary system depicted in FIG. 1 wherein controlled system 101 ( FIG. 1 ) includes M groups of machines, M representing a positive integer. For example, controlled system 101 of FIG. 1 may include a first group of machines 201 ( FIG. 2 ), a second group of machines 202 , and a third group of machines 203 . Each group contains at most K identical machines, where K is a positive integer greater than one, possibly with additional resources shared among these K identical machines. Machines in different groups need not be identical. For example, first group of machines 201 includes a first processing unit 211 and a second processing unit 212 . Illustratively, first and second processing units 211 , 212 may each be implemented, for example, using a CPU, a blade having one or more CPUs, or a computer server.
First and second processing units 211 , 212 are shown for purposes of illustration, as first group of machines 201 could include any number of processing units greater than zero. In the case of a blade implementation, a single chassis could be employed containing at most K blades and an Ethernet switch module. This chassis could possibly be accompanied by a dedicated storage server, with each blade running a Linux operating system. Each machine, which in this example includes each of K blades, is executing zero or more tasks assigned thereto by resource manager 109 . Resource manager 109 is illustratively implemented using a database server or web server. The assignment of tasks to machines may be determined in advance, may change with time, and/or may be determined exogenously (by a human operator, for instance). Optionally, each task is assigned a corresponding level of priority.
Second group of machines 202 includes a first network unit 221 and a second network unit 222 . However, first and second network units 221 , 222 are shown for purposes of illustration, as second group of machines 202 could include any number of network units greater than one. First and second network units 221 , 222 are illustratively implemented using network adapters. Third group of machines 203 includes a first storage unit 231 and a second storage unit 232 . However, first and second storage units 231 , 232 are shown for purposes of illustration, as third group of machines 203 could include any number of storage units greater than one. First and second storage units 231 , 232 are illustratively implemented using hard disk drives, storage drives for magnetic tape, or any other type of data storage drive that includes a computer readable storage medium.
Each group of machines 201 , 202 , 203 may be capable of controlling its maximum power consumption so as to adhere to a given limit called a power budget. Alternatively, each machine in each group of machines 201 , 202 , 203 may be capable of controlling its maximum power consumption so as to adhere to the power budget. Such control may be achieved, for example, by measuring actual power consumption at fixed or repeated intervals (e.g., every 2 milliseconds) and throttling the machine (i.e., decreasing CPU frequency) whenever the actual consumption approaches or exceeds the power budget limit. This limit can be changed in fixed intervals, such as every one second.
Controlling system 107 ( FIGS. 1 and 2 ) assigns a power budget to each of the M machine groups or, alternatively, to each machine. The power budgets must satisfy a constraint that the sum of power budgets cannot exceed a limiting value E max that was given to controlling system 107 . For example, controlling system 107 can possibly split the total power budget equally among the M groups by assigning a budget of E max /M to each group, but this allocation could possibly be improved, for example, if the various groups of machines (1) run different workloads, (2) contain different machines in terms of brand, model, or architecture, or (3) contain a different number of machines. Additionally, controlling system 107 guarantees certain fairness conditions, such that each group of machines may receive a minimum power budget of at least E max /8M, unless a smaller budget suffices for that group to handle its workload (i.e., in the case of a web server that receives very few hits).
Alternatively or additionally, controlling system 107 may assign tasks to individual machines. More precisely, each task is associated with a particular group of the M groups (fixed in advance), and controlling system 107 assigns the task to one of the machines in the particular group. This assignment can be changed over time. However, a certain overhead is incurred in changing the assignment in terms of latency caused by moving data. Controlling system 107 receives details regarding each machine, such as its utilization and power consumption, so as to identify over utilized and underutilized machines, and to transfer tasks from the former to the latter if the underutilized and over utilized machines are in the same group.
FIG. 3 is a flowchart illustrating an exemplary method for maximizing the throughput of a computer system under peak power constraints. The process commences at block 301 where logical and physical information is collected from controlled system 101 ( FIG. 1 ) and external sensors (such as first external sensor 113 and second external sensor 115 ). Next, a mixed integer optimization problem is formulated based upon one or more power constraints ( FIG. 3 , block 303 ). Formulation of this mixed integer optimization problem is described in greater detail hereinafter. The mixed integer optimization problem is solved (block 305 ). The configuration of controlled system 101 ( FIG. 1 ) is updated with a new power budget and new task allocations ( FIG. 3 , block 307 ). The process then loops back to block 301 .
The mixed integer optimization problem of block 303 is formulated as follows. One objective of controlling system 107 ( FIGS. 1 and 2 ) is to maximize overall throughput of controlled system 101 ( FIGS. 1 and 2 ) subject to given power constraints. The throughput is defined as the total number of instructions of all tasks in the system which are executed per unit of time (i.e., one second). Controlling system 107 also ensures additional properties, such as fairness, by introducing additional constraints that avoid undesired effects. In situations where time allows, controlling system 107 may solve a constrained optimization problem whose objective is to process as many instructions per time unit as possible. Accordingly, this optimization problem is formulated as a mixed integer programming problem to be solved during each of a plurality of time intervals.
The elements of the optimization problem are as follows. There is a set of indices of machines {1, . . . ,m}, a set of indices of tasks {1, . . . ,n}, and a set of indices of CPU frequencies {1, . . . ,s}. The following attributes of controlled system 101 are inputted to the mixed in integer programming problem as parameters:
W i —the importance (or “priority”) of task i:
M i —the machine on which task i is currently run (or 0 if none);
G ij —the cost of transferring task i to machine j≠M i ;
F k —the kth CPU frequency value (k=0,1, . . . ,s);
H ik —the average number of cycles per instruction for task i running on a machine operating at the kth CPU frequency (this estimate captures expected I/O and memory delays);
E max —Maximum-energy-consumption bound, which controlled system 101 must obey due to current physical conditions, such as temperature or power supply;
E jk —the amount of energy per time unit consumed by machine j when machine j is operating at frequency F k ;
B—a task-fairness parameter representing the maximum possible ratio between the number of CPU cycles planned for a single task and that of an average task.
Variables. The mixed integer linear programming problem looks for a currently optimal configuration for the managed system. This configuration includes assignment of tasks to machines and an allocation of an energy “budget” for each machine. The mixed integer linear programming problem is solved using an algorithm that uses one or more of the following decision variables:
z j —a Boolean variable indicating whether machine j is active or not;
x ij —a Boolean variable indicating whether or not task i is assigned to machine j;
y jk —a Boolean variable indicating whether or not machine j is working at frequency F k ;
f ijk —a continuous variable representing the number of CPU cycles per time unit that is planned for task i on machine j running at the kth CPU frequency. Note that each task is processed by only one machine having a CPU that operates at only one frequency;
v ij —a continuous variable representing the number of instructions per time unit that is planned for task i on machine j. Each task is processed by only one machine;
u j —a continuous variable representing the energy upper bound (“budget”) allocated to machine j;
Objective function. The algorithm solves the problem of maximizing the total planned number of instructions per time unit. This quantity of instructions is equal to
∑ i = 1 n ∑ j = 1 m W i v ij .
In addition, the algorithm penalized the transferring of tasks from one machine to another; this quantity is equal to
∑ i = 1 n ∑ j ≠ M i G ij x ij .
Hence, the algorithm's objective function is given by
∑
i
=
1
n
(
∑
j
=
1
m
W
i
v
ij
-
∑
j
≠
M
i
G
ij
x
ij
)
Constraints. The optimization is subject to constraints as follows. In the sequel, let [t]={1, . . . ,t}.
Consistency constraints:
x ij ≦z j for all iε[n], jε[m]
meaning that the tasks can be assigned only to active machines;
∑ j = 1 m x ij = 1 for all i ∈ [ n ]
meaning that each task is assigned to a single machine;
∑ k = 0 s y jk = z j for all j ɛ [ m ]
meaning that one frequency has to be selected for each machine;
f ijk ≦F s x ij for all iε[n],jε[m],kε[s]
meaning that task execution takes place only on assigned machines;
f ijk ≦F k y jk for all iε[n],jε[m],kε[s]
meaning that task execution takes place only at assigned CPU frequency;
v ij ≤ ∑ k = 1 s f ijk / H ik for all j ∈ [ m ]
meaning that the number of instructions planned is proportional to the number of cycles planned, according to that task's effectiveness at that frequency.
∑ j = 1 m ∑ k = 1 s f ijk ≥ B · W i ∑ l = 1 n W l · ∑ j = 1 m ∑ k = 1 s F k y jk for all i ∈ [ n ]
meaning that the number of cycles planned for a task is at least a B-fraction the number of cycles planned for an average task.
∑ k = 1 s E jk Y jk ≤ u j for all j ∈ [ m ]
representing an energy budget constraint;
∑ j = 1 n u j ≤ E max
representing the total energy constraint.
Remarks. A preferred embodiment may generalize or specialize the above by having some or all of the following properties.
Machines may each have different maximum CPU frequencies, and this property may be modeled by letting s be the maximum possible frequency and adding the constraint y ik =0 whenever machine j cannot run at the kth CPU frequency. Tasks cannot be transferred to other machines (i.e., task i must be assigned to machine M i ). The cost of transferring a task does not depend on the target machine, i.e., G ij is the same for all j≠M i . The m machines are partitioned into p groups, and a task can only be transferred to machines in the same group, i.e., G ij =∞ for all j in a different group than M i . The total energy consumption of a subset J ⊂ [m] of the machines might be limited to some amount E J (e.g., due to power failure or infrastructure), which is modeled by adding the constraint
∑
j
∈
J
u
j
≤
E
J
The number of cycles planned for task i is limited by a bound C i (e.g., to model task serving a limited number of requests), which is modeled by adding the constraint
∑
j
=
1
m
v
ij
≤
C
i
Additional fairness constraints can limit the ratio between the number of instructions planned for task i and that planned for task i′ by some parameters L 1 ,L 2 >0 (e.g., to make sure these tasks can progress simultaneously), which is modeled by adding the constraint
L
1
∑
j
=
1
m
v
ij
≤
∑
j
=
1
m
v
i
′
j
≤
L
2
∑
j
=
1
m
v
ij
Updating the configuration of controlled system 101 ( FIG. 1 ) as described in block 307 of FIG. 3 may, but need not, include one or more of the following processes. Task scheduling and assignment may be optimized by scheduling a first task to be performed by at least one of the plurality of CPUs simultaneously with a second task to be performed by at least one of the plurality of disk drives. At least one CPU of the plurality of CPUs may be powered down, thereby scheduling a third task to be performed by fewer CPUs of the plurality of CPUs. At least one of the plurality of disk drives may be powered down, thereby scheduling a fourth task to be performed by fewer disk drives of the plurality of disk drives. A lower performing CPU of the plurality of CPUs may be allocated to a fifth task. A lower performing disk drive of the plurality of disk drives may be allocated to a sixth task. A seventh task and an eighth task may be scheduled to execute simultaneously on the plurality of CPUs, wherein the sixth and seventh tasks are independent of each other.
As described above the parameters to this model are given to the system based on the system configuration and recent estimates about the task resource requirements. Thus, every time the mixed-integer program is solved, the parameters may have different values, yielding a different solution. Similarly, new constraints may be added, permanently or temporarily, either by an operator or as an automatic response to existing conditions, again leading to changes in the solution.
The capabilities of the present invention can be implemented in software, firmware, hardware or some combination thereof As one example, one or more aspects of the present invention can be included in an article of manufacture (e.g., one or more computer program products) having, for instance, computer usable media. The media has embodied therein, for instance, computer readable program code means for providing and facilitating the capabilities of the present invention. The article of manufacture can be included as a part of a computer system or sold separately. Additionally, at least one program storage device readable by a machine, tangibly embodying at least one program of instructions executable by the machine to perform the capabilities of the present invention can be provided.
The flow diagrams depicted herein are just examples. There may be many variations to these diagrams or the steps or operations described therein without departing from the spirit of the invention. For instance, the steps may be performed in a differing order, or steps may be added, deleted or modified. All of these variations are considered a part of the claimed invention.
While the preferred embodiment to the invention has been described, it will be understood that those skilled in the art, both now and in the future, may make various improvements and enhancements which fall within the scope of the claims which follow. These claims should be construed to maintain the proper protection for the invention first described.
