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CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] This application claims priority to and the benefit of filing of U.S. Provisional Patent Application Ser. No. 61/605,929, entitled “Waste to Product On Site Generator,” filed on Mar. 2, 2012, the specification and claims of which are incorporated herein by reference.
BACKGROUND OF THE INVENTION
[0002] 1. Field of the Invention (Technical Field)
[0003] The present invention relates to methods and apparatuses for electrolytic processing of waste brine solutions produced by water purification or other industrial processes, thereby producing one or more oxidants and/or disinfectants.
[0004] 2. Background Art
[0005] Note that the following discussion refers to a number of publications and references. Discussion of such publications herein is given for more complete background of the scientific principles and is not to be construed as an admission that such publications are prior art for patentability determination purposes.
[0006] Electrolytic technologies utilizing dimensionally stable anodes have been developed to produce oxidant solutions from brine solutions, and these technologies have grown in market presence and interest across a variety of applications. Dimensionally stable anodes are described in U.S. Pat. No. 3,234,110 to Beer, entitled “Electrode and Method of Making Same,” wherein a noble metal coating is applied over a titanium substrate. Electrolytic cells have had wide use for the production of chlorine and mixed oxidants for the disinfection of water. Some of the simplest undivided electrolytic cells are described in U.S. Pat. No. 4,761,208, entitled “Electrolytic Method and Cell for Sterilizing Water”, and U.S. Pat. No. 5,316,740, entitled “Electrolytic Cell for Generating Sterilizing Solutions Having Increased Ozone Content.” One limitation of these technologies is the operating cost associated with the feedstock of this process, consisting of sodium chloride and other dissolved salts which are converted into solutions comprising at least one oxidant. It is well accepted that one of the major failure mechanisms of undivided electrolytic cells is the buildup of unwanted films on the surfaces of the electrodes. The source of these contaminants can be either from the feed water to the on-site generation process, or contaminants in the salt that is used to produce the brine solution feeding the system. Typically these unwanted films consist of manganese, calcium carbonate, silica, or other unwanted substances. If buildup of these films is not controlled or they are not removed on a fairly regular basis, the electrolytic cells will lose operating efficiency and will eventually catastrophically fail (due to localized high current density, electrical arcing or some other event). Typically, manufacturers protect against this type of buildup by incorporating a water softener on the feed water to the system to prevent these contaminants from ever entering the electrolytic cell. However, these contaminants will enter the process over time from contaminants in the salt used to make the brine. High quality salt is typically specified to minimize the incidence of cell cleaning operations. U.S. Pat. No. 7,922,890 describes methods and apparatuses of creating low maintenance, highly reliable electrolytic cells for creating oxidants. However, this type of approach typically only works for lower hardness waters (<20 grains/gallon for example) and higher quality salts (>99.5% dry).
[0007] Many water purification processes produce a brine solution containing enough dissolved salts to be suitable for processing into a disinfectant/oxidant. Specifically, reverse osmosis, evaporation, distillation, chemical softening, and ion exchange technologies have waste streams with high concentrations of salts. Typically, however, these waste streams also have high concentrations of contaminants (typically measured as hardness) that would foul most electrolytic cells quickly, resulting in premature electrolytic cell failure.
[0008] More recently, though, solutions providers such as GE or Veolia Water have developed offerings such as the HERO or OPUS® technologies, where waste water is pretreated to reduce the hardness prior to exposing them to the RO membranes. This makes this waste stream from the RO membranes much more desirable as a possible feedstock for electrolytic generation of an oxidant from that waste stream, as most of the undesirable contaminants for electrolysis are removed via the pretreatment process.
SUMMARY OF THE INVENTION (DISCLOSURE OF THE INVENTION)
[0009] An embodiment of the present invention is a method for producing an oxidant, the method comprising adjusting the salinity and/or hardness of a waste stream thereby forming a brine solution; and electrolyzing the brine solution to produce at least one oxidant. The adjusting step preferably comprises measuring the salinity and/or hardness of the waste stream. The adjusting step optionally comprises adding water or processed water to the waste stream to reduce the salinity of the waste stream and preferably further comprises varying the relative flow rates of the waste stream and the water or processed water being input into an electrolytic cell. The adjusting step optionally comprises adding a saturated or near saturated salt solution to the waste stream to increase the salinity of the waste stream and preferably further comprises varying the relative flow rates of the waste stream and the saturated or near saturated salt solution being input into an electrolytic cell. The adjusting step preferably comprises treating the waste stream by a method selected from the group consisting of softening, ion exchange, filtering, and reverse osmosis. The brine solution preferably has a salinity between approximately 10 g/L and 40 g/L. The adjusting step preferably reduces a cleaning frequency of the electrolytic cell.
[0010] Another embodiment of the present invention is a method for cleaning an electrolytic cell, the method comprising measuring a salinity and hardness of a waste stream to be electrolyzed, calculating a frequency for cleaning the electrolytic cell based on the measured salinity and hardness of the waste stream and a spacing between electrodes of the electrolytic cell, and cleaning the electrolytic cell in accordance with the calculated frequency. The cleaning step preferably comprises reversing a polarity of the electrolytic cell and/or flushing solid contaminants from the electrolytic cell. The flushing is preferably performed once or twice a day or after the electrolytic cell was cleaned by reversing the polarity of the electrolytic cell. The method preferably further comprises adjusting the salinity and/or hardness of the waste stream, thereby reducing the cleaning frequency.
[0011] Another embodiment of the present invention is an electrolytic cell for electrolyzing a waste stream, the electrolytic cell comprising one or more devices for adjusting a flow rate of the waste stream entering an electrolytic cell; one or more dispersion tubes for transporting the waste stream into the electrolytic cell; a plurality of holes in the dispersion tubes, the holes angled to direct a flow of the waste stream toward bottom edges of the electrolytic cell; and one or more insulators substantially parallel to electrodes in the electrolytic cell and extending from a bottom of the electrolytic cell to at least a level of bottoms of the electrodes. The additive stream may comprise water, processed water, a saturated salt solution, or a near saturated salt solution. At least one of the devices can preferably flush the cell with the waste stream or water at a flushing flow velocity higher than (preferably at least twice) the operational flow velocity of the waste stream. Spacing between adjacent holes is preferably between approximately 0.5″ and approximately 2″. The electrolytic cell preferably comprises electrodes which are spaced more widely than electrodes in an electrolytic cell designed to produce a similar quantity and strength of oxidants from a controlled brine stream. The electrolytic cell preferably comprises intermediate electrodes, wherein spacing between adjacent intermediate electrodes is preferably between approximately 0.15″ and approximately 0.5″, and more preferably 0.25″+/−0.1″.
[0012] Objects, advantages, novel features, and further scope of applicability of the present invention will be set forth in part in the detailed description to follow, taken in conjunction with the accompanying drawings, and in part will become apparent to those skilled in the art upon examination of the following, or may be learned by practice of the invention. The objects and advantages of the invention may be realized and attained by means of the instrumentalities and combinations particularly pointed out in the appended claims.
BRIEF DESCRIPTION OF THE DRAWINGS
[0013] The accompanying drawings, which are incorporated into and form a part of the specification, illustrate an embodiment of the present invention and, together with the description, serve to explain the principles of the invention. The drawings are only for the purpose of illustrating various embodiments of the invention and are not to be construed as limiting the invention. In the drawings:
[0014] FIG. 1 is a schematic showing brine waste at a high salinity being converted electrochemically into usable oxidant.
[0015] FIG. 2 is a schematic showing brine waste at a low salinity being converted electrochemically into usable oxidant.
[0016] FIG. 3 is a schematic showing brine waste with a very high hardness to salinity ratio, where divalent cations are removed prior to electrolysis making the brine waste appropriate for electrolysis.
[0017] FIG. 4 is a high level schematic of an on-site electrolytic generator for converting brine waste to oxidant.
[0018] FIG. 5 is a cross section of an electrolytic cell for converting brine waste to oxidant.
[0019] FIG. 6 is a 3D representation of an electrolytic cell for converting brine waste to oxidant.
DETAILED DESCRIPTION OF THE INVENTION
[0020] Embodiments of the present invention electrolize the waste stream from an industrial process, such as reverse osmosis, ion exchange softening, chemical softening, evaporation, distillation, produced or flowback water from oil and gas wells, to produce an oxidant and/or disinfectant. This waste stream may be highly variable in salt content, presenting a unique challenge for consistent oxidant production. For example, a water source with low dissolved salt may be injected into the electrolyte for a high salinity waste stream at a rate determined by the operating current of the electrolytic cell. When the operating current is high, more water with low dissolved salt is preferably injected to reach the target operating current of the cell. Conversely, when the operating current is low, the water with low dissolved salts may be replaced with a concentrated brine solution injection to raise the current to the desired operating condition.
[0021] As used throughout the specification and claims, the term “waste stream” means an aqueous byproduct of an industrial process or application, including but not limited to frac water, produced water from oil and gas operations, cooling towers, desalination, or evaporation, the byproduct having a sodium chloride content of greater than approximately 1 g/L.
[0022] Embodiments of the present invention utilize an electrochemical process to convert a waste brine stream into a usable oxidant; one such process is shown in FIG. 1 . In FIG. 1 , raw water 1 is first treated via softening process equipment 2 to remove divalent cations (typically those acknowledged as hardness) and other contaminants. Softened waste water 3 is then put through purification processing equipment 4 , such as reverse osmosis or other membrane processing equipment, to remove monovalent cations (i.e. salts) to create processed water 5 and brine waste 6 . Processed water 5 can often be used for industrial processes, is appropriate for discharge, and/or can even potentially be used as potable water. Brine waste 6 is then processed and electrolyzed in on-site electrolytic generator 7 into oxidant 8 . Oxidant 8 can either be stored in a tank or directly used for a variety of applications (not shown). To produce a desired concentration of oxidant 8 (for example 100 to 1000's mg/L) and/or provide electrolyte with the proper salinity for electrolysis, dilution water 9 may optionally be used to dilute brine waste 6 in the on-site electrolytic generator if brine waste 6 is too salty.
[0023] Raw water 1 can be from virtually any source. However, certain sources have, or certain industrial processes produce a waste stream that has, a somewhat higher incidence of dissolved salts in the raw water, such as seawater, produced and/or flowback water from oil and gas operations, ground water, surface water, waste from industrial processes, waste water from municipalities, potable water, etc.
[0024] Brine waste 6 is often at a fairly high salinity, often greater than approximately 40 g/L but less than that for saturated brine (317 g/L). In the event that the salinity is greater than approximately 40 g/L, dilution water 9 may be used to dilute the brine waste to a lower level that is more appropriate for electrolysis, typically between approximately 10 g/L and 40 g/L. A small percentage of processed water 5 may optionally be used as the dilution water 9 .
[0025] Depending on the nature of the raw water 1 and the purification processing equipment 4 , if not required softening process equipment 2 may not be included in order to reduce cost and complexity of the system.
[0026] Some industrial processes produce a brine waste that does not require complicated purification processing equipment 4 because the brine waste has the appropriate hardness to salinity ratio in the brine solution that it can be electrolyzed. Examples of this are waste water remediation and/or flowback or produced waters from oil and gas operations. Thus, in one embodiment of the invention, there is no processed water 5 , and the purification processing equipment comprises or consists essentially of a simple filter to remove large particles (typically >20 microns, but preferably >100 microns) from brine waste 6 .
[0027] FIG. 2 shows another embodiment of the invention. In the event that the salinity of the waste brine 6 is low, less than approximately 10 g/L for example, solid brine storage tank 11 may be utilized. In the solid brine storage tank, solid salt is saturated in water, creating a brine solution 10 at or near saturation (approximately 317 g/L). In this event, a small amount of saturated brine solution 10 is combined with the brine waste 6 for electrolysis by on-site electrolytic generator 7 .
[0028] Another embodiment of the invention is shown in FIG. 3 . In this embodiment, divalent cations are removed from brine waste 6 using selective ion exchange process equipment 12 , leaving a brine solution suitable for electrolytic generation of oxidant in on-site electrolytic generator 7 .
[0029] Compared to existing commercially available on-site electrolytic generators, embodiments of that required to convert waste to oxidant in accordance with the present invention are substantially different. FIG. 4 shows a high level schematic of an embodiment of on-site electrolytic generator 7 . The electrolytic generator takes brine waste 6 and either dilution water 9 or saturated brine solution 10 and generates oxidant 8 by electrolyzing it in electrolytic cell 14 . Depending on the salt concentration of brine waste 6 . the relative flow rates of brine waste 6 and/or dilution water 9 or saturated brine solution 10 are preferably controlled by integrated controls 15 , preferably via devices 13 such as pressure mechanisms, pumps, or valves. These input rates and the current and/or voltage applied to the electrolytic cell are preferably varied to maintain a controlled oxidant concentration.
[0030] During operation, devices 13 can be controlled to intermittently flush the electrolytic cell with very high flow rates (preferably greater than approximately two times the operational flow rate) of water or waste stream 6 . If the latter is used, flushing can occur during the electrolysis process. This flushing prevents or reduces deposits from accumulating at the bottom of the electrolytic cell. Integrated controls 15 also preferably control reversing the polarity of the cell, which removes deposits from the electrode surfaces. This process is more fully described in U.S. Patent Application Publication No. 20090229992.