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Methods are provided for maximizing the throughput of a computer system in the presence of one or more power constraints. Throughput is maximized by repeatedly or continuously or periodically optimizing task scheduling and assignment for each of a plurality of components of a computer system. The components include a plurality of central processing units (CPUs) each operating at a corresponding operating frequency. The components also include a plurality of disk drives. The corresponding operating frequencies of one or more CPUs of the plurality of CPUs are adjusted to maximize computer system throughput under one or more power constraints. Optimizing task scheduling and assignment, as well as adjusting the corresponding operating frequencies of one or more CPUs, are performed by solving a mathematical optimization problem using a first methodology over a first time interval and a second methodology over a second time interval longer than the first time interval. The first methodology comprises a short term heuristic solver for adapting to computer system changes that occur on a short time scale, and the second methodology comprises a long term solver having greater accuracy and greater computational complexity than the first methodology.
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BACKGROUND OF THE INVENTION
The preparation of a mixture of the α and β isomers of α-pivaloyloxyethyl-(S)-3-(3,4-dihydroxyphenyl)-2-methylalaninate (POE Ester) has been described by W. A. Saari, et al., Journal of Medicinal Chemistry, 21, 746 (1978) and U.S. Pat. No. 3,983,138 who also discloses a process for the resolution of this α/β-isomer mixture to obtain only the α-isomer in its pure state as the hydrochloride salt.
SUMMARY OF THE INVENTION
This invention relates to a novel and economical process for resolving the (α),(β)isomeric mixture of α-pivaloyloxyethyl-(S)-3-(3,4-dihydroxyphenyl)-2-methylalaninate (POE Ester) into highly pure α- and β-isomers. This invention further relates to the resolution of the POE Ester into its α- and β-isomers in the form of their highly pure, crystalline hydrogen tartrate salts enabling them to be readily compounded into suitable pharmaceutical formulations. Isolation of the α and β free base POE Ester compounds allows for great versatility in the formation of other pharmaceutically acceptable salt derivatives.
The resolution process of the instant invention generally includes fractional crystallization of the β-isomer of the POE Ester as its (+)-hydrogen tartrate salt; and, crystallization of the α-isomer from the residual mixture of α- and β-isomer (+) tartrates as its hydrochloride dihydrate salt.
Thus there is provided a process for resolving α-pivaloyloxyethyl-(S)-3-(3,4-dihydroxyphenyl)-2-methylalaninate (POE Ester) into its α- and β-isomers which comprises (a) forming a mixture of α-isomer POE Ester- and β-isomer POE Ester-d(+)-hydrogen tartrate salts; (b) isolating said β-isomer-(+)-hydrogen tartrate salt from said mixture by fractional crystallization, leaving mother liquor containing α- and β-isomer(+)-tartrate salts; and (c) treating said mother liquor from step (b) with first a base and second a mineral acid to form the crystalline α-isomer POE Ester mineral acid salt.
DETAILED DESCRIPTION OF THE INVENTION
The following flow sheet outlines the resolution process of the instant invention. ##STR1##
With reference to the Flow Sheet shown above, the resolution process of the invention more particularly includes preparing the α/β-isomer mixture by treating L-α-methyl-3,4-dihydroxyphenylalanine (L-α-Methyldopa) (I) with α-chlorethylpivalate (II) in a suitable solvent according to the method described by W. A. Saari, et al., supra, which is incorporated herein by reference. A suspension of the resulting α/β-isomer mixture (III) is then dissolved in an organic solvent; for example, ethyl acetate with tetrahydrofuran containing d(+)-tartaric acid and cooled to below 0° C., preferably to -12° C., to separate the isomer mixture into the crystalline and therefore mostly insoluble, β-isomer-(+)-hydrogen tartrate salt (IV) and the soluble α-isomer salt containing some of the β-isomer-(+)-hydrogen tartrate salt (V). The crystalline β-isomer-(+)-hydrogen tartrate salt (IV) may then be isolated and dissolved in water and shaken with a mixture of sodium bicarbonate and dichloromethane to provide a base solution which is then crystallized to isolate the β-isomer base (IV).
The α-isomer is recovered from the mother liquor mixture of α- and β-isomer-(+)-hydrogen tartrate salts (V) by evaporating the liquor to a residue, dissolving the residue in water and removing the α-isomer base by treatment of the solution with a mild base, for example, sodium bicarbonate, and dichloromethane. The resulting dichloromethane solution is evaporated to residue and the residue is crystallized with an aqueous mineral acid, for example, cold, 3.5 N hydrochloric acid. The resultant crystalline solid is first isolated and then dried to yield the α-isomer mineral acid (hydrochloride) dihydrate salt (VII).
The α-isomer hydrochloride dihydrate salt (VII) is converted into the α-isomer base (VIII) by treatment with an aqueous solution of base, for example, by shaking it in a water/sodium bicarbonate/ethyl acetate solution followed by separating, drying and evaporating the organic phase to obtain a solid residue. This residue is then triturated with dichloromethane and hexane is added. The resulting suspension is stirred and the solid that forms is collected, washed and dried to afford the α-isomer base (VIII).
Conversion of the α-isomer base (VIII) into its (+)-hydrogen tartrate salt (IX) may be achieved by treating the α-isomer base (VIII) in a tetrahydrofuran/ethyl acetate solution with d(+)-tartaric acid. The α-isomer-(+)-hydrogen tartrate salt (IX) crystallizes upon the addition of more ethyl acetate prior to being isolated as a white solid.
The resolution process of the invention will become more clear when considered in light of the following examples which further illustrate and set forth the best mode currently known for practicing the invention. The reference numbers shown correspond to those used in the flow sheet.
EXAMPLE 1
Preparation of α/β-Isomer mixture of POE Ester (III)
A suspension of dry (S)-3-(3,4-dihydroxyphenyl)-2-methylalaninate (I) (208 g) in toluene (320 ml), hexamethylphosphoric triamide (400 ml) and α-chloroethyl pivalate (II) (180 g) was stirred under nitrogen at 100° C. until solution occurred. The solution was stirred at 60° C. for 2 hr. and then cooled and poured into chloroform (5.4 l). The reaction product was extracted into water and this solution was made alkaline (pH 8-9) by the addition of sodium bicarbonate while the ester was extracted into dichloromethane (700 ml). The dichloromethane solution was dried and concentrated in vacuo and the α-pivaloyloxyethyl-(S)-3-(3,4-dihydroxyphenyl)-2-methylalaninate (III) was caused to precipitate from the concentrate by the addition of hexane (ca.1 l). This solid was collected, washed once with hexane (500 ml) and then dried, to give 100-130 g (31-40%) of white solid; m.p. 121°-122° C. Tlc (SiO 2 :ethyl acetate:n-butanol:formic acid:water 60:25:10:5; iodine) showed equal concentrations of α (Rf 0.6) and β (Rf 0.68) isomers; no other materials.
Found: C, 60.0; H, 7.5; N, 4.1; C 17 H 25 NO 6 requires, C, 60.2; H, 7.4; N, 4.1; IR; (nujol) 3520, 3410, 3350, 3280, 1750, 1720, 1280, 1260, 1230, 1200, 1180, 1150, 1123, 1103, 1060, 926, 870, 815, 795 and 773 cm -1 .
The hexamethylphosphoric triamide/toluene solvent may be replaced by diethylacetamide or dimethylacetamide or tetramethylurea for the alkylation reaction.
EXAMPLE 2
Separation of the α- and β-Isomers
d(+)-Tartaric acid (37.9 g, 0.25 mole) dissolved in hot (60° C.) tetrahydrofuran (200 ml) was added to a suspension of the ester isomer mixture (III) of Example 1 (85.7 g, 0.25 mole) in ethyl acetate (250 ml). The resulting solution was diluted with ethyl acetate (1.45 l) and some β-isomer-(+)-hydrogen tartrate crystals (IV) (2.7 g) obtained from a prior experiment were added. These seed crystals generally appear in the solution in 24 to 48 hours at -12° C. The slowly stirred mixture was then cooled at -12° C. for six days. The solid was then collected, washed once each with ethyl acetate (250 ml) and ether (250 ml) dried at 20° C. in vacuo to give 52.5 g (85%) of the β-isomer-(+)-hydrogen tartrate salt of α-pivaloyloxyethyl-(S)-3-(3,4-dihydroxyphenyl)-2-methylalaninate (IV). Tlc showed pure β-isomer (Rf 0.68). Assay by equivalent weight: 100.7%; m.p. 165°-166° C.; single peak by high pressure liquid chromatography.
Found: C, 51.5; H, 6.3; N, 2.8; C 21 H 31 NO 12 requires, C, 51.5; H, 6.4; N, 2.9%.
EXAMPLE 3
Preparation of the β-Isomer Base (VI)
The β-isomer-(+)-hydrogen tartrate salt (IV) (5 g) obtained from Example 2, was dissolved in water (50 ml) and shaken with sodium bicarbonate (5 g) and dichloromethane (200 ml) in order to neutralize the salt and extract the base. The solution of the base was washed once with water (100 ml), dried over sodium sulfate and the solution concentrated in vacuo to 10 ml. The concentrate was then diluted with hexane (40 ml) and the β-isomer base (VI) was allowed to crystallize. The β-isomer base (VI) was isolated by filtration and dried to give a white solid; m.p. 120° C.
Assay by equiv. wt.: 98.9%; Tlc. showed β-isomer with a trace of α-isomer. L.C. showed 99.9 area % single peak; [α] 265 20 =53.7° (C=1) 0.1 N hydrochloric acid; [α] 405 20 =44.3° (C=1) 0.1 N hydrochloric acid.
Found: C, 59.7; H, 7.3; N, 4.0; C 17 H 25 NO 6 requires, C, 60.2; H, 7.4; N, 4.1%. Proton N.M.R. in deuterated methanol: (group, multiplicity) shift; (O--CH, q.) 6.78, (ArH×3, mult.) 6.7, (CH 2 , AB-q.) 3.02 and 2.58, (CH 3 , d) 1.43, (CH 3 , s) 1.35, (t-Bu, s) 1.18 d.
EXAMPLE 4
Preparation of the α-Isomer Hydrochloride (VII)
The mother liquor containing the remainder of the β-isomer-(+)-hydrogen tartrate and all the α-isomer (+) hydrogen tartrate salts from Example 2 was evaporated to residue in vacuo. The residue was then dissolved in water and the base removed by sodium bicarbonate addition followed by extraction into dichloromethane. The dichloromethane solution of the base was then evaporated to residue in vacuo and the residue crystallized from cold 3.5 N aqueous hydrochloric acid (430 ml).
The solid was isolated by filtration and dried over potassium hydroxide, in vacuo to give 46.8 g (90%) of the α-isomer hydrochloride dihydrate salt of α-pivaloyloxyethyl-(S)-3-(3,4-dihydroxyphenyl)-2-methylalaninate (VII).
EXAMPLE 5
Preparation of the α-Isomer Base (VIII)
The hydrochloride dihydrate salt (VII) (254 g) obtained from Example 4 was converted into the base by shaking it in a mixture of water (200 ml), sodium bicarbonate (63 g) and ethyl acetate (2.0.1). The organic phase was separated in a separation funnel, dried and evaporated to leave a solid residue. This residue was triturated with dichloromethane (300 ml) and then hexane (400 ml) was added. The resulting suspension was stirred 30 min. and the solid collected by filtration to give, after washing once with hexane (500 ml) and drying, 200 g of α-isomer base (VIII) (96% of white solid; m.p. 140° C.).
Assay by equiv. wt.: 100%; Tlc. single spot pure α-isomer; L.C. essentially single peak; [α] 365 20 =+20.1 (C=1); [α] 405 20 =+10.1 (C=1) 0.1 N hydrochloric acid.
Found: C, 60.2; H, 7.4; N, 4.1; C 17 H 25 NO 6 requires, C, 60.2; H, 7.4; N, 4.1%. Proton N.M.R. identical to β-isomer.