[0031] Despite being exposed to high levels of hardness, suspended solids, dissolved solids, and contaminants such as silica, electrolytic cell 14 is preferably designed such that it is robust and has an adequate lifetime. FIG. 5 shows a cross section of an embodiment of a bipolar electrolytic cell useful for the current invention. Primary electrodes 15 and intermediate electrodes 16 are preferably coated with Dimensionally Stable Anode (DSA) material, such as ruthenium, iridium, palladium, or other materials known in the art. Both the primary anode and preferably cathode are coated with DSA so that the polarity of the cell can be intermittently reversed to remove any deposits on the electrodes. A series of intermediate electrodes 16 are disposed between primary electrodes 15 . The spacing from one electrode to the next is wider than on most typical electrolytic cells, preferably greater than 0.15″ but less than approximately 0.5″, preferably 0.25″+/−0.1″. In general, the wider the spacing the more inefficient the cell is, but wider spacing is useful with the present invention to prevent elevated contaminants from the incoming brine waste 6 from depositing on intermediate electrodes 16 and creating an electrical short circuit and arcing and/or premature cell failure. Brine waste 6 is introduced to the electrolytic cell via dispersion tube 18 , which comprises holes which direct the brine waste towards the bottom of electrolytic cell 14 , and more preferably, to the bottom corners of the electrolytic cell 14 . The size, angles, and spacing of these holes down the length of the dispersion tube are preferably chosen to increase the velocity of the fluid, such that particles are less likely to settle into the bottom of the cell. By accelerating the brine waste 14 and angling it down and substantially towards the corners of the bottom of the electrolytic cell, any contaminants and/or particles that have begun to settle into the bottom of the cell can be accelerated and re-suspended up and between electrodes 16 and out of the electrolytic cell 14 . This design makes it particularly easy to flush larger particles and/or contaminants out of the bottom of the cell by performing intermittent flushing, preferably 1-2 times a day, preferably at high flow rates either while the cell is energized or not. During operation, brine waste 6 stream through dispersion tubes 18 and out of the holes, where its flow is directed to agitate any particles that may have settled. The brine waste stream then travels up between the electrodes, and, when power is applied to primary electrodes 15 , it is electrolyzed to form oxidant 8 which leaves the electrolytic cell.
[0032] Electrolytic cell preferably comprises one or more electrical isolator blocks 17 , which preferably extend from the bottom of the cell at least up to the bottom of the electrodes. One isolator block is preferably present every few intermediate electrodes 16 , which prevents loss of electrical efficiency and also protects the electrodes from being exposed to voltages beyond their breakdown voltages, for example due to high salinity of the brine waste. Thus the use of these blocks enables particles to build up in the cell without arcing between electrodes taking place. Typically electrical isolator blocks 17 are spaced every 5-10 electrodes, but depending on the chemistry desired in the oxidant and the salinity of brine waste 6 , one electrical isolator block 17 could be present every 3 electrodes or even up to every 40 electrodes. As shown in the perspective view of electrolytic cell 14 shown in FIG. 6 , dispersion tubes 18 preferably distribute the brine waste 6 into the cell through an array of holes as described above. The holes are preferably spaced apart between approximately 0.5″ and approximately 2″, preferably 1″+/−0.25″.
[0033] The characteristics of the brine waste vary considerably with different waste applications, which has implications on the frequency with which the electrolytic cell is cleaned. Specifically, the ratio of divalent cations to monovalent cations is particularly important. For a given ratio, the growth rate of contaminants on the electrodes is calculated, and for a given electrode spacing, the required cleaning frequency of the cell to prevent arcing between electrodes can be determined, after applying a given safety factor. From this cleaning frequency the expected life of an electrolytic cell can then be predicted given a certain number of cycles to failure. Thus, treating the waste stream so that the salinity and/or hardness are in optimal ranges can greatly increase the lifetime of the cell by reducing required cleaning frequency. By controlling these parameters, as well as flow rate, voltage, and current in the electrolysis cell, the system can be optimized for energy conversion efficiency as salt is a waste product for various industrial processes and is therefore is extremely inexpensive.
Example 1
[0034] A waste brine stream was created by a system very similar to the system shown in FIG. 1 , in which the softening water processing equipment was an ion exchange resin softener, and the purification process equipment was a membrane based reverse osmosis filter. The salinity of the waste brine stream was measured at 40 g/L, and had 100 grains/gallon hardness. Electrolyzing this waste brine stream was completed yielding an oxidant with 3400 mg/L FAC, with a required cell cleaning frequency of about 7 days corresponding to an expected cell life well over 10 years.
Example 2
[0035] A waste brine stream consisting of produced water from an oil and gas operation was created by a system similar to the one shown in FIG. 1 , with the exception that the softening water processing equipment was not present and the process equipment was a simple filter to remove particles >80 microns. The salinity of the waste brine stream was 17 g/L, and the hardness was 24 grains, and electrolyzing it yielded an oxidant with 2200 mg/L FAC, with a cell cleaning frequency of 12 days and an expected cell life well over 10 years.
Example 3
[0036] A waste brine stream from a desalination plant was created with a system similar to the one depicted in FIG. 1 , with no softening processing equipment. The desalination plant relied on reverse osmosis to process the water. The waste brine stream had a salinity of 210 g/L (typically too salty for effective electrolysis) and a hardness of 2800 grains/gallon. The waste brine stream was recombined with a side stream of RO permeate as described herein to deliver a salinity of approximately 15 g/L to the electrolytic cell. Electrolysis of this stream yielded an oxidant with 4200 mg/L FAC, with a cell cleaning frequency of 1.3 days and an expected cell life of 3.9 years.
Example 4
[0037] Waste blowdown from a cooling tower had approximately 4 g/L salt and a hardness of 180 grains/gallon. This waste blowdown was directly electrolyzied, yielding an oxidant with 650 mg/L FAC with a cleaning frequency of 0.4 days and an expected cell life of 1.2 years. When combined with a solid brine source as shown in FIG. 2 , the salinity was increased to 15 g/L, lengthening the cleaning frequency to 1.5 days and increasing expected cell life to over 5 years. In both instances, the oxidant produced was used to disinfect the cooling tower.
[0038] Although the invention has been described in detail with particular reference to the disclosed embodiments, other embodiments can achieve the same results. Variations and modifications of the present invention will be obvious to those skilled in the art and it is intended to cover all such modifications and equivalents. The entire disclosures of all patents and publications cited above are hereby incorporated by reference. | Method and apparatus for adjusting the salinity and/or hardness of a process waste stream so that the stream may be electrolyzed to form an oxidant or disinfectant. Also an electrolytic cell having certain features such as widely spaced electrodes, flushing capabilities, and insulating dividers that can accommodate waste streams that have varying salinity, hardness, and dissolved solids content. | 2 |
[0001] This application claims priority to provisional application U.S. Ser. No. 60/984,562, filed Nov. 1, 2007, the contents of which are incorporated by reference herein in its entirety.
FIELD OF THE INVENTION
[0002] The present invention is directed to certain peptide linkers for conjugating drugs to ligands, and the resulting drug-linker-ligand molecules and compositions thereof. The invention also encompasses processes of preparation of the conjugated molecules, and methods of using them for killing or controlling the growth of cells, particularly malignant cancer cells. The peptide linkers are distinguished from known linkers in that they allow the intracellular release of the drug from the trans Golgi network.
BACKGROUND OF THE INVENTION
[0003] Targeted delivery of cytotoxic drugs to tumor cells is desirable to avoid killing normal cells upon the systemic administration of such agents. Typical targeted drug delivery systems are composed of a cytotoxic agent conjugated to a tumor-specific antibody, forming an “immunoconjugate”. When systemically administered, the immunoconjugate will thus bind only to tumor cells in the body, and thereby deliver the cytotoxic drug intracellularly to the tumor cells, and not normal cells. The cytotoxic agent is not active when conjugated to the antibody, but will become active upon being cleaved from the antibody intracellularly.
[0004] Most endocytosed cell surface proteins are processed via the lysosomal pathway, where they are degraded by proteolysis and acidic conditions in the lysosome. Lysosome specific proteinases have thus previously been exploited to release drugs from systemically stable immunoconjugates. See, e.g., Firestone et al., U.S. Pat. No. 6,214,345. However, this strategy necessarily depends on the immunoconjugate being subject to the lysosomal pathway upon cellular internalization. Others have taken advantage of the lysosomal processing pathway in developing immunoconjugates. For example, Seattle Genetics, Inc. (Bothell, Wash., US) has developed a linker/drug technology based on specific endoproteolytic cleavage and release of MMAE and MMAF auristatins by the lysosomal proteinase cathepsin B.
[0005] Further, hydrazone bonds and stabilized disulfide bonds, which are moderately stable systemically, but labile to hydrolysis and reduction, respectively, under lysosomal conditions, have also been exploited in immunoconjugate anticancer strategies for lysosome-mediated release of highly potent calicheamicin (Wyeth's MYLOTARG™) and DM1 and DM4 maytansinoids (ImmunoGen, Inc., Waltham, Mass., US), respectively.
[0006] However, numerous plant and bacterial toxins have evolved such as to escape lysosomal degradation following cellular internalization, and to instead rely on retrograde transport through the trans Golgi network (TGN), where the specific endoproteolytic cleavage by furin will release active toxin into the cytosol, where the toxin exerts its affects by inactivating the ribosomes.
[0007] While it is known in the art that certain naturally-occurring toxins are activated intracellularly (in the TGN) by the calcium-dependent serine protease, furin, by cleavage between their protein subunits to thereby release the active toxin to the cytosol, up till now, the prior art has not taught the artificial use of a furin cleavage site to link the cell-targeting ligand component (such as an antibody or fragment thereof) to a cytotoxic small molecule drug, for the targeted delivery of the prodrug and the intracellular activation (through cleavage with furin) thereof. The present invention addresses the need for the delivery of cytotoxic drugs in cases in which a conjugated drug-ligand is internalized via the TGN (and not the lysosomal pathway).
SUMMARY OF THE INVENTION
[0008] The present invention was developed to utilize the TGN's furin protease to release a cytotoxic drug from a drug-ligand conjugate into the cytosol, where it can exert its effects. This invention is accomplished by the insertion of an intramolecular protease cleavage site between the cytotoxic drug (i.e., a small molecule drug, rather than a proteinaceous toxin) and the cell-binding components of the targeting ligand moiety. The use of such a peptide linker thus mimics the way certain naturally-occurring toxins are activated intracellularly.
[0009] The present invention has thus been conceived to exploit the endoprotease activity and specific subcellular localization of furin in the trans Golgi network (TGN) to specifically release potent cell killing drug molecules from endocytosed immunoconjugate therapeutic agents, in cases where the internalized cell surface target receptor escapes the endosomal pathway, and thus lysosomal processing, and instead directs the bound immunoconjugate by retrograde transport to the TGN.
[0010] Thus, in one aspect of the present invention are the drug-ligand conjugates, which are linked via a furin-cleavable moiety, and pharmaceutical compositions thereof.
[0011] In other aspect, the present invention provides processes for making the drug-ligand conjugates containing the furin cleavable moiety.
[0012] In yet another aspect are methods of using the drug-ligand conjugates of the present invention to inhibit undesirable growth or activity of cells, such as cancer cells, in a subject by administering to the subject a therapeutically effective amount of the drug-ligand conjugates described herein.
DETAILED DESCRIPTION OF THE INVENTION
[0013] The first object of the present invention is accomplished by chemically synthesizing a linker/drug molecule for chemical conjugation to a targeting ligand component, wherein the linker is composed of a peptide sequence specifically recognized and endoproteolytically cleaved by furin. The peptide sequence recognized by furin is R-X-[R/K]-R, where X is any amino acid, R is arginine, and K is lysine. The linked cytotoxic drug becomes active when released into the cytosol following furin cleavage in the TGN.
[0014] The linker/drug molecule is synthesized to also contain a bifunctional reactive component, which allows for stable chemical conjugation of the linker/drug to the targeting ligand molecule (such as an antibody or other cell surface protein/receptor-targeting molecule). An example of such a bifunctional reactive component is maleimide, which specifically reacts with free thiol groups for covalently bonding the ligand via a thioether to the drug.
[0015] The advantage of the present invention is that such conjugated “prodrugs” allow for proteolytic cleavage by furin, in the Golgi, to thereby release the active drug from a stable, specifically targeted immunoconjugate, which is for use in situations in which the cell surface target receptor for the ligand is one that escapes the typical endosomal pathway and lysosomal processing and is directed instead to the TGN. The highly specific endoproteolytic activity and specific localization of furin to the TGN enables the design of linker/drug molecules for the development of this novel immunoconjugate therapeutic strategy.
[0016] As mentioned above, most endocytosed cell surface proteins are processed via the lysosomal pathway and degraded by proteolysis and the acidic conditions in the lysosome. Lysosome-specific proteinases have thus been exploited in order to release drugs intracellularly from systemically stable immunoconjugates. However, some cell surface proteins that are specifically expressed on a target cell population, and thus highly desirable as a target for immunoconjugate or hormone prodrug therapy, escape lysosomal processing by alternative retrograde transport to the TGN.
[0017] One such cell surface protein that is an especially good target for cancer cells, and is preferred for the present invention, is the biomarker, aspartyl (asparaginyl) β-hydroxlase (AAH). For details about this cancer biomarker, see U.S. Pat. Nos. 6,783,758; 6,797,696; 6,812,206; 6,815,415; 6,835,370; and 7,094,556, the entireties of which are specifically incorporated herein by reference.
[0018] Our work on the antibody targeting of AAH and subsequate intracellular fate of the endocytosed drug-antibody indicated that processing occurs in the Golgi via the TGN, and not via the typical endosomal pathway and lysosomal processing, and thus directs the bound immunoconjugate by retrograde transport to the TGN instead. Thus, if utilizing AAH as the cellular target of an immunoconjugate (for instance), a linker as that disclosed herein, which will be cleaved by furin in the TGN, is required for activation and release of the drug moiety of the immunoconjugate into the cytosol.
[0019] The cell binding ligand component of the conjugates of the present invention is preferably a monoclonal antibody or an antigen-binding fragment thereof. More preferably, the cell binding ligand is a monoclonal antibody, or fragment thereof, that is reactive with an antigen or epitope of an antigen expressed on a cancer (whether hematopoietic or solid malignant neoplasm). The monoclonal antibody may be a murine, chimeric, humanized, or human monoclonal antibody, and may be intact, or in the form of a fragment (such as Fab, Fab′, F(ab) 2 , F(ab′) 2 , or single-chain Fv).
[0020] More preferably, the cell-binding ligand is an antibody, or fragment thereof, that will bind to tumor-associated biomarkers that are expressed at high levels on the target cells and that are expressed predominantly or only on diseased cells versus normal cells. Such an antibody or fragment thereof also is preferably one that will be internalized after binding to the target cell. Antibodies with such characteristics contemplated as useful for cancer-targeted conjugates of the present invention include those that target any cancer-associated antigens that are found to be internalized via the TGN, such AAH. An especially preferred embodiment in this regard are antibodies to HAAH for treating cancer in humans.
[0021] Preferably, the monoclonal antibody or fragment is human or humanized, so as to limit the possibility of an undesirable immune reaction if administered to a human patient. A humanized antibody is a recombinant protein in which the CDRs from an antibody from one species; e.g., a murine antibody, is transferred from the heavy and light variable chains of the murine antibody into human heavy and light variable domains. The constant domains of the antibody molecule are derived from those of a human antibody. Methods of humanizing non-human antibodies are known in the art, and described, for example, in U.S. Pat. Nos. 5,225,539, 5,585,089, and 5,639,641, the disclosures of which are incorporated by reference herein in their entireties. Most preferred for administration to human cancer patients is a human antibody with high specificity for and high affinity to human AAH (HAAH), which can be derived from the disclosure of U.S. Pat. No. 7,413,737, which is hereby incorporated herein in its entirety by reference.
[0022] The drug moiety useful in the linked conjugates of the present invention may be any small molecule, cytotoxic or cytostatic compounds, which are available at the present time or which are developed in the future. Most preferably, the drug is one that is particularly highly toxic in small amounts, as relatively few molecules of it will be internalized into the targeted cells (as opposed to its action systemically). Examples of such drugs are epirubicin, doxorubicin (DOX), morpholinodoxorubicin (morpholino-DOX), cyanomorpholino-doxorubicin (cyanomorpholino-DOX), 2-pyrrolino-doxorubicin (2-PDOX), MMAE and MMAF auristatins, DM1 and DM4 maytansinoids, taxol, and calicheamicin. A preferred embodiment for the drug of the conjugates of the present invention are DOX, the auristatins or the maytansinoids.
[0023] The immunoconjugate thus comprises a cell binding ligand and at least one drug for killing or inhibiting the growth of the targeted diseased cells. The cell binding agent is preferably a monoclonal antibody or a fragment thereof, and the drug moiety is preferably an anti-mitotic agent. In a particularly preferred embodiment, the immunoconjugate comprises the DOX and a human anti-HAAH monoclonal antibody. The pharmaceutical compositions of the conjugates are further comprised of a pharmaceutically acceptable carrier, excipient or diluent. A typical pharmaceutical composition of the present invention is prepared by mixing the conjugate(s) with pharmaceutically acceptable carriers, excipients or stabilizers, in the form of lyophilized formulations or aqueous solutions.
[0024] The furin-sensitive cleavage site of the conjugates of the present invention is selected from the peptide sequence R-X-[R/K]-R, where R denotes arginine, X is any amino acid, and K is lycine. The “R/K” indicates that this amino acid may be either arginine or lysine. One or more amino acids may be present in this peptide sequence for convenience during synthesis of the conjugate, as long as they do not interfere with the ultimate cleavage of the active drug component intracellelularly.
[0025] The furin-cleavage site peptide is synthetically bound to the cell-binding ligand (such as an antibody or fragment thereof), and synthetically linked at its free terminus to the small molecule drug component in such a way that the drug is stable and inactive outside of the target cell (i.e., systemically stable), until cleaved from the conjugated molecule intracellularly to its active form.
[0026] Thus, the present invention addresses a problem in the prior art concerning a way to achieve intracellular drug activation of a conjugated “prodrug” that does not enter the cell by way of the endosomal pathway, but via the TGN, in a simple yet elegant way.
[0027] More specifically, in a preferred embodiment, the drug/linker conjugate of the invention comprises 1) a maleimide group for conjugation to an AAH-targeting ligand via a highly stable thioether bond, 2) an R-X-[K/R]-R consensus recognition amino acid sequence for specific endoproteolytic cleavage by furin either following internalization and retrotransport to the trans-Golgi network or at the cell surface of AAH-expressing cancer cells, 3) a p-aminobenzylcarboxy or γ-aminobutyric acid spacer between the furin cleavage site and drug, and 4) a small molecule drug that is highly toxic to cells following its intracellular proteolytic release by furin.
[0028] The use of p-aminobenzylcarboxy or γ-aminobutyric acid spacers between the drug and furin cleavage site allows the further advantage of spontaneous hydrolytic spacer removal following enzymatic proteolysis, to give a free underivatized drug molecule.
[0029] The drug-linker-ligand conjugates of the present invention can be prepared using the reactants, conditions and synthesis schemes described in detail in U.S. Pat. No. 6,214,345 of Firestone et al. (which is hereby specifically incorporated by reference herein in its entirety), with the exception being that the peptide linker of the instant invention is different from the peptide linker of the '345 patent, requiring a modified synthesis scheme to construct our peptide.
[0030] The present invention further provides methods of treating cancer in a subject in need thereof, comprising administering to the patient a therapeutically effective amount of a conjugate described herein. The cancer to be treated is a malignant solid tumor or a hematopoietic neoplasm, and the subject is preferably a human patient.
[0031] As a preferred embodiment for the treatment of cancer in humans, the conjugate is composed of doxirubicin as drug and an anti-HAAH antibody as ligand. For such treatment, the pharmaceutical composition of this conjugate is administered parenterally in an amount of about 100 ng to about 10 mg of conjugate/kg body weight on a weekly basis during therapy.
[0032] In the further description and examples below, the abbreviations having the following meanings: R (or Arg) is arginine; K (or Lys) is lysine; T is threonine; X, X 1 , and X 2 mean any amino acid, and may be the same or different; Fmoc is fluorenylmethoxycarbonyl; NHS is N-hydroxysuccinimide; DCC is dicyclohexylcarbodiimide; Mtr is 4-methoxytrtyl; EEDQ is N-ethoxycarbonyl-2-ethoxy-1,2-dihydroquinoline; MC is 6-maleimidocaproyl; PABOH is p-aminobenzyl alcohol; DOX is doxorubicin; PABC is p-aminobenzylcarbonyl; THF is tetrahydrofuran; DCU is dicyclohexylurea; Val is L-valine; DCC is dicyclohexylcarbodiimide; DME is 1,2-dimethoxyethane; MMAE is monomethylauristatin; and SSPS means solid phase peptide synthesis.
EXAMPLES
Example 1
Components and Synthesis of the Peptide Linker
[0033] Essentially, the furin cleavage site peptide component of the conjugate, R-X-[R/K]-R (where X is any amino acid), is synthesized as an Mtr-blocked peptide acid by established Fmoc solid phase peptide synthesis procedures, using a hydroxymethyl-functionalized solid support resin (which allows mild acid cleavage from the resin without removing Mtr blocking groups). An Fmoc-X 2 -OH group (is added N-terminally by DCC activation to the NHS ester and coupling to NH 2 -R(Mtr)-X 1 -K(Mtr)-OH (where X 2 is preferably K, F, R or T, but can be any natural amino acid, and X 1 is any amino acid). The C-terminal carboxylic acid is then amidated with p-aminobenzyl alcohol using EEDQ; Fmoc is removed with diethylamine; and the free amine of the N-terminal amino acid X 2 is coupled to malimidocaproyl-NHS to result in the molecule: MC-X 2 -R(Mtr)-X 1 -K(Mtr)-R(Mtr)-PABOH.
[0034] The PABOH group is activated with p-nitrophenol chloroformate and coupled to DOX-HCl. The Mtr blocking groups are then removed with dichloroacetic acid to result in the final drug/linker molecule, MC-X 2 -R-X 1 -K-R-PABC-DOX.
Example 2
Synthesis of the Conjugate MC-Arg-Arg-AA-Lys-Arg-PABC-DOX
[0035] In the synthesis scheme below, Arg is arginine, Lys is lysine, AA is any amino acid, and MC, PABC and DOX have the meanings given above.
[0000]
Example 5
[0036] The immunoconjugates of the preferred embodiments of the invention are obtained by reacting the drug/furin cleavage site molecules of the above examples with the target antibody using methods well known in the art. For instance, the disulfide groups of a monoclonal antibody are reduced with dithiothreitol, and excess DTT is removed by desalting into PBS 1 mM DPTA. The reduced monoclonal antibody is reacted with 1.1 molar equivalents of the drug/linker conjugate in cold 20% acetonitrile and desalted into PBS to give the final antibody-linker-drug conjugate. | Disclosed are certain peptide linkers for conjugating drugs to ligands, and the resulting drug-linker-ligand molecules and compositions thereof. The conjugated molecules useful for the targeted delivery of drugs to the desired cells, and allow for the intracellular release of the drug in cases where the targeted antigen is internalized via the trans Golgi network and not the lysosomal pathway. | 0 |
BACKGROUND OF THE INVENTION
The invention is based on a road sign recognition device and a method for recognizing road signs. From German Patent DE 40 23 952 C2 a road sign recognition device is already known in which an image processing method is employed for the road sign recognition.
SUMMARY OF THE INVENTION
The method of the invention and the apparatus of the invention have the advantage over the prior art that by coupling a road sign recognition device with a navigation device, information can be exchanged between the two systems, and as a result the data ascertained by the two systems can supplement one another, which in turn contributes to enhancing the safety and reliability of each of the systems coupled to one another. This is especially important for instance if interventions are to be made into the speed controller of the vehicle or the like by way of the coupled system; failure to recognize road signs, or recognizing them incorrectly, would mean significant danger to the vehicle driver and to the vehicle itself.
BRIEF DESCRIPTION OF THE DRAWING
FIG. 1 is a view schematically showing an apparatus for road sign recognition and for navigation in accordance with the present invention; and
FIG. 2 is a view showing a process flow diagram illustrating various steps of the inventive method for road sign recognition and for navigation.
DESCRIPTION OF THE PREFERRED EMBODIMENT
FIG. 1 shows a coupled system 20 for road sign recognition and navigation, which can for instance be built into a motor vehicle 11 . The coupled system 20 includes a device 2 for road sign recognition, which is coupled via data exchange lines 1 to a device 3 for navigation. The device 2 for road sign recognition is connected via sensor lines 10 to vehicle area sensors 4
The vehicle area sensors, such as cameras, are installed for instance in the region of the windshield 5 or in the front region 6 near the front headlights or the bumper. The devices 2 and 3 communicate with an evaluation unit 7 via further data lines 14 and 15 .
The device 2 is used for road sign recognition, and in particular for furnishing road sign recognition data. The device 3 for navigation serves to furnish navigation data, for instance by way of digital road maps stored in a memory; these navigation data include for instance the position and current road type. Via the data exchange lines 1 , the device for navigation can communicate data to the road sign recognition device 2 , in order to supplement the road sign recognition data. Examples of data communicated by the navigation device are:
1. Reporting the current road type, such as city street, country road, Autobahn, country lane, and so forth; this can contain context information that for instance indicates the maximum allowed vehicle speed for a type of road.
2. Reporting the change of the vehicle to a new road type or its turning onto a new road, such as a change from a country road to a federal road or the like; as a result of this change, the validity of certain road signs, such as speed limits, is thus cancelled.
3. Reporting when entering and leaving a town. The speed limits are as a rule enforced more strongly inside a town than outside city limits. This can be taken into account in reports made by the road sign recognition system to the driver.
4. Communicating streets running parallel to the current street or road. As a result, the validity of the road signs set up beside a street extending parallel can be blanked out from the current street by the device for road sign recognition. Because of the coupling between road sign recognition and the navigation system, the relevance of the road signs recognized by the device for road sign recognition can be assessed. This enhances the quality of road sign recognition. A reverse order of information flow is also provided, in which the device for road sign recognition communicates information to the device 3 for navigation, via the data exchange lines 1 . For example, the recognition of the danger sign “construction site” can be named, in which the course of the road may have changed because of the construction site and no longer matches the data of the digital map in the navigation system. In particular, the navigation device 3 contains a map memory for storing digital map data in particular, as well as comparison means for comparing the road sign recognition data, which are transmitted from the device for road sign recognition, with the map data. As a result, if there are deviations, a warning can be made to the vehicle driver. In each case, the knowledge of the construction site can be taken into account in reports made by the navigation system to the driver. Conversely, the device for road sign recognition can have a data buffer for temporary storage of data communicated by the navigation device. These data include for instance the current road type, the number of lanes in the road, the width of the roadway, leaving or entering a town, dangers such as a sharp curve at a great distance, implicit cancellation of the validity of road signs because of a change of road, the existence of streets adjacent the current street, entrance and exit lanes, merging lanes, crossings of roadways, intersections, bridges, and footpaths and bicycle paths. If deviations are detected via the comparison means, which for instance is disposed in the device for navigation 3 , then errors detected in the digital road map can also be stored in a suitable data medium, so that the next time the vehicle travels through the defective place, the new course of the road will be available. The new course of the road includes for instance the presence of a new construction site or the presence of an altered road sign. The evaluation unit 7 is used to furnish driver information from the navigation data and the road sign recognition data. Upon reports of information by the navigation system to the driver, information from the road sign recognition device is also taken into account, and/or the database of the navigation system is corrected and/or supplemented, as already noted above. The evaluation unit 7 can selectively generate control signals for intervention into a vehicle controller from the coupled system of a road sign recognition system and a navigation system as well. Control signals here include for instance signals for an electronic vehicle brake, an electronic gas pedal and/or for a steering angle controller and/or for triggering a cruise control. The evaluation unit can furthermore ascertain a currently valid speed limit from the road sign recognition data and the navigation data. The evaluation unit is either a separate component of the coupled system 20 , or a constituent part of the devices 2 and/or 3 . The device 2 , the device 3 , and the device 7 can also be totally integrated into a single unit.