EXAMPLE 6
Preparation of the α-Isomer-(+)-Hydrogen Tartrate Salt (IX)
The α-isomer base (VIII) of Example 5 was converted into its (+)-hydrogen tartrate salt (IX) by treatment in tetrahydrofuran/ethyl acetate (100 ml each) with an equimolar quantity of (+)-tartaric acid. Addition of more ethyl acetate (900 ml) caused the α-isomer of α-pivaloyl-oxyethyl-(S)-3-(3,4-dihydroxyphenyl)-2-methylalaninate (+) hydrogen tartrate salt (IX) to crystallize. This product was then isolated by filtration as a white solid m.p. 161°-162.5° C. Tlc.: Pure α-isomer, no other spots. Assay by equivalent weight: 99.9%; 99.7% pure by high pressure liquid chromatography.
Found: C, 50.7; H, 6.2; N, 2.8; C 21 H 31 NO 12 requires, C, 51.5; H, 6.3; N, 2.9%.
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Resolution of the α and β isomers of α-pivaloyloxyethyl-(S)-3-(3,6-dihydroxyphenyl)-2-methylalaninate is accomplished by; (a) forming the (+) hydrogen tartrate salt of the mixture; (b) fractionally crystallizing the β-isomer salt; and (c) recovering the α-isomer from the mother liquor by treatment with first a base and second a mineral acid.
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RELATED APPLICATIONS
This application claims priority of U.S. Provisional Application Ser. No. 60/530,132, which was filed on Dec. 16, 2003.
TECHNICAL FIELD
The present invention relates to rope systems and methods and, in particular, to wrapped yarns that are combined to form strands for making ropes having predetermined surface characteristics.
BACKGROUND OF THE INVENTION
The characteristics of a given type of rope determine whether that type of rope is suitable for a specific intended use. Rope characteristics include breaking strength, elongation, flexibility, weight, and surface characteristics such as abrasion resistance and coefficient of friction. The intended use of a rope will determine the acceptable range for each characteristic of the rope. The term “failure” as applied to rope will be used herein to refer to a rope being subjected to conditions beyond the acceptable range associated with at least one rope characteristic.
The present invention relates to ropes with improved surface characteristics, such as the ability to withstand abrasion or to provide a predetermined coefficient of friction. Typically, a length of rope is connected at first and second end locations to first and second structural members. Often, the rope is supported at one or more intermediate locations by intermediate structural surfaces between the first and second structural members. In the context of a ship, the intermediate surface may be formed by deck equipment such as a closed chock, roller chock, bollard or bit, staple, bullnose, or cleat.
When loads are applied to the rope, the rope is subjected to abrasion where connected to the first and second structural members and at any intermediate location in contact with an intermediate structural member. Abrasion and heat generated by the abrasion can create wear on the rope that can affect the performance of the rope and possibly lead to failure of the rope. In other situations, a rope designed primarily for strength may have a coefficient of friction that is too high or low for a given use.
The need thus exists for improved ropes having improved surface characteristics, such as abrasion resistance or coefficient of friction; the need also exists for systems and methods for producing such ropes.
RELATED ART
U.S. Pat. No. 3,367,095 to Field, Jr, discloses a process and apparatus for making wrapped yarns. The wrapped yarn of the '095 patent comprises a core formed of continuous fibers and a wrapping formed of discontinuous fibers. The '095 patent generally teaches that all synthetic and natural fibers including metal, glass, and asbestos may be used to form the core and wrapping but does not specify particular combinations of such materials for particular purposes.
SUMMARY OF THE INVENTION
The present invention is a rope having improved surface characteristics and method of making the same. The rope comprises a plurality of yarns. At least one of the yarns comprises first and second sets of fibers. The first fibers are formed of a first material, and the second set of second fibers at least partly surrounds the first fibers. The second fibers are formed of a second material. The first material defines a set of operating characteristics adapted to bear tension loads on the rope. The second material defines a set of operating characteristics adapted to affect at least one surface characteristic of the rope.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1A is a side elevation view of a wrapped yarn that may be used to construct a rope of the present invention;
FIG. 1B is an end elevation cutaway view depicting the yarn of FIG. 1A ;
FIG. 2 is a side elevation view of a first example of a rope of the present invention;
FIG. 3 is a radial cross-section of the rope depicted in FIG. 2 ;
FIG. 4 is a close-up view of a portion of FIG. 3 ;
FIG. 5 is a side elevation view of a second example of a rope of the present invention;
FIG. 6 is a radial cross-section of the rope depicted in FIG. 5 ;
FIG. 7 is a close-up view of a portion of FIG. 6 ;
FIG. 8 is a side elevation view of a first example of a rope of the present invention;
FIG. 9 is a radial cross-section of the rope depicted in FIG. 8 ;
FIG. 10 is a close-up view of a portion of FIG. 9 ; and
FIG. 11 is a side elevation view of a first example of a rope of the present invention;
FIG. 12 is a radial cross-section of the rope depicted in FIG. 8 ;
FIG. 13 is a close-up view of a portion of FIG. 9 ; and
FIG. 14 is a schematic diagram representing an example process of fabricating the yarn depicted in FIGS. 1A and 1B .
DETAILED DESCRIPTION OF THE INVENTION
Referring initially to FIGS. 1A and 1B of the drawing, depicted therein is a blended yarn 20 constructed in accordance with, and embodying, the principles of the present invention. The blended yarn 20 comprises at least a first set 22 of fibers 24 and a second set 26 of fibers 28 .
The first and second fibers 24 and 28 are formed of first and second materials having first and second sets of operating characteristics, respectively. The first material is selected primarily to provide desirable tension load bearing characteristics, while the second material is selected primarily to provide desirable abrasion resistance characteristics.
In addition to abrasion resistance, the first and second sets of operating characteristics can be designed to improve other characteristics of the resulting rope structure. As another example, certain materials, such as HMPE, are very slick (low coefficient of friction). In a yarn consisting primarily of HMPE as the first set 22 for strength, adding polyester as the second set 26 provides the resulting yarn 20 with enhanced gripping ability (increased coefficient of friction) without significantly adversely affecting the strength of the yarn 20 .
The first and second sets 22 and 26 of fibers 24 and 28 are physically combined such the first set 22 of fibers 24 is at least partly surrounded by the second set 26 of fibers 28 . The first fibers 24 thus form a central portion or core that is primarily responsible for bearing tension loads. The second fibers 28 form a wrapping that at least partly surrounds the first fibers 24 to provide the rope yarn 20 with improved abrasion resistance.
The example first fibers 24 are continuous fibers that form what may be referred to as a yarn core. The example second fibers 28 are discontinuous fibers that may be referred to as slivers. The term “continuous” indicates that individual fibers extend along substantially the entire length of the rope, while the term “discontinuous” indicates that individual fibers do not extend along the entire length of the rope.
As will be described below, the first and second fibers 24 and 28 may be combined to form the example yarn using a wrapping process. The example yarn 20 may, however, be produced using process for combining fibers into yarns other than the wrapping process described below.
With the foregoing understanding of the basic construction and characteristics of the blended yarn 20 of the present invention in mind, the details of construction and composition of the blended yarn 20 will now be described.
The first material used to form the first fibers 24 may be any one or more materials selected from the following group of materials: HMPE, LCP, or PBO fibers. The second material used to form the second fibers 28 may be any one or more materials selected from the following group of materials: polyester, nylon, Aramid, LCP, and HMPE fibers.
The first and second fibers 24 and 28 may be the same size or either of the fibers 24 and 28 may be larger than the other. The first fibers 24 are depicted with a round cross-section and the second fibers 28 are depicted with a flattened cross-section in FIG. 1B for clarity. However, the cross-sectional shapes of the fibers 24 and 28 can take forms other than those depicted in FIG. 1B . The first fibers 24 are preferably generally circular. The second fibers 28 are preferably also generally circular.
The following discussion will describe several particular example ropes constructed in accordance with the principles of the present invention as generally discussed above.
First Rope Example
Referring now to FIGS. 2 , 3 , and 4 , those figures depict a first example of a rope 30 constructed in accordance with the principles of the present invention. As shown in FIG. 2 , the rope 30 comprises a rope core 32 and a rope jacket 34 . FIG. 2 also shows that the rope core 32 and rope jacket 34 comprise a plurality of strands 36 and 38 , respectively. FIG. 4 shows that the strands 36 and 38 comprise a plurality of yarns 40 and 42 and that the yarns 40 and 42 in turn each comprise a plurality of fibers 44 and 46 , respectively.
One or both of the example yarns 40 and 42 may be formed by a yarn such as the abrasion resistant yarn 20 described above. However, because the rope jacket 34 will be exposed to abrasion more than the rope core 32 , at least the yarn 42 used to form the strands 38 should be fabricated at least partly from the abrasion resistant yarn 20 described above.
The exemplary rope core 32 and rope jacket 34 are formed from the strands 36 and 38 using a braiding process. The example rope 30 is thus the type of rope referred to in the industry as a double-braided rope.
The strands 36 and 38 may be substantially identical in size and composition. Similarly, the yarns 40 and 42 may also be substantially identical in size and composition. However, strands and yarns of different sizes and compositions may be combined to form the rope core 32 and rope jacket 34 .
As described above, fibers 44 and 46 forming at least one of the yarns 40 and 42 are of two different types. In the yarn 40 of the example rope 30 , the fibers 44 are of a first type corresponding to the first fibers 24 and a second type corresponding to the second fibers 28 . Similarly, in the yarn 42 of the example rope 30 , the fibers 46 are of a first type corresponding to the first fibers 24 and a second type corresponding to the second fibers 28 .
Second Rope Example
Referring now to FIGS. 5 , 6 , and 7 , those figures depict a second example of a rope 50 constructed in accordance with the principles of the present invention. As perhaps best shown in FIG. 6 , the rope 50 comprises a plurality of strands 52 . FIG. 7 further illustrates that each of the strands 52 comprises a plurality of yarns 54 and that the yarns 54 in turn comprise a plurality of fibers 56 .
The example yarn 54 may be formed by a yarn such as the abrasion resistant yarn 20 described above. In the yarn 54 of the example rope 50 , the fibers 56 are of a first type corresponding to the first fibers 24 and a second type corresponding to the second fibers 28 .
The strands 52 are formed by combining the yarns 54 using any one of a number of processes. The exemplary rope 50 is formed from the strands 52 using a braiding process. The example rope 50 is thus the type of rope referred to in the industry as a braided rope.
The strands 52 and yarns 54 forming the rope 50 may be substantially identical in size and composition. However, strands and yarns of different sizes and compositions may be combined to form the rope 50 . The first and second types of fibers combined to form the yarns 54 are different as described above with reference to the fibers 24 and 28 .
Third Rope Example
Referring now to FIGS. 8 , 9 , and 10 , those figures depict a third example of a rope 60 constructed in accordance with the principles of the present invention. As perhaps best shown in FIG. 6 , the rope 60 comprises a plurality of strands 62 . FIG. 7 further illustrates that each of the strands 62 in turn comprises a plurality of yarns 64 , respectively. The yarns 64 are in turn comprised of a plurality of fibers 66 .
The example yarn 64 may be formed by a yarn such as the abrasion resistant yarn 20 described above. The fibers 66 of at least some of the yarns 64 are of a first type and a second type, where the first and second types and correspond to the first and second fibers 24 and 28 , respectively.
The strands 62 are formed by combining the yarns 64 using any one of a number of processes. The exemplary rope 60 is formed from the strands 62 using a twisting process. The example rope 60 is thus the type of rope referred to in the industry as a twisted rope.
The strands 62 and yarns 64 forming the rope 60 may be substantially identical in size and composition. However, strands and yarns of different sizes and compositions may be combined to form the rope 60 . The first and second types of fibers are combined to form at least some of the yarns 64 are different as described above with reference to the fibers 24 and 28 .
Fourth Rope Example
Referring now to FIGS. 11 , 12 , and 13 , those figures depict a fourth example of a rope 70 constructed in accordance with the principles of the present invention. As perhaps best shown in FIG. 12 , the rope 70 comprises a plurality of strands 72 . FIG. 13 further illustrates that each of the strands 72 comprise a plurality of yarns 74 and that the yarns 74 in turn comprise a plurality of fibers 76 , respectively.
One or both of the example yarns 74 may be formed by a yarn such as the abrasion resistant yarn 20 described above. In particular, in the example yarns 74 of the example rope 70 , the fibers 76 are each of a first type corresponding to the first fibers 24 and a second type corresponding to the second fibers 28 .