The device for road sign recognition can, for Instance, be a video system. A device 2 using a radio system or a laser scanning system can also be employed. A prerequisite of radio methods is that road signs have a built-in, road-sign-specific transmitter, which transmits signals that the road sign recognition device of the vehicle is capable of receiving. In all cases, the information about road signs recognized can be imparted to the driver in a suitable way, for instance acoustically or also optically through warning signals The device 3 for navigation for the driver or vehicle guidance, for instance, includes a memory, in which the location of streets and roads and other information are stored in digital maps. Finding the position of the vehicle within this digital map is typically achieved by a satellite-base positioning method (GPS, for global positioning system), and a GPS module that employs this method is integrated with the navigation device 3 .
FIG. 2 shows a process flow diagram which illustrates various steps of the method for road sign recognition and for navigation, described herein above. | A method and a coupled system for road sign recognition and for navigation is proposed, which enables a bidirectional data transmission between the road sign recognition device and the navigation device. | 6 |
This is a division of application Ser. No. 769,475, filed Feb. 17, 1977, U.S. Pat. No. 4,144,338.
BACKGROUND OF THE INVENTION
Excess secretion of gastric acid can cause indigestion and stomach distress and, if prolonged, can result in ulcer formation. Treatment of excess secretion of gastric acid has heretofore consisted mainly of a bland diet, abstinence from certain foods and the use of antacids to neutralize the gastric acid after it is secreted into the stomach. An improved method of treatment would result from the inhibition of gastric acid secretion. It is thus an object of the present invention to provide compounds which inhibit gastric acid secretion. Another object is to provide methods for the preparation of these compounds. A further object is to provide pharmaceutical formulations for the administration of these compounds. Still another object is to provide a method to inhibit gastric secretion. These and other objects of the present invention will become apparent from the following description.
DESCRIPTION OF THE INVENTION
The compounds of the instant invention are best described by reference to the following structural formula: ##STR1## wherein R is a 6 membered heterocyclic ring system containing 2 or 3 nitrogen heteroatoms, which heterocyclic ring may be optionally substituted with from 1 to 3 of loweralkyl, halo, hydroxy, amino, mono or di-loweralkylamino, loweralkoxy or phenylloweralkoxy;
R 1 and R 2 are independently loweralkyl;
R 3 and R 4 are independently hydrogen or loweralkyl;
X is oxygen or sulfur; and
n is an integer of from 2 to 6, such that the direct linkage between the nitrogen atoms is either two or three carbon atoms.
In the foregoing structural formula R is a heterocyclic moiety consisting of 6 membered heterocycles containing 2 nitrogen atoms such as pyrimidine, pyridazine and pyrazine; and 6 membered heterocycles containing 3 nitrogen atoms referred to as triazines. The heterocyclic group may be optionally substituted with from 1 to 3 of loweralkyl, halo, hydroxy, amino or mono or di-loweralkylamino, loweralkoxy or phenylloweralkoxy.
In the instant specification the term "loweralkyl" is intended to include those alkyl groups of either straight or branched configuration which contain from 1 to 5 carbon atoms. Exemplary of such alkyl groups are methyl, ethyl, propyl, isopropyl, butyl, tertiary butyl, pentyl and the like.
The term "halo" or "halogen" is intended to include the halogen atoms fluorine, chlorine, bromine and iodine.
PREFERRED EMBODIMENTS OF THE INVENTION
The preferred embodiments of the instant invention are realized in the foregoing structural formula wherein:
R is pyrimidinyl, pyridazinyl or pyrazinyl optionally substituted with one to three of methyl, chloro or dimethylamino;
R 1 , R 2 , R 3 and R 4 are independently methyl, ethyl or isopropyl;
n is 2; and
X is oxygen.
Further preferred embodiments are realized when the substituents on the pyrimidinyl group consist of 1 or 2 methyl groups or a chloro and 2 methyl groups. R 1 and R 2 are isopropyl; and R 3 and R 4 are methyl.
The compounds of the present invention are prepared by reacting an appropriately substituted alkylene diamine (II) with an appropriately substituted carbamoyl halide or tricarbamoylhalide (II-A) as described in the following reaction scheme: ##STR2## wherein X, n, R, R 1 , R 2 , R 3 and R 4 are as previously defined, and Hal is a halogen. The reaction is generally carried out in an inert solvent, preferably an aromatic solvent such as benzene at a temperature of from about 20° to 120° C., preferably from about 75° to 100° C. Where the reaction temperature exceeds the boiling point of the reaction solution, the reaction is carried out under pressure. It is preferred to contain in the reaction mixture a scavenger for the hydrohalic acid liberated during the course of the reaction. Non-reactive bases, either inorganic or organic may be employed such as triethylamine, pyridine, sodium carbonate, and the like. The base is required in a single molar equivalent to the acid being liberated, however, excess base has not been found to be detrimental. The product (I) is isolated and purified as the free base or acid addition salt using known techniques. The halogen Hal may be any halogen, however, it is preferred to use chlorine.
Optionally the diamine (II) may be converted into an anion before it is reacted with the carbamoylhalide. Reactive alkali metal compounds such as sodium hydride, lithium aluminum hydride, butyl lithium and the like may be employed. The diamine and the alkali metal compound are combined preferably at room temperature in the foregoing inert solvent in equivalent amounts. If this method is employed the acid scavenger is not needed since an alkali metal halide is the reaction by-product.
The alkylene diamine starting materials (II) for the foregoing processes are made from the appropriately substituted heterocyclic amine wherein the amine function has been activated by a labile activating group. The process is best exemplified by the following reaction scheme: ##STR3##
In the foregoing reaction scheme Hal, R, R 1 , R 2 and n are as previously defined and Z is an activating group. The reaction is carried out in the presence of a strong base such as sodium hydride, butyl lithium, lithium diisopropylamide and the like, in an appropriate, nonreactive solvent such as dimethylformamide, toluene, dioxane, and the like. The reaction temperature may be in the range of -70° to about 160° C. It is preferred, however, that the reaction temperature be maintained at from about 0° to 100° C.
The labile activating group (Z) may be an acyl group readily bonded to the amino group and which may be selectively removed therefrom. Examples of such groups are acetyl, formyl, and the like.
The labile activating group is removed hydrolytically with acidic (such as aqueous mineral acid) or basic (such as alkali hydroxide) reagents, under conditions known to those skilled in this art.
Alternatively the substituted ethylene diamines (II) are prepared from appropriately substituted halo heterocyclic compounds (VI). The halogen substituent is displaced by the unsubstituted amino group of an appropriately substituted alkylene diamine (VII) as shown in the following reaction scheme: ##STR4##
R, R 1 , R 2 , Hal and n are as previously defined.
The reaction is carried out generally in the absence of a solvent at temperatures of from about 50° to 150° C. at from 2 hours to as much as one week for difficult reactions. If a solvent is employed it must have a sufficiently high boiling point to allow the reaction to progress. Dimethylformamide, toluene and xylene are exemplary. Generally the reactions are complete in from about 10 hours to 3 days. For those reactions requiring a prolonged heating period, a catalyst, cuprous chloride, may be employed. The use of catalytic amounts of such catalyst will generally reduce the reaction time to within the preferred range. The products are isolated using techniques known to those skilled in this art.
In addition, the substituted alkylene diamines (II) are prepared from an appropriately alkoxy or alkythio substituted heterocyclic compound (VIII) and the above substituted ethylene diamine (VII) as in the following reaction scheme: ##STR5##
X, R, R 1 , R 2 and n are as previously defined and R 5 is loweralkyl, preferably methyl. The reaction is carried out under the conditions described in the immediately preceding paragraph, and the product is isolated using known techniques.
The compounds of the present invention where X is oxygen (I-A) are prepared by reacting a substituted urea (IX) with the above substituted amino alkyl halide (IV) as follows: ##STR6##
where R, R 1 , R 2 , R 3 , R 4 , Hal and n are as previously defined. The reaction is carried out by first preparing the alkyl metal, preferably lithium salt of the urea (IX) by treating it with lithium hydride in dioxene or butyl lithium in benzene. The reaction is refluxed for from 1 to 16 hours and then cooled and the substituted amino ethylhalide (IV) added and the reaction refluxed for from 2 to 24 hours. The product is isolated using known means.
The substituted urea compounds (IX) are prepared by reacting an appropriately substituted heterocyclic amine (X) with the above substituted carbamoyl halide (II-A) wherein X is oxygen according to the following reaction scheme: ##STR7##
wherein R, R 3 , R 4 , and Hal are as previously defined.
The foregoing reaction is carried out by combining the heterocyclic amine (X) with two moles of an alkali metal hydride such as sodium hydride or lithium hydride in a solvent and refluxing for from 10 minutes to 4 hours. The carbamoyl halide reagent is added and the reaction mixture then maintained at from room temperature to reflux for from 1/2 to 6 hours. Preferred solvents are inert solvents such as benzene, toluene, xylene and the like. It is also preferred to have an acid scavenger such as triethyl amine or pyridine to neutralize the liberated hydrohalic acid.
Further, the compounds of the instant invention (I) wherein one of R 3 or R 4 is hydrogen may be prepared by reacting the above alkylene diamine (II) with an appropriately substituted loweralkyl isocyanate or isothiocyanate as follows: ##STR8## wherein R, R 1 , R 2 , X and n are as previously defined and R 3 is loweralkyl. The reaction is generally carried out at from 0° C. to the boiling point of the isocyanate or isothiocyanate reagent. Preferably the reaction is stirred at room temperature in an aprotic solvent such as benzene, toluene, xylene, tetrahydrofuran and the like, for from 10 hours to one week. Generally the reaction is complete in from 24 to 72 hours.
The compounds of the present invention where X is oxygen and R 3 and R 4 are hydrogen may be prepared by reacting cyanogen bromide with the above alkylene diamine (II): ##STR9## The reaction is generally carried out in a solvent such as tetrahydrofuran with an acid scavenger such as triethyl amine at from 0° to 50° C. for from 6 hours to 3 days. The intermediate cyanamide(XI) is then hydrolized using acid hydrolysis such as aqueous hydrohalic acids at about room temperature for from 5 minutes to 6 hours. Preferably hydrochloric acid is employed at from 4 to 8 normal strength. The product (I-B) is recovered using known techniques.
In addition, the compounds of the present invention wherein X is oxygen (I-A) may be prepared from an appropriately substituted urethane (XII) and ammonia or a substituted amine as follows: ##STR10## wherein R, R 1 , R 2 , R 3 , R 4 , and n are as previously defined and A is a lower alkyl group, a phenyl group or a phenyl group substituted with a non-reactive substituent such as loweralkyl. The unsubstituted phenyl group is preferred. The reaction is optionally carried out in a solvent such as tetrahydrofuran, at from room temperature to the reflux temperature of the reaction mixture. When ammonia is employed, concentrated aqueous ammonia is employed and the solvent may be omitted. In such cases room temperature is adequate to complete the reaction. With substituted amines higher temperatures are beneficial, and occasionally temperatures higher than reflux, in a bomb, are also beneficial. Temperatures to 150° C. may be employed. The reaction is generally complete in from 1 to 24 hours, and the product (I-A) recovered using standard techniques.
The starting urethanes (VII) of the foregoing reaction are prepared from the alkylene diamine (II) and a chloroformate ester (XIII) as follows: ##STR11## wherein R, R 1 , R 2 , R 3 , R 4 , Hal, n, and A are as previously defined. The reaction is carried out in an inert solvent such as tetrahydrofuran, benzene, toluene, xylene, and the like at from 0° to 75° C., preferably room temperature for from 1/2 to 3 days. An acid scavenger such as triethyl amine or pyridine may also be employed, but its use is not required.
The compounds of this invention may be isolated and used as the free base or as a pharmaceutically acceptable acid addition salt. Such salts are formed by reaction of the free base with the desired inorganic or organic acid. The salts are prepared using methods known to those skilled in this art. Exemplary inorganic acids are hydrohalic acids such as hydrochloric or hydrobromic, or other mineral acids such as sulfuric, nitric, phosphoric and the like. Suitable organic acids are maleic, fumaric, tartaric, citric, acetic, benzoic, succinic, isethionic and the like.
The compounds of the present invention in the described dosages may be administered orally, however, other routes such as intra peritoneal, subcutaneous, intramuscular or intravenous may be employed.