The strands 72 are formed by combining the yarns 74 using any one of a number of processes. The exemplary rope 70 is formed from the strands 72 using a braiding process. The example rope 70 is thus the type of rope commonly referred to in the industry as a braided rope.
The strands 72 and yarns 74 forming the rope 70 may be substantially identical in size and composition. However, strands and yarns of different sizes and compositions may be combined to form the rope 70 . The first and second types of fibers are combined to form at least some of the yarns 74 are different as described above with reference to the fibers 24 and 28 .
Yarn Fabrication
Turning now to FIG. 14 of the drawing, depicted at 120 therein is an example system 120 for combining the first and second materials 24 and 28 to form the example yarn 20 . The system 120 basically comprises a transfer duct 122 , a convergence duct 124 , a suction duct 126 , and a false-twisting device 128 . The first material 24 is passed between a pair of feed rolls 130 and into the convergence duct 124 . The second material 28 is initially passed through a pair of back rolls 142 , a pair of drafting aprons 144 , a pair of drafting rolls 146 , and into the transfer duct 122 .
The example first fibers 24 are continuous fibers that extend substantially the entire length of the example yarn 20 formed by the system 120 . The example second fibers 26 are slivers, or discontinuous fibers that do not extend the entire length of the example yarn 20 .
The second fibers 28 become airborne and are drawn into convergence duct 124 by the low pressure region within the suction duct 126 . The first fibers 24 converge with each other and the airborne second fibers 28 within the convergence duct 124 . The first fibers 24 thus pick up the second fibers 28 . The first and second fibers 24 and 28 are then subsequently twisted by the false-twisting device 128 to form the yarn 20 . The twist is removed from the first fibers 24 of the yarn 20 as the yarn travels away from the false-twisting device 128 .
After the yarn 20 exits the false-twisting device 128 and the twist is removed, the yarn passes through let down rolls 150 and is taken up by a windup spool 152 . A windup roll 154 maintains tension of the yarn 20 on the windup spool 152 .
First Yarn Example
A first example of yarn 20 a that may be fabricated using the system 120 as described above comprises the following materials. The first fibers 24 are formed of HMPE fibers and the second fibers are formed of polyester fibers. The yarn 20 a of the first example comprises between about sixty to eighty percent by weight of the first fibers 24 and between about twenty to forty percent by weight of the second fibers 28 .
Second Yarn Example
A second example of yarn 20 b that may be fabricated using the system 120 as described above comprises the following materials. The first fibers 24 are formed of LCP fibers and the second fibers are formed of a combination of LCP fibers and Aramid fibers. The yarn 20 a of the first example comprises between about fifteen and thirty-five percent by weight of the first fibers 24 and between about sixty-five and eighty-five percent by weight of the second fibers 28 . More specifically, the second fibers 28 comprise between about forty and sixty percent by weight of LCP and between about forty and sixty percent by weight of Aramid.
Given the foregoing, it should be clear to one of ordinary skill in the art that the present invention may be embodied in other forms that fall within the scope of the present invention.
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A rope and method of making the same. The rope comprises a plurality of yarns. At least one of the yarns comprises first and second sets of fibers. The first fibers are formed of a first material, and the second set of second fibers at least partly surrounds the first fibers. The second fibers are formed of a second material. The first material defines a set of operating characteristics adapted to bear tension loads on the rope. The second material defines a set of operating characteristics adapted to affect at least one surface characteristic of the rope.
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FIELD OF THE INVENTION
The present invention relates to the field of inkjet printers and discloses an inkjet printing system using printheads manufactured with micro-electromechanical systems (MEMS) techniques.
CO-PENDING APPLICATIONS
The following applications have been filed by the Applicant simultaneously with the present application:
11/246676
11/246677
11/246678
11/246679
11/246680
11/246681
11/246714
11/246713
11/246689
11/246671
11/246670
11/246669
11/246704
11/246710
11/246688
11/246716
11/246715
11/246707
11/246706
11/246705
11/246708
11/246693
11/246692
11/246696
11/246695
11/246694
11/246687
11/246718
11/246685
11/246686
11/246703
11/246691
11/246711
11/246690
11/246712
11/246717
11/246709
11/246700
11/246701
11/246702
11/246668
11/246697
11/246698
11/246699
11/246675
11/246674
11/246667
11/246672
11/246673
11/246683
11/246682
The disclosures of these co-pending applications are incorporated herein by reference.
CROSS REFERENCES TO RELATED APPLICATIONS
Various methods, systems and apparatus relating to the present invention are disclosed in the following US Patents/Patent Applications filed by the applicant or assignee of the present invention:
6750901
6476863
6788336
09/517539
6566858
6331946
6246970
6442525
09/517384
09/505951
6374354
09/517608
6816968
6757832
6334190
6745331
09/517541
10/203559
7197642
7093139
10/636263
10/636283
10/866608
7210038
10/902833
10/940653
10/942858
11/003786
11/003616
11/003418
11/003334
11/003600
11/003404
11/003419
11/003700
11/003601
11/003618
11/003615
11/003337
11/003698
11/003420
6984017
11/003699
11/071473
11/003643
11/003701
11/003683
11/003614
11/003702
11/003684
11/003619
11/003617
6623101
6406129
6505916
6457809
6550895
6457812
7152962
6428133
7204941
10/815624
10/815628
10/913375
10/913373
10/913374
10/913372
7138391
7153956
10/913380
10/913379
10/913376
7122076
7148345
11/172816
11/172815
11/172814
10/407212
10/407207
10/683064
10/683041
6746105
7156508
7159972
7083271
7165834
7080894
7201469
7090336
7156489
10/760233
10/760246
7083257
10/760243
10/760201
7219980
10/760253
10/760255
10/760209
7118192
10/760194
10/760238
7077505
7198354
7077504
10/760189
7198355
10/760232
10/760231
7152959
7213906
7178901
7222938
7108353
7104629
10/728804
7128400
7108355
6991322
10/728790
7118197
10/728970
10/728784
10/728783
7077493
6962402
10/728803
7147308
10/728779
7118198
7168790
7172270
10/773199
6830318
7195342
7175261
10/773183
7108356
7118202
10/773186
7134744
10/773185
7134743
7182439
7210768
10/773187
7134745
7156484
7118201
7111926
10/773184
7018021
11/060751
11/060805
11/188017
11/097308
11/097309
11/097335
11/097299
11/097310
11/097213
11/210687
11/097212
7147306
09/575197
7079712
09/575123
6825945
09/575165
6813039
6987506
7038797
6980318
6816274
7102771
09/575186
6681045
6728000
7173722
7088459
09/575181
7068382
7062651
6789194
6789191
6644642
6502614
6622999
6669385
6549935
6987573
6727996
6591884
6439706
6760119
09/575198
6290349
6428155
6785016
6870966
6822639
6737591
7055739
09/575129
6830196
6832717
6957768
09/575172
7170499
7106888
7123239
10/727181
10/727162
10/727163
10/727245
7121639
7165824
7152942
10/727157
7181572
7096137
10/727257
10/727238
7188282
10/727159
10/727180
10/727179
10/727192
10/727274
10/727164
10/727161
10/727198
10/727158
10/754536
10/754938
10/727227
10/727160
10/934720
7171323
10/296522
6795215
7070098
7154638
6805419
6859289
6977751
6398332
6394573
6622923
6747760
6921144
10/884881
7092112
7192106
11/039866
7173739
6986560
7008033
11/148237
7195328
7182422
10/854521
10/854522
10/854488
10/854487
10/854503
10/854504
10/854509
7188928
7093989
10/854497
10/854495
10/854498
10/854511
10/854512
10/854525
10/854526
10/854516
10/854508
10/854507
10/854515
10/854506
10/854505
10/854493
10/854494
10/854489
10/854490
10/854492
10/854491
10/854528
10/854523
10/854527
10/854524
10/854520
10/854514
10/854519
10/854513
10/854499
10/854501
10/854500
10/854502
10/854518
10/854517
10/934628
7163345
10/760254
10/760210
10/760202
7201468
10/760198
10/760249
10/760263
10/760196
10/760247
7156511
10/760264
10/760244
7097291
10/260222
10/760248
7083273
10/760192
10/760203
10/760204
10/760205
10/760206
10/760267
10/760270
7198352
10/760271
10/760275
7201470
7121655
10/760184
10/760195
10/760186
10/760261
7083272
11/014764
11/014763
11/014748
11/014747
11/014761
11/014760
11/014757
11/014714
11/014713
11/014762
11/014724
11/014723
11/014756
11/014736
11/014759
11/014758
11/014725
11/014739
11/014738
11/014737
11/014726
11/014745
11/014712
11/014715
11/014751
11/014735
11/014734
11/014719
11/014750
11/014749
11/014746
11/014769
11/014729
11/014743
11/014733
11/014754
11/014755
11/014765
11/014766
11/014740
11/014720
11/014753
11/014752
11/014744
11/014741
11/014768
11/014767
11/014718
11/014717
11/014716
11/014732
11/014742
11/097268
11/097185
11/097184
The disclosures of these applications and patents are incorporated herein by reference.
BACKGROUND OF THE INVENTION
The present invention involves the ejection of ink drops by way of forming gas or vapor bubbles in a bubble forming liquid. This principle is generally described in U.S. Pat. No. 3,747,120 (Stemme). Each pixel in the printed image is derived ink drops ejected from one or more ink nozzles. In recent years, inkjet printing has become increasing popular primarily due to its inexpensive and versatile nature. Many different aspects and techniques for inkjet printing are described in detail in the above cross referenced documents.
Completely immersing the heater element in ink dramatically improves the printhead efficiency. Much less heat dissipates into the underlying wafer substrate so more of the input energy is used to generate the bubble that ejects the ink.
A convenient way of suspending the heater element is to deposit it on sacrificial photoresist that is subsequently removed by a release etch. The sacrificial material (SAC) is deposited into a pit or trench etched into the substrate adjacent the electrodes. However, it is difficult to precisely match the mask with the sides of the pit. Usually, when the masked photoresist is exposed, gaps form between the sides of the pit and the SAC. When the heater material layer is deposited, it fills these gaps to form ‘stringers’ (as they are known). The stringers remain in the pit after the metal etch (that shapes the heater element) and the release etch (to finally remove the SAC). The stringers can short circuit the heater so that it fails to generate a bubble.
By making the mask bigger than the trench, the SAC will be deposited over the side walls so that no gaps form. Unfortunately, this produces a raised lip around top of the trench. When the heater material layer is deposited, it is thinner on the vertical or inclined surfaces of the lip. After the metal etch and release etch, these thin lip formations remain and cause ‘hotspots’ because the localized thinning increases resistance. These hotspots affect the operation of the heater and typically reduce heater life.
SUMMARY OF THE INVENTION
Accordingly, the present invention provides a method of fabricating a suspended beam in a MEMS process, said method comprising the steps of:
(a) etching a pit in a substrate, said pit having a base and sidewalls; (b) depositing sacrificial material on a surface of said substrate so as to fill said pit; (c) removing said sacrificial material from a perimeter region within said pit and from said substrate surface surrounding said pit; (d) reflowing remaining sacrificial material within said pit such that said remaining sacrificial material contacts said sidewalls; (e) depositing beam material on said substrate surface and on said reflowed sacrificial material; and (f) removing said reflowed sacrificial material to form said suspended beam.
Preferably said suspended beam is substantially planar. In a further preferred form, all parts of said suspended beam have substantially the same thickness.
Optionally, said suspended beam is an actuator for an inkjet nozzle.
In a first aspect the present invention provides a method of fabricating a suspended beam in a MEMS process, said method comprising the steps of:
(a) etching a pit in a substrate, said pit having a base and sidewalls; (b) depositing sacrificial material on a surface of said substrate so as to fill said pit; (c) removing said sacrificial material from a perimeter region within said pit and from said substrate surface surrounding said pit; (d) reflowing remaining sacrificial material within said pit such that said remaining sacrificial material contacts said sidewalls; (e) depositing beam material on said substrate surface and on said reflowed sacrificial material; and (f) removing said reflowed sacrificial material to form said suspended beam.
Optionally, said suspended beam is substantially planar.
Optionally, all parts of said suspended beam have substantially the same thickness.
Optionally, said suspended beam is an actuator for an inkjet nozzle.
Optionally, said actuator is a heater element.
Optionally, said heater element is suspended between a pair of electrodes.
Optionally, said substrate is a silicon wafer.
Optionally, said silicon wafer comprises at least one surface oxide layer.
Optionally, said sacrificial material is photoresist.
Optionally, said photoresist is removed by exposure through a mask followed by development.
Optionally, said perimeter region comprises an area adjacent at least two of said sidewalls.
Optionally, said perimeter region comprises an area adjacent all of said sidewalls.
Optionally, removal of said sacrificial material from said perimeter region results in a space of less than 1 micron between said remaining sacrificial material and at least two of said sidewalls.
Optionally, removal of said sacrificial material from said perimeter region results in a space of less than 1 micron between said remaining sacrificial material and all of said sidewalls.
Optionally, said reflowing is performed by heating said sacrificial material.
Optionally, said sacrificial material is treated to prevent further reflow prior to deposition of beam material.
Optionally, said treatment comprises UV curing.
Optionally, said beam material is etched into a predetermined configuration after deposition.
Optionally, further MEMS process steps are performed after deposition of said beam material and prior to said removal of said reflowed sacrificial material.
Optionally, said further MEMS process steps comprise forming an inkjet nozzle containing said suspended beam.
In a second aspect the present invention provides a method of fabricating a plurality of inkjet nozzles on a substrate, each nozzle comprising a nozzle chamber having a roof spaced apart from said substrate and sidewalls extending from said roof to said substrate, one of said sidewalls having a chamber entrance for receiving ink from an ink conduit extending along a row of nozzles, said ink conduit receiving ink from a plurality of ink inlets defined in said substrate, said method comprising the steps of:
(a) providing a substrate having a plurality of trenches corresponding to said ink inlets; (b) depositing sacrificial material on said substrate so as fill said trenches and form a scaffold on said substrate; (c) defining openings in said sacrificial material, said openings being positioned to form said chamber sidewalls and said ink conduit when filled with roof material; (d) depositing roof material over said sacrificial material to form simultaneously said nozzle chambers and said ink conduit; (e) etching nozzle apertures through said roof material, each nozzle chamber having at least one nozzle aperture; and (f) removing said sacrificial material.
Optionally, each nozzle chamber contains an actuator for ejecting ink through said nozzle aperture.
Optionally, said actuator is formed prior to fabrication of said nozzle chamber.
Optionally, said substrate is a silicon wafer.
Optionally, said silicon wafer comprises at least one surface oxide layer.
Optionally, said sacrificial material is photoresist.
Optionally, said openings are defined by exposing said photoresist through a mask followed by development.
Optionally, said photoresist is UV cured prior to deposition of said roof material, thereby preventing reflow of said photoresist during deposition.
Optionally, said photoresist is removed by plasma ashing.
In a further aspect there is provided a method further comprising the step of etching ink supply channels from an opposite backside of said substrate, said ink supply channels being in fluid communication with said ink inlets.
Optionally, each ink inlet has at least one priming feature extending from a respective rim thereof, and said method further comprises defining at least one opening corresponding to said at least one priming feature in said photoresist.
Optionally, said at least one priming feature comprises a column of roof material extending from said rim.
Optionally, each ink inlet has a plurality of priming features positioned about a respective rim thereof.
Optionally, said plurality of priming features together form a columnar cage extending from said rim.
Optionally, said chamber entrance includes at least one filter structure, and said method further comprises defining at least one opening corresponding to said at least one priming feature in said photoresist.
Optionally, said at least one filter structure comprises a column of roof material extending from said substrate to said roof.
Optionally, each chamber entrance includes a plurality of filter structures arranged across said entrance.
Optionally, each chamber entrance includes a plurality of rows of filter structures arranged across said entrance.
Optionally, said rows of filter structures are staggered.
In a third aspect there is provided a method of fabricating a plurality of inkjet nozzles on a substrate, each nozzle comprising a nozzle chamber having a roof spaced apart from said substrate and sidewalls extending from said roof to said substrate, said chamber having an entrance for receiving ink from at least one ink inlet defined in said substrate, said at least one ink inlet having at least one priming feature extending from a respective rim thereof, said method comprising the steps of:
(a) providing a substrate having a plurality of trenches corresponding to said ink inlets; (b) depositing sacrificial material on said substrate so as fill said trenches and form a scaffold on said substrate; (c) defining openings in said sacrificial material, said openings being positioned to form said chamber sidewalls and said at least one priming feature when filled with roof material; (d) depositing roof material over said sacrificial material to form simultaneously said nozzle chambers and said at least one priming feature; (e) etching nozzle apertures through said roof material, each nozzle chamber having at least one nozzle aperture; and (f) removing said sacrificial material.
Optionally, said at least one priming feature comprises a column of roof material extending from said rim.
Optionally, each ink inlet has a plurality of priming features positioned about a respective rim thereof.
Optionally, said plurality of priming features together form a columnar cage extending from said rim.
Optionally, each nozzle chamber contains an actuator for ejecting ink through said nozzle aperture.
Optionally, said actuator is formed prior to fabrication of said nozzle chamber.
Optionally, said substrate is a silicon wafer.
Optionally, said silicon wafer comprises at least one surface oxide layer.
Optionally, said sacrificial material is photoresist.
Optionally, said openings are defined by exposing said photoresist through a mask followed by development.
Optionally, said photoresist is UV cured prior to deposition of said roof material, thereby preventing reflow of said photoresist during deposition.
Optionally, said photoresist is removed by plasma ashing.
In a further aspect there is provided a method further comprising the step of etching ink supply channels from an opposite backside of said substrate, said ink supply channels being in fluid communication with said ink inlets.
Optionally, said chamber entrance is defined in one of said sidewalls of said nozzle chamber.
Optionally, said chamber entrance receives ink from an ink conduit extending along a row of nozzles, whereby step (c) further comprises defining further openings in said sacrificial material, said further openings being positioned to form said ink conduit when filled with roof material.
Optionally, said ink conduit receives ink from said at least one ink inlet.
In a fourth aspect the present invention provides a method of fabricating a plurality of inkjet nozzles on a substrate, each nozzle comprising a nozzle chamber having a roof spaced apart from said substrate and sidewalls extending from said roof to said substrate, one of said sidewalls having a chamber entrance for receiving ink from at least one ink inlet defined in said substrate, said chamber entrance including at least one filter structure, said method comprising the steps of:
(a) providing a substrate having a plurality of trenches corresponding to said ink inlets; (b) depositing sacrificial material on said substrate so as fill said trenches and form a scaffold on said substrate; (c) defining openings in said sacrificial material, said openings being positioned to form said chamber sidewalls and said at least one filter structure when filled with roof material; (d) depositing roof material over said sacrificial material to form simultaneously said nozzle chambers and said at least one filter structure; (e) etching nozzle apertures through said roof material, each nozzle chamber having at least one nozzle aperture; and (f) removing said sacrificial material.
Optionally, said filter structure comprises a column of roof material extending from said substrate to said roof.
Optionally, each chamber entrance includes a plurality of filter structures arranged across said entrance.
Optionally, each chamber entrance includes a plurality of rows of filter structures arranged across said entrance.
Optionally, said rows of filter structures are staggered.
Optionally, each nozzle chamber contains an actuator for ejecting ink through said nozzle aperture.
Optionally, said actuator is formed prior to fabrication of said nozzle chamber.
Optionally, said substrate is a silicon wafer.
Optionally, said silicon wafer comprises at least one surface oxide layer.
Optionally, said sacrificial material is photoresist.
Optionally, said openings are defined by exposing said photoresist through a mask followed by development.
Optionally, said photoresist is UV cured prior to deposition of said roof material, thereby preventing reflow of said photoresist during deposition.
Optionally, said photoresist is removed by plasma ashing.
In a further aspect there is provided a method further comprising the step of etching ink supply channels from an opposite backside of said substrate, said ink supply channels being in fluid communication with said ink inlets.
Optionally, said chamber entrance receives ink from an ink conduit extending along a row of nozzles, whereby step (c) further comprises defining further openings in said sacrificial material, said further openings being positioned to form said ink conduit when filled with roof material.
Optionally, said ink conduit receives ink from said at least one ink inlet.
In a fifth aspect the present invention provides a method of forming a low-stiction nozzle plate for an inkjet printhead, said nozzle plate having a plurality of nozzle apertures defined therein, each nozzle aperture having a respective nozzle rim, said method comprising the steps of:
(a) providing a partially-fabricated printhead comprising a plurality of inkjet nozzle assemblies sealed with roof material; (b) etching partially into said roof material to define simultaneously said nozzle rims and a plurality of stiction-reducing formations; and (c) etching through said roof material to define said nozzle apertures, thereby forming said nozzle plate.
Optionally, each nozzle rim comprises at least one projection around a perimeter of each nozzle aperture.
Optionally, each nozzle rim comprises a plurality of coaxial projections around a perimeter of each nozzle aperture.
Optionally, said at least one rim projection projects at least 1 micron from said nozzle plate.
Optionally, each stiction-reducing formation comprises a columnar projection on said nozzle plate.
Optionally, each columnar projection projects at least 1 micron from said nozzle plate.
Optionally, each columnar projection is spaced apart from an adjacent columnar projection by less than 2 microns.
Optionally, each stiction-reducing formation comprises an elongate wall projection on said nozzle plate.
Optionally, each wall projection projects at least 1 micron from said nozzle plate.
Optionally, said wall projections are positioned for minimizing color-mixing of inks on said nozzle plate.
Optionally, said wall projections extend along said nozzle plate parallel with rows of nozzles, each nozzle in a row ejecting the same colored ink.
Optionally, the positions of said nozzle rims and said stiction-reducing formations are defined by photolithographic masking.
Optionally, at least half of the surface area of said nozzle plate is tiled with stiction-reducing formations.
Optionally, said inkjet nozzle assemblies are formed on a silicon substrate and said nozzle plate is spaced apart from said substrate.
Optionally, said nozzle plate is comprised of silicon nitride, silicon oxide, silicon oxynitride or aluminium nitride.
Optionally, said nozzle assemblies are sealed by CVD or PECVD deposition of said roof material.
Optionally, said roof material is deposited onto a sacrificial scaffold.
Optionally, each inkjet nozzle assembly has at least one nozzle aperture associated therewith for ejection of ink.
Optionally, said nozzle plate is subsequently treated with a hydrophobizing material.
The printhead according to the invention comprises a plurality of nozzles, as well as a chamber and one or more heater elements corresponding to each nozzle. The smallest repeating units of the printhead will have an ink supply inlet feeding ink to one or more chambers. The entire nozzle array is formed by repeating these individual units. Such an individual unit is referred to herein as a “unit cell”.
Also, the term “ink” is used to signify any ejectable liquid, and is not limited to conventional inks containing colored dyes. Examples of non-colored inks include fixatives, infra-red absorber inks, functionalized chemicals, adhesives, biological fluids, medicaments, water and other solvents, and so on. The ink or ejectable liquid also need not necessarily be a strictly a liquid, and may contain a suspension of solid particles.