The active compounds of the present invention are orally administered, for example, with an inert diluent or with an assimilable edible carrier, or they may be enclosed in hard or soft gelatin capsules, or they may be compressed into tablets, or they may be incorporated directly with the food of the diet. For oral therapeutic administration, the active compounds of this invention may be incorporated with excipients and used in the form of tablets, troches, capsules, elixirs, suppositories, suspensions, syrups, wafers, chewing gum, and the like. The amount of active compound in such therapeutically useful compositions or preparations is such that a suitable dosage will be obtained.
The tablets, troches, pills, capsules and the like may also contain the following: a binder such as gum tragacanth, acacia, corn starch or gelatin; an excipient such as dicalcium phosphate; a disintegrating agent such as corn starch, potato starch, alginic acid and the like; a lubricant such as magnesium stearate; and a sweetening agent such as sucrose, lactose or saccharin may be added or a flavoring agent such as peppermint, oil of wintergreen or cherry flavoring. When the dosage unit form is a capsule, it may contain in addition to materials of the above type, a liquid carrier such as a fatty oil. Various other materials may be present as coatings or to otherwise modify the physical form of the dosage unit, for instance, tablets, pills or capsules may be coated with shellac, sugar or both. A syrup or elixir may contain the active compounds, sucrose as a sweetening agent, methyl and propyl parabens as preservatives, a dye and a flavoring such as cherry or orange flavor. Of course, any material used in preparing any dosage unit form should be pharmaceutically pure and substantially non-toxic in the amounts employed.
EXAMPLE 1
N,N-Dimethyl-N'-(2 -diisopropylaminoethyl)-N'-(4,6-dimethyl-2-pyrimidinyl)urea
A. 2-(2-Diisopropylaminoethylamino)-4,6-dimethyl pyrimidine.
To 600 ml of dry dimethylformamide is added 2-acetamido-4,6-dimethylpyrimidine (34.8 g, 0.21 mole) and 2-diisopropylaminoethyl chloride hydrochloride (48 g, 0.24 mole). The mixture is stirred under nitrogen and sodium hydride (50% in mineral oil) (24.7 g, 0.515 mole) is added in portions over one hour while the temperature is maintained below 45° C. The mixture is then heated at 75°-78° C. for 1/2 hour and then at 90°-95° C. for 31/2 hours. On cooling, ethanol, 25 ml, is added and the solvents removed under reduced pressure. The residue is suspended in 75 ml of 1-propanol and 400 ml of 5 N sodium hydroxide and refluxed with stirring for 18 hours. On cooling the mixture is extracted with methylene chloride. The organic extracts are then extracted with dilute hydrochloric acid. The acid extracts are extracted with hexane and then made alkaline with a molar excess of sodium hydroxide. The crude product is extracted from the basic solution with diethyl ether. The ethereal extracts are washed with saturated sodium chloride solution, dried over sodim sulfate and concentrated under vacuum. The residue is distilled and the product diamine (37.2 g, 0.149 mole) collected at 130°-134° C./0.4 mm; melting point 79.5°-82° C.
B. N,N-Dimethyl-N'-(2-diisopropylaminoethyl)-N'-(4,6-dimethyl-2-pyrimidinylurea
A mixture of 2-(2-diisopropylaminoethylamino)-4,6-dimethyl pyrimidine (17.0 g. 0.068 mole) and sodium hydride (50% in mineral oil) (4.19 g., 0.86 mole) in 175 ml. of dry toluene is stirred under nitrogen at 85°-95° C. for one half hour and then heated under reflux for one half hour. Dimethylcarbamoyl chloride (8.6 g., 0.08 mole) is added and heating under reflux is continued for twenty-four hours. The reaction is cooled and ethanol (10 ml) and sodium hydroxide (75 ml., 3.3 N) are added. The aqueous layer is extracted with methylene chloride and the extracts are dried over sodium sulfate and concentrated to an oil. The oil is distilled at 0.5 mm of Hg and the product boiling at 155°-158° C. is collected.
EXAMPLE 2
N,N-Dimethyl-N'-(2-dimethylaminoethyl)-N'-(2-pyrazinyl) urea Dihydrobromide
To a solution of 2-(2-dimethylaminoethylamino) pyrazine (10 g, 0.0601 mole) and triethylamine (7.2 g, 0.072 mole) in 150 ml of dry benzene is added dimethylcarbamoyl chloride (6.93 g, 0.0645 mole) with stirring. The mixture is refluxed for 18 hours, cooled to room temperature, diluted with 100 ml of ether and filtered. The filtrate is concentrated under vacuum and the residual oil diluted with 250 ml of petroleum ether, treated with charcoal and filtered. Removal of the solvent under reduced pressure gives 13 g (0.055 mole) of an amber oil. The oil is dissolved in 250 m. of ether and gaseous hydrogen bromide is passed into the solution, the precipitated salt is filtered, redissolved in isopropanol and the solution concentrated to dryness under reduced pressure. The solid is triturated with 35 ml of isopropanol, filtered and recrystallized from ethanol to obtain 12.6 g (0.031 mole) of N,N-Dimethyl-N'-(2-dimethylaminoethyl)-N'-(2-pyrazinyl)urea dihydrobromide, melting point 157.5°-159.5° C.
EXAMPLE 3
N,N-Dimethyl-N'-(2-dimethylaminoethyl)-N'-(5,6-dimethyl-2-pyrazinyl)urea Dihydrobromide
A. 2-(2-Dimethylaminoethylamino)-5,6-dimethyl pyrazine.
2-chloro-5,6-dimethylpyrazine (12.8 g, 0.09 mole) is added to unsym-dimethylethylenediamine (26 g, 0.295 mole) containing cuprous chloride (0.25 g) and the mixture is heated for 48 hours in an oil bath maintained at 135°-140° C. On cooling, 50 ml of water and a single molar excess of 10 N sodium hydroxide are added. The mixture is extracted with methylene chloride. The organic extracts are backwashed with saturated sodium chloride solution, dried over sodium sulfate, filtered and concentrated under vacuum. The residual oil is dissolved in hexane, filtered and reconcentrated to obtain the product oil (15.8 g, 0.081 mole).
B. N,N-Dimethyl-N'-(2-dimethylaminoethyl)-N'-(5,6-dimethyl-2-pyrazinyl) urea Dihydrobromide
Following the process of Example 2 using 2-(2-dimethylaminoethylamino)-5,6-dimethyl pyrazine there is obtained N,N-Dimethyl-N'-(2-dimethylaminoethyl)-N'-(5,6-dimethyl-2-pyrazinyl) urea dihydrobromide, melting point 188° C.
EXAMPLE 4
N,N-Dimethyl-N'-(2-dimethylaminoethyl)-N'-(6-dimethylamino-2-pyrazinyl)urea Dihydrochloride
A. 2-Chloro-6-dimethylaminopyrazine
Cuprous chloride (50 mg) is added to a solution of dimethylamine (36 g, 0.8 mole) in 260 ml of isopropanol. 2,6-Dichloropyrazine (49.9 g, 0.33 mole) is added to the mixture with stirring and cooling to maintain the temperature at 35°-40° C. After 3/4 hr. the cooling bath is removed and the reaction mixture is stored at ambient temperature for 16 hours and finally at 42°-48° C. for 3 hours. The solvent is removed under vacuum and the residue is dissolved in dilute hydrochloric acid. The aqueous solution is extracted with ether and then made basic with solid sodium bicarbonate and extracted with methylene chloride. The organic extracts are washed with brine, dried over sodium sulfate and concentrated under vacuum to obtain 49 g of product, melting point 46°-8° C.
B. 2-(2-Dimethylaminoethylamino)-6-dimethylaminopyrazine
Following the process of Example 3A using 2-chloro-6-dimethylaminopyrazine there is obtained, 2-(2-dimethylaminoethylamino)-6-dimethylaminopyrazine.
C. N,N-Dimethyl-N'-(2-dimethylaminoethyl)-N'-(6-dimethylamino-2-pyrazinyl)urea Dihydrochloride
2-(2-Dimethylaminoethylamino)-6-dimethylaminopyrazine (16.5 g, (0.079 mole) is dissolved in 150 ml dry toluene under nitrogen and sodium hydride (50% in mineral oil) (4.17 g, 0.087 mole) is added. The mixture is heated with stirring at 90°-98° C. for 1/2 hour and then refluxed for 1/2 hour. After cooling to 35° C. dimethylcarbamoylchloride (9.35 g, 0.087 mole) is added and the mixture is refluxed for 3 hours and cooled. Ethanol, 5 ml is added and the solvents are removed under reduced pressure. The residue is dissolved in dilute hydrochloric acid and extracted with ether. The aqueous layer is made alkaline with aqueous sodium hydroxide with a cooling bath to maintain the temperature below 35° C. The alkaline solution is extracted with methylene chloride. The organic extracts are washed with saturated sodium chloride solution, dried over sodium sulfate and concentrated under vacuum. The residual oil is dissolved in isopropanol, 50 ml and diethyl ether, 300 ml and then gaseous hydrogen chloride is passed into the solution. The product dihydrochloride crystallizes, is filtered, and washed with 100 ml of 1:1 acetone: isopropanol. Recrystallization from 150 ml isopropanol and 75 ml of diethyl ether yields 8 g (0.029 mole) of the dihydrochloride salt, melting point 189° C. (dec).
EXAMPLE 5
N,N-Dimethyl-N'-(2-dimethylaminoethyl)-N'-(4,6-dimethyl-2-pyrimidinyl)urea Hydrochloride
A. 2-(2-Dimethylaminoethylamino)-4,6-dimethylpyrimidine
Following the procedure of Example 1-A using 2-dimethylaminoethyl chloride hydrochloride, there is obtained 2-(2-dimethylaminoethyl)-4,6-dimethylpyrimidine boiling at 90°-100° C. at 0.5 mm.
B. N,N (Dimethyl)-N'-(2-dimethylaminoethyl)-N'-(4,6-dimethyl-2-pyrimidinyl) urea Hydrochloride
Following the procedure of Example 2 using 2-(2-dimethylaminoethylamino)-4,6-dimethylpyrimidine and neutralizing with hydrogen chloride instead of hydrogen bromide, N,N (dimethyl-N'-(2-dimethylaminoethyl)-N'-(4,6-dimethyl-2-pyrimidinyl) urea hydrochloride is obtained having a melting point of 177°-179° C.
EXAMPLE 6
N,N-Dimethyl-N'-(2-dimethylaminoethyl)-N'-(2-pyrimidinyl) urea Hydrochloride
Following the procedure of Example 2 using 2-(2-dimethylaminoethylamino) pyrimidine and neutralizing with hydrogen chloride instead of hydrogen bromide, N,N-dimethyl-N'-(2-dimethylaminoethyl)-N'-(2-pyrimidinyl) urea hydrochloride is obtained having a melting point of 182°-184° C.
EXAMPLE 7
N,N-Dimethyl-N'-(2-dimethylaminoethyl)-N'-(4-methyl-6-dimethylamino-2-pyrimidinyl)urea Dihydrobromide
A. 2-Amino-4-methyl-6-dimethylaminopyrimidine
2-Amino-4-methyl-6-chloropyrimidine (52 g, 0.36 mole) is heated at 160° C. for 18 hours with ethanol and an equimolar amount of dimethylamine in a pressure vessel. The reaction mixture is evaporated in vacuo taken up in 200 ml. of water containg 50 ml. 10 N sodium hydroxide and 300 ml. of methylene chloride. The mixture is extracted with methylene chloride and the organic layer dried and evaporated to dryness in vacuo affording 46 g of 2-amino-4-methyl-6-dimethylaminopyrimidine with a melting point of 172°-174° C.
B. 2-Acetamido-4-methyl-6-dimethylamino pyrimidine
A mixture of 44 g. (0.29 moles) of 2-amino-4-methyl-6-dimethylaminopyrimidine (46 g. (0.45 moles) of acetic anhydride and 100 ml. toluene is stirred at reflux for 4 hours. The reaction mixture is cooled, 25 ml. of ethanol and 100 ml. of hexane are added and the mixture is filtered. The filtrate is evaporated in vacuo and the residue combined with 200 ml. of methylene chloride and 100 ml. of water containing excess ammonium hydroxide. The organic layer is separated and the aqueous layer extracted with methylene chloride. The combined extracts are dried with sodium sulfate and concentrated to a small volume and filtered. The filtrate is concentrated to dryness and taken up in 50 ml. of methylene chloride and filtered. The solid materials from both filtrations are combined affording 48.4 g. of 2-acetamido-4-methyl-6-dimethylamino pyrimidine melting point 153°-157° C.
C. 2-(2-Dimethylaminoethylamino)-4-methyl-6-dimethylaminopyrimidine.
Following the procedure of Example 1, Part A 2-acetamido-4-methyl-6-dimethylaminopyrimidine and 2-dimethylaminoethyl chloride hydrochloride, 2-(2-dimethylaminoethylamino)-4-methyl-6-dimethylaminopyrimidine is obtained with a boiling point of 120°-124° C. at 0.03 mm.
D. N,N-Dimethyl-N'-(2-dimethylaminoethyl)-N'-(4-methyl-6-dimethylaminopyrimidinyl) urea Dihydrobromide
Following the procedure of Example 4, Part C using 2-(2-dimethylaminoethylamino)-4-methyl-6-dimethylaminopyrimidine, and hydrogen bromide instead of hydrogen chloride for the final salt formation N,N-dimethyl-N'-(2-dimethylaminoethyl)-N'-(4-methyl-6-dimethylamino-2-pyrimidinyl)urea dihydrobromide is obtained with a melting point of 213° C.