BRIEF DESCRIPTION OF THE DRAWINGS
Preferred embodiments of the present invention will now be described by way of example only with reference to the accompanying drawings, in which:
FIG. 1 shows a partially fabricated unit cell of the MEMS nozzle array on a printhead according to the present invention, the unit cell being section along A-A of FIG. 3 ;
FIG. 2 shows a perspective of the partially fabricated unit cell of FIG. 1 ;
FIG. 3 shows the mark associated with the etch of the heater element trench;
FIG. 4 is a sectioned view of the unit cell after the etch of the trench;
FIG. 5 is a perspective view of the unit cell shown in FIG. 4 ;
FIG. 6 is the mask associated with the deposition of sacrificial photoresist shown in FIG. 7 ;
FIG. 7 shows the unit cell after the deposition of sacrificial photoresist trench, with partial enlargements of the gaps between the edges of the sacrificial material and the side walls of the trench;
FIG. 8 is a perspective of the unit cell shown in FIG. 7 ;
FIG. 9 shows the unit cell following the reflow of the sacrificial photoresist to close the gaps along the side walls of the trench;
FIG. 10 is a perspective of the unit cell shown in FIG. 9 ;
FIG. 11 is a section view showing the deposition of the heater material layer;
FIG. 12 is a perspective of the unit cell shown in FIG. 11 ;
FIG. 13 is the mask associated with the metal etch of the heater material shown in FIG. 14 ;
FIG. 14 is a section view showing the metal etch to shape the heater actuators;
FIG. 15 is a perspective of the unit cell shown in FIG. 14 ;
FIG. 16 is the mask associated with the etch shown in FIG. 17 ;
FIG. 17 shows the deposition of the photoresist layer and subsequent etch of the ink inlet to the passivation layer on top of the CMOS drive layers;
FIG. 18 is a perspective of the unit cell shown in FIG. 17 ;
FIG. 19 shows the oxide etch through the passivation and CMOS layers to the underlying silicon wafer;
FIG. 20 is a perspective of the unit cell shown in FIG. 19 ;
FIG. 21 is the deep anisotropic etch of the ink inlet into the silicon wafer;
FIG. 22 is a perspective of the unit cell shown in FIG. 21 ;
FIG. 23 is the mask associated with the photoresist etch shown in FIG. 24 ;
FIG. 24 shows the photoresist etch to form openings for the chamber roof and side walls;
FIG. 25 is a perspective of the unit cell shown in FIG. 24 ;
FIG. 26 shows the deposition of the side wall and risk material;
FIG. 27 is a perspective of the unit cell shown in FIG. 26 ;
FIG. 28 is the mask associated with the nozzle rim etch shown in FIG. 29 ;
FIG. 29 shows the etch of the roof layer to form the nozzle aperture rim;
FIG. 30 is a perspective of the unit cell shown in FIG. 29 ;
FIG. 31 is the mask associated with the nozzle aperture etch shown in FIG. 32 ;
FIG. 32 shows the etch of the roof material to form the elliptical nozzle apertures;
FIG. 33 is a perspective of the unit cell shown in FIG. 32 ;
FIG. 34 shows the oxygen plasma release etch of the first and second sacrificial layers;
FIG. 35 is a perspective of the unit cell shown in FIG. 34 ;
FIG. 36 shows the unit cell after the release etch, as well as the opposing side of the wafer;
FIG. 37 is a perspective of the unit cell shown in FIG. 36 ;
FIG. 38 is the mask associated with the reverse etch shown in FIG. 39 ;
FIG. 39 shows the reverse etch of the ink supply channel into the wafer;
FIG. 40 is a perspective of unit cell shown in FIG. 39 ;
FIG. 41 shows the thinning of the wafer by backside etching;
FIG. 42 is a perspective of the unit cell shown in FIG. 41 ;
FIG. 43 is a partial perspective of the array of nozzles on the printhead according to the present invention;
FIG. 44 shows the plan view of a unit cell;
FIG. 45 shows a perspective of the unit cell shown in FIG. 44 ;
FIG. 46 is schematic plan view of two unit cells with the roof layer removed but certain roof layer features shown in outline only;
FIG. 47 is schematic plan view of two unit cells with the roof layer removed but the nozzle openings shown in outline only;
FIG. 48 is a partial schematic plan view of unit cells with ink inlet apertures in the sidewall of the chambers;
FIG. 49 is schematic plan view of a unit cells with the roof layer removed but the nozzle openings shown in outline only;
FIG. 50 is a partial plan view of the nozzle plate with stiction reducing formations and a particle of paper dust;
FIG. 51 is a partial plan view of the nozzle plate with residual ink gutters;
FIG. 52 is a partial section view showing the deposition of SAC 1 photoresist in accordance with prior art techniques used to avoid stringers;
FIG. 53 is a partial section view showing the depositon of a layer of heater material onto the SAC1 photoresist scaffold deposited in FIG. 52 ; and,
FIG. 54 is a partial schematic plan view of a unit cell with multiple nozzles and actuators in each of the chambers.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
In the description than follows, corresponding reference numerals relate to corresponding parts. For convenience, the features indicated by each reference numeral are listed below.
MNN MPN SERIES PARTS LIST
1 . Nozzle Unit Cell
2 . Silicon Wafer
3 . Topmost Aluminium Metal Layer in the CMOS metal layers
4 . Passivation Layer
5 . CVD Oxide Layer
6 . Ink Inlet Opening in Topmost Aluminium Metal Layer 3 .
7 . Pit Opening in Topmost Aluminium Metal Layer 3 .
8 . Pit
9 . Electrodes
10 . SAC1 Photoresist Layer
11 . Heater Material (TiAlN)
12 . Thermal Actuator
13 . Photoresist Layer
14 . Ink Inlet Opening Etched Through Photo Resist Layer
15 . Ink Inlet Passage
16 . SAC2 Photoresist Layer
17 . Chamber Side Wall Openings
18 . Front Channel Priming Feature
19 . Barrier Formation at Ink Inlet
20 . Chamber Roof Layer
21 . Roof
22 . Sidewalls
23 . Ink Conduit
24 . Nozzle Chambers
25 . Elliptical Nozzle Rim
25 ( a ) Inner Lip 25 ( b ) Outer Lip
26 . Nozzle Aperture
27 . Ink Supply Channel
28 . Contacts
29 . Heater Element.
30 . Bubble cage
32 . bubble retention structure
34 . ink permeable structure
36 . bleed hole
38 . ink chamber
40 . dual row filter
42 . paper dust
44 . ink gutters
46 . gap between SAC1 and trench sidewall
48 . trench sidewall
50 . raised lip of SAC1 around edge of trench
52 . thinner inclined section of heater material
54 . cold spot between series connected heater elements
56 . nozzle plate
58 . columnar projections
60 . sidewall ink opening
62 . ink refill opening
MEMS Manufacturing Process
The MEMS manufacturing process builds up nozzle structures on a silicon wafer after the completion of CMOS processing. FIG. 2 is a cutaway perspective view of a nozzle unit cell 100 after the completion of CMOS processing and before MEMS processing.
During CMOS processing of the wafer, four metal layers are deposited onto a silicon wafer 2 , with the metal layers being interspersed between interlayer dielectric (ILD) layers. The four metal layers are referred to as M1, M2, M3 and M4 layers and are built up sequentially on the wafer during CMOS processing. These CMOS layers provide all the drive circuitry and logic for operating the printhead.
In the completed printhead, each heater element actuator is connected to the CMOS via a pair of electrodes defined in the outermost M4 layer. Hence, the M4 CMOS layer is the foundation for subsequent MEMS processing of the wafer. The M4 layer also defines bonding pads along a longitudinal edge of each printhead integrated circuit. These bonding pads (not shown) allow the CMOS to be connected to a microprocessor via wire bonds extending from the bonding pads.
FIGS. 1 and 2 show the aluminium M4 layer 3 having a passivation layer 4 deposited thereon. (Only MEMS features of the M4 layer are shown in these Figures; the main CMOS features of the M4 layer are positioned outside the nozzle unit cell). The M4 layer 3 has a thickness of 1 micron and is itself deposited on a 2 micron layer of CVD oxide 5 . As shown in FIGS. 1 and 2 , the M4 layer 3 has an ink inlet opening 6 and pit openings 7 . These openings define the positions of the ink inlet and pits formed subsequently in the MEMS process.
Before MEMS processing of the unit cell 1 begins, bonding pads along a longitudinal edge of each printhead integrated circuit are defined by etching through the passivation layer 4 . This etch reveals the M4 layer 3 at the bonding pad positions. The nozzle unit cell 1 is completely masked with photoresist for this step and, hence, is unaffected by the etch.
Turning to FIGS. 3 to 5 , the first stage of MEMS processing etches a pit 8 through the passivation layer. 4 and the CVD oxide layer 5 . This etch is defined using a layer of photoresist (not shown) exposed by the dark tone pit mask shown in FIG. 3 . The pit 8 has a depth of 2 microns, as measured from the top of the M4 layer 3 . At the same time as etching the pit 8 , electrodes 9 are defined on either side of the pit by partially revealing the M4 layer 3 through the passivation layer 4 . In the completed nozzle, a heater element is suspended across the pit 8 between the electrodes 9 .
In the next step ( FIGS. 6 to 8 ), the pit 8 is filled with a first sacrificial layer (“SAC1”) of photoresist 10 . A 2 micron layer of high viscosity photoresist is first spun onto the wafer and then exposed using the dark tone mask shown in FIG. 6 . The SAC1 photoresist 10 forms a scaffold for subsequent deposition of the heater material across the electrodes 9 on either side of the pit 8 . Consequently, it is important the SAC1 photoresist 10 has a planar upper surface that is flush with the upper surface of the electrodes 9 . At the same time, the SAC1 photoresist must completely fill the pit 8 to avoid ‘stringers’ of conductive heater material extending across the pit and shorting out the electrodes 9 .
Typically, when filling trenches with photoresist, it is necessary to expose the photoresist outside the perimeter of the trench in order to ensure that photoresist fills against the walls of the trench and, therefore, avoid ‘stringers’ in subsequent deposition steps. However, this technique results in a raised (or spiked) rim of photoresist around the perimeter of the trench. This is undesirable because in a subsequent deposition step, material is deposited unevenly onto the raised rim—vertical or angled surfaces on the rim will receive less deposited material than the horizontal planar surface of the photoresist filling the trench. The result is ‘resistance hotspots’ in regions where material is thinly deposited.
As shown in FIG. 7 , the present process deliberately exposes the SAC1 photoresist 10 inside the perimeter walls of the pit 8 (e.g. within 0.5 microns) using the mask shown in FIG. 6 . This ensures a planar upper surface of the SAC1 photoresist 10 and avoids any spiked regions of photoresist around the perimeter rim of the pit 8 .
After exposure of the SAC1 photoresist 10 , the photoresist is reflowed by heating. Reflowing the photoresist allows it to flow to the walls of the pit 8 , filling it exactly. FIGS. 9 and 10 show the SAC1 photoresist 10 after reflow. The photoresist has a planar upper surface and meets flush with the upper surface of the M4 layer 3 , which forms the electrodes 9 . Following reflow, the SAC1 photoresist 10 is U.V. cured and/or hardbaked to avoid any reflow during the subsequent deposition step of heater material.
FIGS. 11 and 12 show the unit cell after deposition of the 0.5 microns of heater material 11 onto the SAC1 photoresist 10 . Due to the reflow process described above, the heater material 11 is deposited evenly and in a planar layer over the electrodes 9 and the SAC1 photoresist 10 . The heater material may be comprised of any suitable conductive material, such as TiAl, TiN, TAlN, TiAlSiN etc. A typical heater material deposition process may involve sequential deposition of a 100 Å seed layer of TiAl, a 2500 Å layer of TiAlN, a further 100 Å seed layer of TiAl and finally a further 2500 Å layer of TiAlN.
Referring to FIGS. 13 to 15 , in the next step, the layer of heater material 11 is etched to define the thermal actuator 12 . Each actuator 12 has contacts 28 that establish an electrical connection to respective electrodes 9 on either side of the SAC1 photoresist 10 . A heater element 29 spans between its corresponding contacts 28 .
This etch is defined by a layer of photoresist (not shown) exposed using the dark tone mask shown in FIG. 13 . As shown in FIG. 15 , the heater element 12 is a linear beam spanning between the pair of electrodes 9 . However, the heater element 12 may alternatively adopt other configurations, such as those described in Applicant's U.S. Pat. No. 6,755,509, the content of which is herein incorporated by reference. For example, heater element 29 configurations having a central void may be advantageous for minimizing the deleterious effects of cavitation forces on the heater material when a bubble collapses during ink ejection. Other forms of cavitation protection may be adopted such as ‘bubble venting’ and the use of self passivating materials. These cavitation management techniques are discussed in detail in U.S. patent application (our docket MTC001US).
In the next sequence of steps, an ink inlet for the nozzle is etched through the passivation layer 4 , the oxide layer 5 and the silicon wafer 2 . During CMOS processing, each of the metal layers had an ink inlet opening (see, for example, opening 6 in the M 4 layer 3 in FIG. 1 ) etched therethrough in preparation for this ink inlet etch. These metal layers, together with the interspersed ILD layers, form a seal ring for the ink inlet, preventing ink from seeping into the CMOS layers.
Referring to FIGS. 16 to 18 , a relatively thick layer of photoresist 13 is spun onto the wafer and exposed using the dark tone mask shown in FIG. 16 . The thickness of photoresist 13 required will depend on the selectivity of the deep reactive ion etch (DRIE) used to etch the ink inlet. With an ink inlet opening 14 defined in the photoresist 13 , the wafer is ready for the subsequent etch steps.
In the first etch step ( FIGS. 19 and 20 ), the dielectric layers (passivation layer 4 and oxide layer 5 ) are etched through to the silicon wafer below. Any standard oxide etch (e.g. O 2 /C 4 F 8 plasma) may be used.
In the second etch step ( FIGS. 21 and 22 ), an ink inlet 15 is etched through the silicon wafer 2 to a depth of 25 microns, using the same photoresist mask 13 . Any standard anisotropic DRIE, such as the Bosch etch (see U.S. Pat. Nos. 6,501,893 and 6,284,148) may be used for this etch. Following etching of the ink inlet 15 , the photoresist layer 13 is removed by plasma ashing.
In the next step, the ink inlet 15 is plugged with photoresist and a second sacrificial layer (“SAC2”) of photoresist 16 is built up on top of the SAC1 photoresist 10 and passivation layer 4 . The SAC2 photoresist 16 will serve as a scaffold for subsequent deposition of roof material, which forms a roof and sidewalls for each nozzle chamber. Referring to FIGS. 23 to 25 , a ˜6 micron layer of high viscosity photoresist is spun onto the wafer and exposed using the dark tone mask shown in FIG. 23 .
As shown in FIGS. 23 and 25 , the mask exposes sidewall openings 17 in the SAC2 photoresist 16 corresponding to the positions of chamber sidewalls and sidewalls for an ink conduit. In addition, openings 18 and 19 are exposed adjacent the plugged inlet 15 and nozzle chamber entrance respectively. These openings 18 and 19 will be filled with roof material in the subsequent roof deposition step and provide unique advantages. in the present nozzle design. Specifically, the openings 18 filled with roof material act as priming features, which assist in drawing ink from the inlet 15 into each nozzle chamber. This is described in greater detail below. The openings 19 filled with roof material act as filter structures and fluidic cross talk barriers. These help prevent air bubbles from entering the nozzle chambers and diffuses pressure pulses generated by the thermal actuator 12 .
Referring to FIGS. 26 and 27 , the next stage deposits 3 microns of roof material 20 onto the SAC2 photoresist 16 by PECVD. The roof material 20 fills the openings 17 , 18 and 19 in the SAC2 photoresist 16 to form nozzle chambers 24 having a roof 21 and sidewalls 22 . An ink conduit 23 for supplying ink into each nozzle chamber is also formed during deposition of the roof material 20 . In addition, any priming features and filter structures (not shown in FIGS. 26 and 27 ) are formed at the same time. The roofs 21 , each corresponding to a respective nozzle chamber 24 , span across adjacent nozzle chambers in a row to form a continuous nozzle plate. The roof material 20 may be comprised of any suitable material, such as silicon nitride, silicon oxide, silicon oxynitride, aluminium nitride etc.
Referring to FIGS. 28 to 30 , the next stage defines an elliptical nozzle rim 25 in the roof 21 by etching away 2 microns of roof material 20 . This etch is defined using a layer of photoresist (not shown) exposed by the dark tone rim mask shown in FIG. 28 . The elliptical rim 25 comprises two coaxial rim lips 25 a and 25 b , positioned over their respective thermal actuator 12 .
Referring to FIGS. 31 to 33 , the next stage defines an elliptical nozzle aperture 26 in the roof 21 by etching all the way through the remaining roof material 20 , which is bounded by the rim 25 . This etch is defined using a layer of photoresist (not shown) exposed by the dark tone roof mask shown in FIG. 31 . The elliptical nozzle aperture 26 is positioned over the thermal actuator 12 , as shown in FIG. 33 .
With all the MEMS nozzle features now fully formed, the next stage removes the SAC1 and SAC2 photoresist layers 10 and 16 by O 2 plasma ashing ( FIGS. 34 to 35 ). After ashing, the thermal actuator 12 is suspended in a single plane over the pit 8 . The coplanar deposition of the contacts 28 and the heater element 29 provides an efficient electrical connection with the electrodes 9 .
FIGS. 36 and 37 show the entire thickness (150 microns) of the silicon wafer 2 after ashing the SAC1 and SAC2 photoresist layers 10 and 16 .
Referring to FIGS. 38 to 40 , once frontside MEMS processing of the wafer is completed, ink supply channels 27 are etched from the backside of the wafer to meet with the ink inlets 15 using a standard anisotropic DRIE. This backside etch is defined using a layer of photoresist (not shown) exposed by the dark tone mask shown in FIG. 38 . The ink supply channel 27 makes a fluidic connection between the backside of the wafer and the ink inlets 15 .
Finally, and referring to FIGS. 41 and 42 , the wafer is thinned 135 microns by backside etching. FIG. 43 shows three adjacent rows of nozzles in a cutaway perspective view of a completed printhead integrated circuit. Each row of nozzles has a respective ink supply channel 27 extending along its length and supplying ink to a plurality of ink inlets 15 in each row. The ink inlets, in turn, supply ink to the ink conduit 23 for each row, with each nozzle chamber receiving ink from a common ink conduit for that row.
Features and Advantages of Particular Embodiments
Discussed below, under appropriate sub-headings, are certain specific features of embodiments of the invention, and the advantages of these features. The features are to be considered in relation to all of the drawings pertaining to the present invention unless the context specifically excludes certain drawings, and relates to those drawings specifically referred to.
Low Loss Electrodes
As shown in FIGS. 41 and 42 , the heater element 29 is suspended within the chamber. This ensures that the heater element is immersed in ink when the chamber is primed. Completely immersing the heater element in ink dramatically improves the printhead efficiency. Much less heat dissipates into the underlying wafer substrate so more of the input energy is used to generate the bubble that ejects the ink.
To suspend the heater element, the contacts may be used to support the element at its raised position. Essentially, the contacts at either end of the heater element can have vertical or inclined sections to connect the respective electrodes on the CMOS drive to the element at an elevated position. However, heater material deposited on vertical or inclined surfaces is thinner than on horizontal surfaces. To avoid undesirable resistive losses from the thinner sections, the contact portion of the thermal actuator needs to be relatively large. Larger contacts occupy a significant area of the wafer surface and limit the nozzle packing density.
To immerse the heater, the present invention etches a pit or trench 8 between the electrodes 9 to drop the level of the chamber floor. As discussed above, a layer of sacrificial photoresist (SAC) 10 (see FIG. 9 ) is deposited in the trench to provide a scaffold for the heater element. However, depositing SAC 10 in the trench 8 and simply covering it with a layer of heater material, can lead to stringers forming in the gaps 46 between the SAC 10 and the sidewalls 48 of the trench 8 (as previously described in relation to FIG. 7 ). The gaps form because it is difficult to precisely match the mask with the sides of the trench 8 . Usually, when the masked photoresist is exposed, the gaps 46 form between the sides of the pit and the SAC. When the heater material layer is deposited, it fills these gaps to form ‘stringers’ (as they are known). The stringers remain in the trench 8 after the metal etch (that shapes the heater element) and the release etch (to finally remove the SAC). The stringers can short circuit the heater so that it fails to generate a bubble.
Turning now to FIGS. 52 and 53 , the ‘traditional’ technique for avoiding stringers is illustrated. By making the UV mask that exposes the SAC slightly bigger than the trench 8 , the SAC 10 will be deposited over the side walls 48 so that no gaps form. Unfortunately, this produces a raised lip 50 around top of the trench. When the heater material layer 11 is deposited (see FIG. 53 ), it is thinner on the vertical or inclined surfaces 52 of the lip 50 . After the metal etch and release etch, these thin lip formations 52 remain and cause ‘hotspots’ because the localized thinning increases resistance. These hotspots affect the operation of the heater and typically reduce heater life.
As discussed above, the Applicant has found that reflowing the SAC 10 closes the gaps 46 so that the scaffold between the electrodes 9 is completely flat. This allows the entire thermal actuator 12 to be planar. The planar structure of the thermal actuator, with contacts directly deposited onto the CMOS electrodes 9 and suspended heater element 29 , avoids hotspots caused by vertical or inclined surfaces so that the contacts can be much smaller structures without acceptable increases in resistive losses. Low resistive losses preserves the efficient operation of a suspended heater element and the small contact size is convenient for close nozzle packing on the printhead.
Multiple Nozzles for Each Chamber
Referring to FIG. 49 , the unit cell shown has two separate ink chambers 38 , each chamber having heater element 29 extending between respective pairs of contacts 28 . Ink permeable structures 34 are positioned in the ink refill openings so that ink can enter the chambers, but upon actuation, the structures 34 provide enough hydraulic resistance to reduce any reverse flow or fluidic cross talk to an acceptable level.
Ink is fed from the reverse side of the wafer through the ink inlet 15 . Priming features 18 extend into the inlet opening so that an ink meniscus does not pin itself to the peripheral edge of the opening and stop the ink flow. Ink from the inlet 15 fills the lateral ink conduit 23 which supplies both chambers 38 of the unit cell.
Instead of a single nozzle per chamber, each chamber 38 has two nozzles 25 . When the heater element 29 actuates (forms a bubble), two drops of ink are ejected; one from each nozzle 25 . Each individual drop of ink has less volume than the single drop ejected if the chamber had only one nozzle. By ejecting multiple drops from a single chamber simultaneously improves the print quality.
With every nozzle, there is a degree of misdirection in the ejected drop. Depending on the degree of misdirection, this can be detrimental to print quality. By giving the chamber multiple nozzles, each nozzle ejects drops of smaller volume, and having different misdirections. Several small drops misdirected in different directions are less detrimental to print quality than a single relatively large misdirected drop. The Applicant has found that the eye averages the misdirections of each small drop and effectively ‘sees’ a dot from a single drop with a significantly less overall misdirection.
A multi nozzle chamber can also eject drops more efficiently than a single nozzle chamber. The heater element 29 is an elongate suspended beam of TiAlN and the bubble it forms is likewise elongated. The pressure pulse created by an elongate bubble will cause ink to eject through a centrally disposed nozzle. However, some of the energy from the pressure pulse is dissipated in hydraulic losses associated with the mismatch between the geometry of the bubble and that of the nozzle.
Spacing several nozzles 25 along the length of the heater element 29 reduces the geometric discrepancy between the bubble shape and the nozzle configuration through which the ink ejects. This in turn reduces hydraulic resistance to ink ejection and thereby improves printhead efficiency.
Ink Chamber Re-Filled Via Adjacent Ink Chamber
Referring to FIG. 46 , two opposing unit cells are shown. In this embodiment, unit cell has four ink chambers 38 . The chambers are defined by the sidewalls 22 and the ink permeable structures 34 . Each chamber has its own heater element 29 . The heater elements 29 are arranged in pairs that are connected in series. Between each pair is ‘cold spot’ 54 with lower resistance and or greater heat sinking. This ensures that bubbles do not nucleate at the cold spots 54 and thus the cold spots become the common contact between the outer contacts 28 for each heater element pair.
The ink permeable structures 34 allow ink to refill the chambers 38 after drop ejection but baffle the pressure pulse from each heater element 29 to reduce the fluidic cross talk between adjacent chambers. It will be appreciated that this embodiment has many parallels with that shown in FIG. 49 discussed above. However, the present embodiment effectively divides the relatively long chambers of FIG. 49 into two separate chambers. This further aligns the geometry of the bubble formed by the heater element 29 with the shape of the nozzle 25 to reduce hydraulic losses during drop ejection. This is achieved without reducing the nozzle density but it does add some complexity to the fabrication process.
The conduits (ink inlets 15 and supply conduits 23 ) for distributing ink to every ink chamber in the array can occupy a significant proportion of the wafer area. This can be a limiting factor for nozzle density on the printhead. By making some ink chambers part of the ink flow path to other ink chambers, while keeping each chamber sufficiently free of fluidic cross talk, reduces the amount of wafer area lost to ink supply conduits.