EXAMPLE 8
N,N-Dimethyl-N'-(2-dimethylaminoethyl)-N'-(6-chloro-3-pyridazinyl)urea Hydrochloride
A. 3-(2-Dimethylaminoethylamino)-6-chloropyridazine
Following the procedure of Example 3, Part A using 3,6-dichloropyridazine there is obtained 3-(2-dimethylaminoethylamino)-6-chloropyridazine with melting point of 86°-92° C.
B. N,N-Dimethyl-N'-(2-dimethylaminoethyl)-N'-(6-chloro-3-pyridazinyl)urea Hydrochloride
Following the procedure of Example 2 using 3-(2-dimethylaminoethylamino)-6-chloropyridazine and forming the hydrohalide salt of the product with hydrogen chloride there is obtained N,N-dimethyl-N'-(2-dimethylaminoethyl)-N'-(6-chloro-3-pyridazinyl) urea hydrochloride with melting point of 194° C.
EXAMPLE 9
N,N-Dimethyl-N'-(2-dimethylaminoethyl)-N'-(3-pyridazinyl) urea Dihydrochloride
N,N-Dimethyl-N'-(2-dimethylaminoethyl)-N'-(6-chloro-3-pyridazinyl) urea hydrochloride (10.5 g, 0.034 mole) (Example 8) and 1.5 g of 5% palladium on carbon catalyst are added to a mixture of 35 ml of 2 N sodium hydroxide in 250 ml of ethyl alcohol. Treatment with hydrogen is performed in a Parr apparatus at 40-50 lbs. per sq. in. pressure and ambient temperature. The catalyst is removed by filtration, the filtrate is concentrated under reduced pressure, water is added and the mixture is extracted with benzene. The extracts are concentrated, the residue is dissolved in ether, hydrogen chloride is added and N,N-dimethyl-N'-(2-dimethylaminoethyl)-N'-(3-pyridazinyl) urea dihydrochloride melting at 187.5°-188.5° C. is obtained.
EXAMPLE 10
N,N-Dimethyl-N'-(2-dimethylaminoethyl)-N'-(2,6-dimethyl-4-pyrimidinyl) urea Dihydrochloride
A. 4-(2-Dimethylaminoethylamino)-2,6-dimethyl-pyrimidine
Following the procedure of Example 3, Part A using 4-chloro-2,6-dimethylpyrimidine, 4-(2-dimethylaminoethylamino)-2,6-dimethylpyrimidine is obtained as an oil which is vacuum distilled and boils at 108°-111° C. at 0.5 mm of Hg.
B. N,N-Dimethyl-N'-(2-dimethylaminoethyl)-N'-(2,6-dimethyl-4-pyrimidinyl)urea Dihydrochloride
Following the procedure of Example 2 using 4-(2-dimethylaminoethylamino)-2,6-dimethylpyrimidine and forming the hydrohalide salt of the product with hydrogen chloride there is obtained N,N-dimethyl-N'-(2-dimethylaminoethyl)-N'-(2,6-dimethyl-4-pyrimidinyl) urea dihydrochloride with melting point of 220°-222° C.
EXAMPLE 11
N,N-Dimethyl-N'-(2-dimethylaminoethyl)-N'-(3,5,6-trimethyl-2 pyrazinyl) urea Dihydrochloride
A. 2-(2-Dimethylaminoethylamino)-3,5,6-Trimethylpyrazine
Following the procedure of Example 3, Part A using 2-chloro-3,5,6-trimethylpyrazine, 2-(2-dimethylaminoethylamino)-3,5,6-trimethylpyrazine is obtained.
B. N,N-Dimethyl-N'-(2-dimethylaminoethyl)-N'-(3,5,7-trimethyl-2-pyrazinyl) urea Dihydrochloride
Following the procedure of Example 2 usin 2-(2-dimethylaminoethylamino)-3,5,6-trimethylpyrazine, and forming the hydrohalide salt of the product with hydrogen chloride, N,N-dimethyl-N'-(2-dimethylaminoethyl)-N'-(3,5,6-trimethyl-2-pyrazinyl) urea dihydrochloride is obtained with a melting point of 224° C.
EXAMPLE 12
N,N-Dimethyl-N'-(2-dimethylaminoethyl)-N'-(6-methyl-2-pyrazinyl) urea Dihydrobromide
A. 2-(2-Dimethylaminoethylamino)-6-methylpyrazine
Following the procedure of Example 3, Part A using 2-chloro-6-methylpyrazine, 2-(2-dimethylaminoethylamino)-6-methylpyrazine is obtained as an oil.
B. N,N-Dimethyl-N'-(2-dimethylaminoethyl)-N'-(6-methyl-2-pyrazinyl) urea Dihydrobromide
Following the procedure of Example 2, using 2-(2-dimethylaminoethylamino)-6-methylpyrazine, N,N-dimethyl-N'-(2-dimethylaminoethyl)-N'-(6-methyl-2-pyrazinyl) urea dihydrobromide is obtained with a melting point of 189° C.
EXAMPLE 13
N,N-Dimethyl-N'-(2-dimethylaminoethyl)-N'-(4-pyrimidinyl) urea Dihydrochloride
A. 4-(2-Dimethylaminoethylamino) pyrimidine
A solution of 4-methoxypyrimidine (12.9 g, 0.117 mole) and unsym-dimethylethylene diamine (20.7 g, 0.23 mole) in 40 ml of xylene is heated under reflux for 64 hours. The reaction is concentrated and the oil is distilled at 15 mm of Hg. 4-(2-Dimethylaminoethylamino) pyrimidine, boiling at 164°-169° C., is collected.
B. N,N-Dimethyl-N'-(2-dimethylaminoethyl)-N'-(4-pyrimidinyl) urea Dihydrochloride
Following the procedure of Example 2, using 4-(2-dimethylaminoethylamino)pyrimidine and forming the hydrohalide salt of the product with hydrogen chloride, there is obtained N,N-dimethyl-N'-(2-dimethylaminoethyl)-N'-(4-pyrimidinyl)urea dihydrochloride with a melting point of 206°-208° C.
EXAMPLE 14
N,N-Dimethyl-N'-(2-diisopropylaminoethyl)-N'-(2-pyrazinyl) urea Dihydrobromide
A. 2-(2-Diisopropylaminoethylamino)pyrazine
Following the procedure of Example 3, Part A using 2-chloropyrazine and unsym-diisopropylethylenediamine, 2-(2-diisopropylaminoethylamino)pyrazine is obtained with a boiling range of 180°-190° C. upon distillation at 17 mm. of Hg.
B. N,N-Dimethyl-N'-(2-diisopropylaminoethyl)-N'-(2-pyrazinyl)urea Dihydrobromide
Following the procedure of Example 4, Part C using 2-(2-diisopropylaminoethylamino)pyrazine and forming the hydrohalide salt with hydrogen bromide, N,N-dimethyl-N'-(2-diisopropylaminoethyl)-N'-(2-pyrazinyl)urea dihydrobromide with melting point of 186°-188° C. is obtained.
EXAMPLE 15
N,N-Dimethyl-N'-(2-dimethylaminoethyl)-N'-(6-chloro-2-pyrazinyl) urea Hydrobromide
A. 2-(2-Diethylaminoethylamino)-6-Chloropyrazine
Following the procedure of Example 3, Part A using 2,6-dichloropyrazine, 2-(2-dimethylaminoethylamino)-6-chloropyrazine is obtained as an oil.
B. N,N-Dimethyl-N'-(2-dimethylaminoethyl)-N'-(6-chloro-2-pyrazinyl)urea Hydrobromide
Following the procedure of Example 2, using 2-(2-dimethylaminoethylamino)-6-chloropyrazine, N,N-dimethyl-N'-(2-dimethylaminoethyl)-N'-(6-chloro-2-pyrazinyl)urea hydrobromide with a melting point of 159.5°-161° C. is obtained.
EXAMPLE 16
N,N-Dimethyl-N'-(2-dimethylaminoethyl)-N'-(3,6-dimethyl-2-pyrazinyl)urea
A. 2-(2-Dimethylaminoethylamino)-3,6-dimethylpyrazine
Following the procedure of Example 3, Part A using 2-chloro-3,6-methylpyrazine, 2-(2-dimethylaminoethylamino)-3,6-dimethylpyrazine is obtained as an oil which is distilled at 0.5 mm of Hg. and collected at a boiling point of 89.5°-91.5° C.
B. N,N-Dimethyl-N'-(2-dimethylaminoethyl)-N'-(3,6-dimethyl-2-pyrazinyl)urea
Following the procedure of Example 2 using 2-(2-dimethylaminoethylamino)-3,6-dimethylpyrazine and omitting hydrohalide salt formation, N,N-dimethyl-N'-(2-dimethylaminoethyl)-N'-(3,6-dimethyl-2-pyrazinyl)urea is obtained with melting point of 96°-98° C.
EXAMPLE 17
N,N-Dimethyl-N'-(2-dimethylaminoethyl)-N'-[3-(1,2,4-triazinyl)] urea Hydrochloride
A. 3-(2-Dimethylaminoethylamino)-1,2,4-triazine
3-Methylthio-1,2,4-triazine (19.1 g, 0.15 mole) and unsym-dimethylethylene diamine (35.2 g, 0.40 mole) are dissolved in 100 ml of isopropyl alcohol and the mixture is heated under reflux in a nitrogen atmosphere for five days. The solvent is removed under reduced pressure and the residue is distilled at 0.5 mm of Hg. 3-(2-Dimethylaminoethylamino)-1,2,4-triazine is collected at 168°-169° C.
B. N,N-Dimethyl-N'-(2-dimethylaminoethyl)-N'-[3-(1,2,4-triazinyl)]urea Hydrochloride
Following the procedure of Example 2, using 3-(2-dimethylaminoethylamino)-1,2,4-triazine and forming the hydrohalide salt of the product with hydrogen chloride, there is obtained N,N-dimethyl-N'-(2-dimethylaminoethyl)-N'-[3-(1,2,4-triazinyl)] urea hydrochloride with melting point of 192°-193° C.
EXAMPLE 18
N,N-Dimethyl-N'-(2-diisopropylaminoethyl)-N'-(4-methyl-6-benzyloxy-2-pyrimidinyl)urea
A. 2-Amino-4-methyl-6-benzyloxypyrimidine
2-Amino-4-methyl-6-hydroxypyrimidine (62.5 g, 0.50 mole) is dissolved in 500 ml of dimethylformamide and sodium hydride (0.5 mole) is added over a 1 hour period under a nitrogen atmosphere. The mixture is heated at 75° C. for 11/2 hours. Benzyl chloride (69.3 g, 0.55 moles) is then added over 15 minutes and the mixture is heated at 90° C. and stirred for 11/2 hours. After cooling, the reaction mixture is filtered and concentrated under vacuum to an oil from which 2-amino-4-methyl-6-benzyloxypyrimidine melting at 108°-109.5° C. is obtained by crystallization from n-butyl chloride.
B. 2-Acetamido-4-methyl-6-benzyloxypyrimidine
Acetic anhydride (15.3 g, 0.15 mole) is added to a stirred suspension of 2-amino-4-methyl-6-benzyloxypyrimidine (23.6 g, 0.11 mole) in 150 ml of benzene. The mixture is heated at reflux for 4 hours. It is cooled, neutralized with aqueous sodium carbonate and the benzene layer separated. The benzene solution is concentrated under vacuum to an oil from which 2-acetamido-4-methyl-6-benzyloxy-pyrimidine melting at 121°-122° C. is isolated by crystallization from hexane n-butyl chloride.
C. 2-(2-Diisopropylaminoethylamino)-4-methyl-6-hydroxypyrimidine
Following the procedure of Example 1 part A using 2-acetamido-4-methyl-6-benzyloxypyrimidine and conducting the final hydrolysis with 3 N hydrochloric acid, there is obtained 2-(2-diisopropylaminoethylamino)-4-methyl-6-hydroxypyrimidine.
D. 2-(2-Diisopropylaminoethylamino)-4-methyl-6-benzyloxypyrimidine
Following the procedure of part A using 2-(2-diisopropylaminoethylamino)-4-methyl-6-hydroxypyrimidine, 2-(2-diisopropylaminoethylamino)-4-methyl-6-benzyloxypyrimidine is obtained as an oil which is distilled at 0.6 mm of Hg and is collected at 198°-200° C.
E. N,N-Dimethyl-N'-(2-diisopropylaminoethyl)-N'-(4-methyl-6-benzyloxy-2-pyrimidinyl)urea
Under a nitrogen atmosphere, n-butyl lithium solution (22.2 ml, 0.036 mole) is added dropwise with stirring to a solution of 2-(2-diisopropylaminoethylamino)-4-methyl-6-benzyloxypyrimidine (12.4 g, 0.036 mole) in 75 ml. of dry benzene at 25° to 30° C. with occasional cooling over a 20 minute period. After stirring an additional 3/4 hour, dimethylcarbamoyl chloride (4.3 g, 0.04 mole) is added dropwise over 15 minutes. The reaction is stirred at room temperature for 16 hours. After cooling, the reaction mixture is treated with water and the benzene layer is separated. The crude product is extracted into 1 N-hydrochloric acid. This aqueous solution is basified and the product is extracted into ether, dried over sodium sulfate, filtered and concentrated in vacuo. Chromatography on silica gel eluting with 25% methanol, 75% chloroform yields N,N-dimethyl-N'-(2-diisopropylaminoethyl)-N'-(4-methyl-6-benzyloxy-2-pyrimidinyl)urea.