Ink Chamber with Multiple Actuators and Respective Nozzles
Referring to FIG. 54 , the unit cell shown has two chambers 38 ; each chamber has two heater elements 29 and two nozzles 25 . The effective reduction in drop misdirection by using multiple nozzles per chamber is discussed above in relation to the embodiment shown in FIG. 49 . The additional benefits of dividing a single elongate chamber into separate chambers, each with their own actuators, is described above with reference to the embodiment shown in FIG. 46 . The present embodiment uses multiple nozzles and multiple actuators in each chamber to achieve much of the advantages of the FIG. 46 embodiment with a markedly less complicated design. With a simplified design, the overall dimensions of the unit cell are reduced thereby permitting greater nozzle densities. In the embodiment shown, the footprint of the unit cell is 64 μm long by 16 μm wide.
The ink permeable structure 34 is a single column at the ink refill opening to each chamber 38 instead of three spaced columns as with the FIG. 46 embodiment. The single column has a cross section profiled to be less resistive to refill flow, but more resistive to sudden back flow from the actuation pressure pulse. Both heater elements in each chamber can be deposited simultaneously, together with the contacts 28 and the cold spot feature 54 . Both chambers 38 are supplied with ink from a common ink inlet 15 and supply conduit 23 . These features also allow the footprint to be reduced and they are discussed in more detail below. The priming features 18 have been made integral with one of the chamber sidewalls 22 and a wall ink conduit 23 . The dual purpose nature of these features simplifies the fabrication and helps to keep the design compact.
Multiple Chambers and Multiple Nozzles for Each Drive Circuit
In FIG. 54 , the actuators are connected in series and therefore fire in unison from the same drive signal to simplify the CMOS drive circuitry. In the FIG. 46 unit cell, actuators in adjacent nozzles are connected in series within the same drive circuit. Of course, the actuators in adjacent chambers could also be connected in parallel. In contrast, were the actuators in each chamber to be in separate circuits, the CMOS drive circuitry would be more complex and the dimensions of the unit cell footprint would increase. In printhead designs where the drop misdirection is addressed by substituting multiple smaller drops, combining several actuators and their respective nozzles into a common drive circuit is an efficient implementation both in terms of printhead IC fabrication and nozzles density.
High Density Thermal Inkjet Printhead
Reduction in the unit cell width enables the printhead to have nozzles patterns that previously would have required the nozzle density to be reduced. Of course, a lower nozzle density has a corresponding influence on printhead size and/or print quality.
Traditionally, the nozzle rows are arranged in pairs with the actuators for each row extending in opposite directions. The rows are staggered with respect to each other so that the printing resolution (dots per inch) is twice the nozzle pitch (nozzles per inch) along each row. By configuring the components of the unit cell such that the overall width of the unit is reduced, the same number of nozzles can be arranged into a single row instead of two staggered and opposing rows without sacrificing any print resolution (d.p.i.). The embodiments shown in the accompanying figures achieve a nozzle pitch of more than 1000 nozzles per inch in each linear row. At this nozzle pitch, the print resolution of the printhead is better than photographic (1600 dpi) when two opposing staggered rows are considered, and there is sufficient capacity for nozzle redundancy, dead nozzle compensation and so on which ensures the operation life of the printhead remains satisfactory. As discussed above, the embodiment shown in FIG. 54 has a footprint that is 16 μm wide and therefore the nozzle pitch along one row is about 1600 nozzles per inch.
Accordingly, two offset staggered rows yield a resolution of about 3200 d.p.i.
With the realisation of the particular benefits associated with a narrower unit cell, the Applicant has focused on identifying and combining a number of features to reduce the relevant dimensions of structures in the printhead. For example, elliptical nozzles, shifting the ink inlet from the chamber, finer geometry logic and shorter drive FETs (field effect transistors) are features developed by the Applicant to derive some of the embodiments shown. Each contributing feature necessitated a departure from conventional wisdom in the field, such as reducing the FET drive voltage from the widely used traditional 5V to 2.5V in order to decrease transistor length.
Reduced Stiction Printhead Surface
Static friction, or “stiction” as it has become known, allows dust particles to “stick” to nozzle plates and thereby clog nozzles. FIG. 50 shows a portion of the nozzle plate 56 . For clarity, the nozzle apertures 26 and the nozzle rims 25 are also shown. The exterior surface of the nozzle plate is patterned with columnar projections 58 extending a short distance from the plate surface. The nozzle plate could also be patterned with other surface formations such as closely spaced ridges, corrugations or bumps. However, it is easy to create a suitable UV mask for the pattern columnar projections shown, and it is a simple matter to etch the columns into the exterior surface.
By reducing the co-efficient of static friction, there is less likelihood that paper dust or other contaminants will clog the nozzles in the nozzle plate. Patterning the exterior of the nozzle plate with raised formations limits the surface area that dust particles contact. If the particles can only contact the outer extremities of each formation, the friction between the particles and the nozzle plate is minimal so attachment is much less likely. If the particles do attach, they are more likely to be removed by printhead maintenance cycles.
Inlet Priming Feature
Referring to FIG. 47 , two unit cells are shown extending in opposite directions to each other. The ink inlet passage 15 supplies ink to the four chambers 38 via the lateral ink conduit 23 . Distributing ink through micron-scale conduits, such as the ink inlet 15 , to individual MEMS nozzles in an inkjet printhead is complicated by factors that do not arise in macro-scale flow. A meniscus can form and, depending on the geometry of the aperture, it can ‘pin’ itself to the lip of the aperture quite strongly. This can be useful in printheads, such as bleed holes that vent trapped air bubbles but retain the ink, but it can also be problematic if stops ink flow to some chambers. This will most likely occur when initially priming the printhead with ink. If the ink meniscus pins at the ink inlet opening, the chambers supplied by that inlet will stay unprimed.
To guard against this, two priming features 18 are formed so that they extend through the plane of the inlet aperture 15 . The priming features 18 are columns extending from the interior of the nozzle plate (not shown) to the periphery of the inlet 15 . A part of each column 18 is within the periphery so that the surface tension of an ink meniscus at the ink inlet will form at the priming features 18 so as to draw the ink out of the inlet. This ‘unpins’ the meniscus from that section of the periphery and the flow toward the ink chambers.
The priming features 18 can take many forms, as long as they present a surface that extends transverse to the plane of the aperture. Furthermore, the priming feature can be an integral part of other nozzles features as shown in FIG. 54 .
Side Entry Ink Chamber
Referring to FIG. 48 , several adjacent unit cells are shown. In this embodiment, the elongate heater elements 29 extend parallel to the ink distribution conduit 23 . Accordingly, the elongate ink chambers 38 are likewise aligned with the ink conduit 23 . Sidewall openings 60 connect the chambers 38 to the ink conduit 23 . Configuring the ink chambers so that they have side inlets reduces the ink refill times. The inlets are wider and therefore refill flow rates are higher. The sidewall openings 60 have ink permeable structures 34 to keep fluidic cross talk to an acceptable level.
Inlet Filter for Ink Chamber
Referring again to FIG. 47 , the ink refill opening to each chamber 38 has a filter structure 40 to trap air bubbles or other contaminants. Air bubbles and solid contaminants in ink are detrimental to the MEMS nozzle structures. The solid contaminants can obvious clog the nozzle openings, while air bubbles, being highly compressible, can absorb the pressure pulse from the actuator if they get trapped in the ink chamber. This effectively disables the ejection of ink from the affected nozzle. By providing a filter structure 40 in the form of rows of obstructions extending transverse to the flow direction through the opening, each row being spaced such that they are out of registration with the obstructions in an adjacent row with respect to the flow direction, the contaminants are not likely to enter the chamber 38 while the ink refill flow rate is not overly retarded. The rows are offset with respect to each other and the induced turbulence has minimal effect on the nozzle refill rate but the air bubbles or other contaminants follow a relatively tortuous flow path which increases the chance of them being retained by the obstructions 40 . The embodiment shown uses two rows of obstructions 40 in the form of columns extending between the wafer substrate and the nozzle plate.
Intercolour Surface Barriers in Multi Colour Inkjet Printhead
Turning now to FIG. 51 , the exterior surface of the nozzle 56 is shown for a unit cell such as that shown in FIG. 46 described above. The nozzle apertures 26 are positioned directly above the heater elements (not shown) and a series of square-edged ink gutters 44 are formed in the nozzle plate 56 above the ink conduit 23 (see FIG. 46 ).
Inkjet printers often have maintenance stations that cap the printhead when it's not in use. To remove excess ink from the nozzle plate, the capper can be disengaged so that it peels off the exterior surface of the nozzle plate. This promotes the formation of a meniscus between the capper surface and the exterior of the nozzle plate. Using contact angle hysteresis, which relates to the angle that the surface tension in the meniscus contacts the surface (for more detail, see the Applicant's co-pending USSN (our docket FND007US) incorporated herein by reference), the majority of ink wetting the exterior of the nozzle plate can be collected and drawn along by the meniscus between the capper and nozzle plate. The ink is conveniently deposited as a large bead at the point where the capper fully disengages from the nozzle plate. Unfortunately, some ink remains on the nozzle plate. If the printhead is a multi-colour printhead, the residual ink left in or around a given nozzle aperture, may be a different colour than that ejected by the nozzle because the meniscus draws ink over the whole surface of the nozzle plate. The contamination of ink in one nozzle by ink from another nozzle can create visible artefacts in the print. Gutter formations 44 running transverse to the direction that the capper is peeled away from the nozzle plate will remove and retain some of the ink in the meniscus. While the gutters do not collect all the ink in the meniscus, they do significantly reduce the level of nozzle contamination of with different coloured ink.
Bubble Trap
Air bubbles entrained in the ink are very bad for printhead operation. Air, or rather gas in general, is highly compressible and can absorb the pressure pulse from the actuator. If a trapped bubble simply compresses in response to the actuator, ink will not eject from the nozzle. Trapped bubbles can be purged from the printhead with a forced flow of ink, but the purged ink needs blotting and the forced flow could well introduce fresh bubbles.
The embodiment shown in FIG. 46 has a bubble trap at the ink inlet 15 . The trap is formed by a bubble retention structure 32 and a vent 36 formed in the roof layer. The bubble retention structure is a series of columns 32 spaced around the periphery of the inlet 15 . As discussed above, the ink priming features 18 have a dual purpose and conveniently form part of the bubble retaining structure. In use, the ink permeable trap directs gas bubbles to the vent where they vent to atmosphere. By trapping the bubbles at the ink inlets and directing them to a small vent, they are effectively removed from the ink flow without any ink leakage.
Multiple Ink Inlet Flow Paths
Supplying ink to the nozzles via conduits extending from one side of the wafer to the other allows more of the wafer area (on the ink ejection side) to have nozzles instead of complex ink distribution systems. However, deep etched, micron-scale holes through a wafer are prone to clogging from contaminants or air bubbles. This starves the nozzle(s) supplied by the affected inlet.
As best shown in FIG. 48 , printheads according to the present invention have at least two ink inlets 15 supplying each chamber 38 via an ink conduit 23 between the nozzle plate and underlying wafer.
Introducing an ink conduit 23 that supplies several of the chambers 38 , and is in itself supplied by several ink inlets 15 , reduces the chance that nozzles will be starved of ink by inlet clogging. If one inlet 15 is clogged, the ink conduit will draw more ink from the other inlets in the wafer.
Although the invention is described above with reference to specific embodiments, it will be understood by those skilled in the art that the invention may be embodied in many other forms.
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A method of fabricating a suspended beam in a MEMS process, said method comprising the steps of:
(a) etching a pit in a substrate, said pit having a base and sidewalls; (b) depositing sacrificial material on a surface of said substrate so as to fill said pit; (c) removing said sacrificial material from a perimeter region within said pit and from said substrate surface surrounding said pit; (d) reflowing remaining sacrificial material within said pit such that said remaining sacrificial material contacts said sidewalls; (e) depositing beam material on said substrate surface and on said reflowed sacrificial material; and (f) removing said reflowed sacrificial material to form said suspended beam.
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