EXAMPLE 19
N,N-Dimethyl-N'-(2-diisopropylaminoethyl)-N'-(4-methyl-6-hydroxy-2-pyrimidinyl)urea Hydrochloride
N,N-Dimethyl-N'-(2-diisopropylaminoethyl)-N'-(4-methyl-6-benzyloxy-2-pyrimidinyl)urea (3.4 g, 0.0082 mole) is dissolved in 50 ml of ethyl alcohol and 0.3 g of 10% palladium on carbon catalyst is added. Hydrogenolytic debenzylation is conducted at 301 lbs. per sq. in., the catalyst is removed, hydrogen chloride is added and N,N-dimethyl-N'-(2-diisopropylaminoethyl)-N'-(4-methyl-6-hydroxy-2-pyrimidinyl)urea hydrochloride melting (dec.) at 198°-208° C. is obtained.
EXAMPLE 20
N,N-Dimethyl-N'-(2-dimethylaminoethyl)-N'-(5-chloro-2-pyrimidinyl)urea Dihydrobromide
A. 2-(2-Dimethylaminoethylamino)-5-chloropyrimidine
Following the procedure of Example 1 part A and replacing the 2-acetamido-4,6-dimethylpyrimidine and 2-diisopropylaminoethyl chloride hydrochloride with equivalent amounts of 2-acetamido-5-chloropyrimidine and 2-dimethylaminoethyl chloride hydrochloride respectively, there is obtained 2-(2-dimethyl-aminoethylamino)-5-chloropyrimidine which is distilled at 115°-118° C. at 1.8 mm of mercury.
B. N,N-Dimethyl-N'-(2-dimethylaminoethyl)-N'-(5-chloro-2-pyrimidinyl)urea Dihydrobromide
Following the procedure of Example 18 part E using 2-(2-dimethylaminoethylamino)-5-chloropyrimidine and forming the hydrohalide salt of the product with hydrogen bromide, N,N-dimethyl-N'-(2-dimethylaminoethyl)-N'-(5-chloro-2-pyrimidinyl)urea dihydrobromide melting at 182° C. is obtained.
EXAMPLE 21
N,N-Dimethyl-N'-(2-diisopropylaminoethyl)-N'-(4,6-dimethyl-5-chloro-2-pyrimidinyl)urea Hydrochloride
A. N,N-Dimethyl-N'-(4,6-dimethyl-5-chloro-2-pyrimidinyl)urea
Sodium hydride (6 g, 55%, 0.137 mole) is added to a mixture of 2-amino-4,6-dimethyl-5-chloropyrimidine (19.5 g, 0.125 mole) in 250 ml of toluene. The mixture, under a nitrogen atmosphere is heated to reflux and stirred for one hour. Another portion of sodium hydride (6 g, 55%, 0.137 mole) is added and after two hours of reflux, dimethyl carbamoyl chloride (13.9 g, 0.125 mole) is added. After one hours of reflux the reaction is cooled, water is added, the toluene is removed by vacuum concentration and the product is extracted into petroleum ether from which it is crystallized by evaporation. N,N-Dimethyl-N'-(4,6-dimethyl-5-chloro-2-pyrimidinyl)urea melting at 127°-129° C. is obtained.
B. N,N-Dimethyl-N'-(2-diisopropylaminoethyl)-N'-(4,6-dimethyl-5-chloro-2-pyrimidinyl)urea Hydrochloride
The product of part A (12.8 g, 0.056 mole) is dissolved in 185 ml of dioxane, lithium hydride (1.16 g, 0.146 mole) is added and the mixture is stirred under nitrogen at reflux. Diisopropylaminoethyl chloride hydrochloride (11.2 g, 0.056 mole) is added and the mixture is heated under reflux for eight hours. Water (20 ml) and isopropyl alcohol (20 ml) are added and the mixture is concentrated in vacuo. Water (100 ml) and saturated sodium carbonate are added and the mixture is extracted with methylene. The combined extract is concentrated, ethanolic hydrogen chloride is added and N,N-dimethyl-N'-(2-diisopropylaminoethyl)-N-(4,6-dimethyl-5-chloro-2-pyrimidinyl)urea hydrochloride is crystallized from ether. The melting point is 202°-204° C.
EXAMPLE 22
N-(2-Diisopropylaminoethyl)-N-(4,6-dimethyl-2-pyrimidinyl) urea
A. Phenyl N-(2-diisopropylaminoethyl)-N-(4,6-dimethyl-2-pyrimidinyl) carbamate Hydrochloride
A solution of 2-(2-diisopropylaminoethylamino)-4,6-dimethylpyrimidine (12.5 g, 0.05 mole) in 50 ml of benzene is added to a solution of phenyl chloroformate in 50 ml of benzene. After 72 hours, the solid product is collected and recrystallized from acetone to give phenyl N-(2-diisopropylaminoethyl)-N-(4,6-dimethyl-2-pyrimidinyl) carbamate hydrochloride melting at 190°-202° C.
B. N-(2-Diisopropylaminoethyl)-N-(4,6-dimethyl-2-pyrimidinyl) urea
Concentrated ammonia (10 ml) is added to a solution of phenyl N-(2-diisopropylaminoethyl)-N-(4,6-dimethyl-2-pyrimidinyl) carbamate hydrochloride (7.33 g, 0.018 mole) in 50 ml of tetrahydrofuran and the mixture is allowed to stand for twenty-four hours. It is concentrated, water and chloroform are added to the residue, the chloroform is separated and concentrated. Crystallization of the residue from hexane yields N-(2-diisopropylaminoethyl)-N-(4,6-dimethyl-2-pyrimidinyl)urea melting at 134°-136° C.
EXAMPLE 23
N-(2-Dimethylaminoethyl)-N-(2-pyrazinyl)urea
A. N-(2-Dimethylaminoethyl)-N-(2-pyrazinyl)cyanamide
A solution of cyanogen bromide (15.9 g, 0.150 mole) in 75 ml of tetrahydrofuran is added to a solution of 2-(2-dimethylaminoethylamino) pyrazine (16.6 g, 0.1 mole) and triethylamine (20.9 g, 0.15 mole) in 100 ml of tetrahydrofuran. After 72 hours, dilute sodium hydroxide is added and the mixture is extracted with ether. The extracts are concentrated and the residue is distilled under reduced pressure. N-(2-Dimethylaminoethyl)-N-(2-pyrazinyl) cyanamide boiling at 130°-132° C. at 0.7 mm if collected.
B. N-(2-Dimethylaminoethyl)-N-(2-pyrazinyl)urea
N-(2-Dimethylaminoethyl)-N-(2-pyrazinyl) cyanamide (2.83 g, 0.015 mole) is dissolved in 20 ml of 6 N hydrochloric acid. After one hour, the mixture is made alkaline with concentrated sodium hydroxide and concentrated. The residue is extracted with ether which is concentrated. The residue is crystallized from butyl chloride and N-(2-dimethylaminoethyl)-N-(2-pyrazinyl)urea melting at 105°-108° C. is obtained.
EXAMPLE 24
N,N-Dimethyl-N'-(2-dimethylaminoethyl)-N'-[5,6-dimethyl-3-(1,2,4-triazinyl)]urea Hydrochloride
A. 3-(2-Dimethylaminoethylamino)-5,6-dimethyl-1,2,4-triazine
Following the procedure of Example 17 part A using 3-methylthio-5,6-dimethyl-1,2,4-triazine, 3-(2-dimethylaminoethylamino)-5,6-dimethyl-1,2,4-triazine is obtained with a melting point of 46°-49° C.
B. N,N-Dimethyl-N'-(2-dimethylaminoethyl)-N'-[5,6-dimethyl-3-(1,2,4-triazinyl)]urea Hydrochloride
Following the procedure of Example 2 using 3-(2-dimethylaminoethylamino) 5,6-dimethyl-1,2,4-triazine and forming the hydrohalide salt of the product with hydrogen chloride, there is obtained N,N-dimethyl-N'-(2-dimethylaminoethyl)-N'-[5,6-dimethyl-3-(1,2,4-triazinyl)]urea hydrochloride melting at 173°-175° C.
EXAMPLE 25
N-(2-Dimethylaminoethyl)-N-(4,6-dimethyl-2-pyrimidinyl) N'-ethylurea Hydrochloride
A solution of 11.6 g (0.06 mole) of 2-(2-dimethylaminoethylamino)-4,6-dimethylpyrimidine in 150 ml. of benzene is dried by azeotropic distillation. The solution is then treated with 8.5 g (0.120 mole) of ethyl isocyanate and heated at reflux for 24 hours. After removal of the solvent, the residue is dissolved in 100 ml of ethyl ether and the solution is neutralized with 3 ml of 10.6 N hydrogen chloride in ethanol. The resulting white precipitate is recrystallized from isopropanol to give N-(2-dimethylaminoethyl)-N-(4,6-dimethyl-2-pyrimidinyl)-N'-ethylurea hydrochloride.
EXAMPLE 26
N,N-Dimethyl-N'-(2-dimethylaminoethyl)-N'-(3,6-dimethyl-2-pyrazinyl) thiourea
A solution of 11.6 g (0.06 mole) of 2-dimethylaminoethylamino-3,6-dimethylpyrazine in 175 ml of dry tetrahydrofuran is allowed to react with 40.8 ml (0.066 mole) of 1.62 M butyl lithium in hexane. Then 8.16 g (0.066 mole) of dimethyl thiocarbamoyl chloride in 75 ml of dry tetrahydrofuran is added over 20 minutes with ice cooling. The reaction mixture is allowed to stir overnight at room temperature. After quenching with water, the product is extracted into ether. The ether extract is washed with water and saturated sodium chloride solutions and dried over magnesium sulfate. The crude product is obtained as a brown oil.
The crude product is chromatographed on silica gel, eluting with 5% methanol in chloroform. After combining the appropriate fractions, the solvent is removed in vacuum and the residue distilled through a short path still. There is obtained N,N-dimethyl-N'-(2-dimethylaminoethyl)-N'-(3,6-dimethyl-2-pyrazinyl) thiourea.
EXAMPLE 27
N-(2-Dimethylaminoethyl)-N-(2-pyrazinyl)-N'-methylthiourea Hydrochloride
Following the procedure of Example 25 using 2-(2-dimethylaminoethylamino)pyrazine and methylisothiocyanate, there is obtained N-(2-dimethylaminoethyl)-N-(2-pyrazinyl)-N'-methylthiourea hydrochloride.
EXAMPLE 28
N,N-Dimethyl-N'-(2-methyl-3-dimethylaminopropyl)-N'-(5-chloro-2-pyrimidinyl)urea
A. 2-(2-Methyl-3-dimethylaminopropylamino)-5-chloropyrimidine
Following the procedure of Example 1 part A using 2-acetamido-5-chloropyrimidine and 2-methyl-3-dimethylaminopropyl chloride hydrochloride, there is obtained 2-(2-methyl-3-dimethylamino-propylamino)-5-chloropyrimidine.
B. N,N-Dimethyl-N'-(2-methyl-3-dimethylaminopropyl)-N'-(5-chloro-2-pyrimidinyl)urea
Following the procedure of Example 1 part B using 2-(2-methyl-3-dimethylaminopropylamino)-5-chloropyrimidine there is obtained N,N-dimethyl-N'-(2-methyl-3-dimethylaminopropyl)-N'-(5-chloro-2-pyrimidinyl)urea.
EXAMPLE 29
N,N-Dimethyl-N'-(2-methyl-2-dimethylaminopropyl)-N'-(4-methyl-6-dimethylamino-2-pyrimidinyl)urea
A. 2-(2-Methyl-2-dimethylaminopropylamino)-4-methyl-6-dimethylaminopyrimidine
Following the procedure of Example 1 part A using 2-acetamido-4-methyl-6-dimethylaminopyrimidine and 2-methyl-2-dimethylaminopropyl chloride hydrochloride, there is obtained 2-(2-methyl-2-dimethylaminopropylamino)-4-methyl-6-dimethyl minopyrimidine.
B. N,N-Dimethyl-N'-(2-methyl-2-dimethylaminopropyl)-N'-(4-methyl-6-dimethylamino-2-pyrimidinyl)urea
Following the procedure of Example 1 part B using 2-(2-methyl-2-dimethylaminopropylamino)-4-methyl-6-dimethylaminopyrimidine, there is obtained N,N-dimethyl-N'-(2-methyl-2-dimethylaminopropyl)-N'-(4-methyl-6-dimethylamino-2-pyrimidinyl)urea.
EXAMPLE 30
N,N-Diethyl-N'-(2-diisopropylaminoethyl)-N'-(2-pyrazinyl) urea Hydrochloride
Following the procedure of Example 4 part C using 2-(2-diisopropylaminoethylamino)pyrazine and diethylcarbamoylchloride, there is obtained N,N-diethyl-N'-(2-diisopropylaminoethyl)-N'-(2-pyrazinyl)urea hydrochloride. | Organic chemical compounds based upon the urea molecule are disclosed which have potent gastric secretion inhibitory properties. The urea is substituted with a 6 membered heterocyclic substituent containing 2 or 3 heteroatoms, and also with a substituted amino alkyl group. Further substitution is also possible. The compounds have profound effects on the inhibition of gastric secretions in the gastro-intestinal tract, and compositions for such uses are also disclosed. | 2 |
The work described herein was partially funded under Grant CA-16049-05-12 awarded by the Division of Cancer Treatment, NCI, DHHS and by the Arizona Disease Control Research Commission.
INTRODUCTION
The present invention relates to the isolation and structural eludication of a new cyclo-octapeptide denominated "Hymenistatin 1". Hymenistatin 1 was isolated from the South Pacific Ocean sponge Hymeniacidon and found to demonstrate utility as a tumor growth inhibitor when measured by the P388 murine leukemia cell line (N.C.I. Protocol). Hymenistatin 1 has the general chemical structure: ##STR2##
BACKGROUND OF THE INVENTION
Early investigations directed at isolation of antineoplastic constituents from marine sponges initially led to the geodiastatin proteins and later to a series of pyrrolactams. More recently, other promising leads have been detected in the Porifera phylum, including antineoplastic peptides. To date, only a few new amino acids, peptides and antineoplastic substances have been isolated from marine sponges. One of the Hymeniacidon sp. (Demospongiae Class) which was collected in Palau in 1979 yielded aqueous 2-propanol-methylene chloride extracts which demonstrated a 30% life extension against the U.S. National Cancer Institute's murine P388 lymphocytic leukemia (PS system). Bioassay directed isolation using the PS leukemia data led to isolation and identification of a new cytostatic peptide, herein denominated designated "Hymenistatin 1". The cyclo-octapeptide was isolated and subjected to structural elucidation.
In the continuing effort to locate and define various natural and synthetic substances for treatment of one or more varieties of cancer, research chemists continue to look at natural flora and fauna in an attempt to isolate and identify new substances which exhibit tumor growth inhibitory or antineoplastic activity while minimizing, if not totally eliminating, some of the severe side effects accompanying known chemotherapeutic agents.
It is in the further pursuit of these goals that marine species heretofore ignored are now being examined to determine whether they contain constituents which, when isolated, will exhibit useful biological properties such, for instance, as inhibiting tumor growth.
Accordingly, a principal object of the present invention is to provide new agents which possess useful biological properties.
Another object of the present invention is to provide methods and procedures for isolating antineoplastic substances from marine life in a form whereby they may be readily and usefully employed in the therapeutic treatment and management of one or more types of cancer which occur in human hosts and are manifested by malignant tumor growth.
A further object of the present invention is the provision of unique means and methods of isolating and elucidating the structure of a new cyclo-octapeptide from the South Pacific sponge Hymeniacidon sp.
These and still further objects of the present invention as shall hereinafter appear are readily fulfilled by the present invention in a remarkably unexpected manner as will be readily discerned from the following detailed description of exemplary embodiments thereof.
BRIEF SUMMARY OF THE INVENTION
The continuing search for biologically active substances from marine biotica in the South Pacific has led to the discovery of a new cyclo-octapeptide, herein denominated "Hymenistatin 1", which exhibits tumor growth inhibiting properties against the National Cancer Institute's murine P388 lymphocytic leukemia (PS system) showing ED 50 3.5 μg/mL. Structural determination and absolute configuration was accomplished using high field NMR (400 MH z ) and mass spectral techniques (FAB MS/MS) in conjunction with chiral gas chromatographic analysis. The direct correlation between the PS System and ultimate human efficacy of the substance as tested has been established (See: Vendetti and Abbot, Lloydia, 30, 322 et seq. (1967) and the references cited therein).
Hymenistatin I has the following general structure: ##STR3##
DESCRIPTION OF PREFERRED EMBODIMENTS
General Methods
Solvents used for chromatographic procedures were redistilled. The SEPHADEX LH-20 (25-100μ) employed for gel permeation and partition chromatography was obtained from Pharmacia Fine Chemicals AB, Uppsala, Sweden. GILSON FC-220 race track and FC-80 microfractionators connected to GILSON HM UV-visible detectors were used for chromatographic fractionation experiments, and column chromatographic procedures with silica gel utilizing the SILICA GEL 60 prepacked "LOBAR" columns supplied by E. Merck, Darmstadt, West Germany. The SILICA GEL GF UNIPLATES for TLC were obtained from Analtech Inc., Newark, Del. All TLC plates were viewed with uv light and/or developed with a ceric sulphate-sulfuric acid spray (heating to approximately 150° C. for 10 min).
The uncorrected melting points were observed using a KOFLER-type melting point apparatus. The uv spectrum was recorded using a HEWLETT-PACKARD 8450A uv-visible spectrophotometer equipped with a HP7225A plotter. Optical rotation and ir spectral data were obtained using a PERKIN-ELMER 241 polarimeter and a NICOLET MX-1 FTIR spectrophotometer, respectively. Mass spectra (70 eV and FAB) were recorded employing a KRATOS MS-50 spectrometer. The nmr experiments were conducted with a BRUKER WH-400 instrument and deuteriochloroform as solvent (TMS internal standard).
Animal Collection and Preliminary Experiments
In early 1979, approximately 2 kg (wet wt) of the sponge Hymeniacidon sp. (Hymeniacidonidae family, Halichondrida Order, Ceratinomorpha Subclass, Demospongiae Class) was collected by scuba near the Long Island (south side) in the Palau Archipelago, Western Caroline Islands. Taxonomic identification was conducted in the Smithsonian Institution where reference specimens are on file. The initial sample of Hymeniacidon sp. was preserved in 2-propanol-methylene chloride. Removal of solvent gave an extract that reached a confirmed level of activity against the U.S. National Cancer Institute's murine P388 lymphocytic leukemia (PS system) with 30% life extension at 5.5 mg/kg.
Animal Extraction and Solvent Partitioning
In March 1985, 218 kg (wet wt) of the Hymeniacidon sp. was recollected from the same area in Palau near the south side of Long Island and preserved in 2-propanol. The 2-propanol solution was later decanted and the sponge was re-extracted with the same alcohol. The first extract was reduced to a 50 liter water concentrate under partial vacuum and found to contain a considerable amount (1.2 kg) of a pale brown suspension (PS T/C toxic at ≧50 mg/kg), which was removed by centrifugation and decantation. The cream-colored aqueous phase was successively partitioned between methylene chloride (90 liters) and n-butanol (90 liters). Evaporation of solvent from each of the two combined organic extracts gave respectively, a very dark brown gel-like solid (180 g, PS ED 50 1.8 μg/mL and T/C toxic at ≧50 mg/kg) and a pale brown amorphous solid (330 g, PS ED 50 6.1 μg/mL and T/C toxic at ≧50 mg/kg). The remaining aqueous extract was found to be PS inactive and was discarded. A solution of the methylene chloride fraction (180 g) in 9:1 methanol-water (1 liter) was extracted with hexane (3×1 liter). The methanol-water phase was diluted to 3:2 and extracted with methylene chloride. The resulting hexane (146 g), methylene chloride (20 g) and 3:2 methanol-water (14 g) fractions were concentrated and aliquots submitted for bioassay. Significant PS cytostatic activity (PS ED 50 0.26 μg/mL) was found to reside in the methylene chloride extract.
Isolation of Hymenistatin 1.
In a typical series of procedures, the 20 g active methylene chloride fraction in 3:2 methylene chloride-methanol produced as described was chromatographed on a column of SEPHADEX LH-20 (1.2 kg; 20×120 cm). While no pronounced separation of components was observed, a further concentration of active material (Fraction A, 18 g, PS ED 50 1.6 μg/mL) was realized. Further partition chromatography on SEPHADEX LH-20 (1.2 kg; 20×120 cm) and elution with 3:1:1 hexane-toluene-methanol gave active fractions B (0.50 g, PS ED 50 2.6 μg/mL) and C (1.64 g, PS ED 50 1.7 μg/mL) among eleven distinct composite fractions. Fractions B and C were combined and further separated in methanol on a SEPHADEX LH-20 column. Among the nine fraction groups obtained, a fraction labeled D (0.75 g, PS ED 50 3.1 μg/mL) showed an almost single spot on tlc. Final purification was achieved utilizing a medium pressure (to 50 p.s.i.) liquid chromatography unit with a pre-packed SILICA GEL 60 column (2.5×30 cm) and elution with 97.5-2.5 methylene chloride-methanol.
Hymenistatin 1 was obtained as a colorless, crystalline amorphous solid (49 mg, 3.1×10 -5 % yield), melting at 180°-182° C. [α] D -8.6° (c=1, CHCl 3 ); uv (CH 3 OH) λ max (logε), 222 (3.82), 278 (3.16) nm; ir (NaCl plate) 3320, 2960, 2920, 1680, 1617, 1517 cm -1 ; ms (HRSP-SIMS), 893.5505 [M+H] + for C 47 H 73 N 8 O 8 , calcd. 893.5501; nmr (CDCl 3 ), δ; Proline-a unit, 1 H, 4.20 (H-2), 3.72 (H-5a), 3.38 (H-5b), 2.15 (H-3a), 2.11 (H-4a), 1.95 (H-4b), 1.93 (H-3b); 13 C; 60.89 (C-2), 47.35 (C-5), 31.87 (C-3), 25.06 (C-4); Proline-b unit, 1 H, 4.10 (dd, J=9.4, 3.5; H-2), 3.28 (H-5a), 3.21 (H-5b), 2.16 (H-3a), 1.77 (H-3b), 1.60 (H-4a), 0.85 (H-4b); 13 C: 59.19 (C-2), 46.94 (C-5), 28.52 (C-3), 21.11 (C-4), Tyrosine unit, 1 H, 8.70 (br s, OH), 7.03 (d, J═8.l; H-5), 6.84 (d, J═8.0; H-6), 4.22 (H-2), 3.29 (H-3a), 2.90 (t, J═13.0; H-3b), 13 C, 156.56 (C-7), 129.67 (C-5, C-9), 127.00 (C-4), 115.94 (C-6, C-8), 58.13 (C-2), 36.67 (C-3), Valine unit, 1 H: 7.58 (d, J═8.8; NH), 4.56 (t, J═5.9; H-2), 1.95 (H-3), 0.98 (6H; H-4, H-5); 13 C: 56.29 (C-2), 31.67 (C-3), 19.29 (C-4), 18.19 (C-5). Proline c unit, 1 H, 3.92 (H-5a), 3.79 (t, J═7.8; H-2), 3.68 (H-5b), 2.31 (H-3a), 2.08 (H-4a), 2.06 (H-4b), 1.91 (H-3b), 13 C, 63.11 (C-2), 48.55 (C-5), 30.00 (C-3), 24.75 (C-4), Leucine unit, 1 H, 6.25 (br s, NH), 3.98 (H-2), 1.96 (H-3a), 1.82 (H-3b), 1.55 (H-4), 0.93 (3H; d, J═6.3, H-6), 0.88 (3H, H-5), 13 C, 55.79 (C-2, 39.27 (C-3), 25.31 (C-4), 22.95 (C-6), 21.27 (C-5), Isoleucine-a unit, 1 H, 7.70 (d, J═8.5,NH), 4.40 (t, J═8.5, H-2), 1.57 (H-3), 1.50 (H-4a), 1.15 (H-4b), 0.96, (3H; H-6), 0.87 (3H; H-5); 13 C: 60 52 (C-2), 38.26 (C-3), 24.95 (C-4), 15.47 (C-6), 10.64 (C-5), Isoleucine-b unit, 1 H, 7.40 (d, J═8.5, NH), 4.69 (t, J═9.0, H-2), 1.76 (H-3), 1.53 (H-4a), 1.05 (H-4b), 0.82 (3H; H-6), 0.80 (3H; H-5); 13 C, 55.01 (C-2), 36.94 (C-3), 24.79 (C-4), 16.20 (C-6), 11.87 (C-5). Eight carbonyl 13 C resonances appear at 172.72, 172.29, 172.10, 171.98, 171.95, 171.18, 170.35 (where no multiciplicity is indicated it could not be determined due to overlapping signals).
Assignment of the Hymenistatin 1 Chiral Centers
The cyclo-octapeptide was hydrolyzed with 1:1 propionic acid l2N hydrochloric acid at 160° for 15 min. The corresponding amino acids were converted to N-pentafluropropionyl-isopropyl ester derivatives and configurations established by chiral capillary chromatography as described by Shaw and Cotter (See: Chromatographia, 21, 197 (1986)) using a Chirasil Val III column. Each amino acid component was found to belong to the S(L)-series.
In one practice of the present invention, initially, the isopropyl alcohol-water solution employed to preserve some 218 kg of the sponge was concentrated to 50 liters of an aqueous fraction containing a rather viscous beige colored suspension that required removal by centrifugation at 1000 G and filtration. The opaque, cream-colored aqueous portion was successively partitioned between methylene chloride followed by n-butanol to provide two active fractions as shown in the process scheme produced below. ##STR4##
The PS active methylene chloride extract was partitioned between 9:1 methanol-water and hexane, followed by dilution to 3:2 methanol-water and partition with methylene chloride. Upon evaporation of the chlorocarbon an orange-colored solid was obtained which significantly inhibited the PS leukemia (PS ED 50 0.26 μg/mL). Initial gel-permeation chromatographic separation of the methylene chloride-soluble fraction on SEPHADEX LH-20 and elution with 3:2 methylene chloride-methanol led to a further concentration of activity in Fraction A. A better separation was achieved employing partition chromatography on SEPHADEX LH-20 with 3:1:1 hexane-toluene-methanol to provide fractions B and C. These two principal active fractions B and C were then combined and separated on a column of SEPHADEX LH-20 in methanol to provide Fraction D. The nearly pure cytostatic constituent obtained by this means was chromatographed using a SILICA GEL 60 LOBAR B column. Elution with 97.5:2.5 methylene chloride-methanol afforded the cell growth inhibitory (PS ED 50 3.5 μg/mL) biosynthetic product herein designated Hymenistatin 1.
Mass spectral measurements of Hymenistatin 1, as reported herein, indicated the presence of eight nitrogen atoms, which with eight amide carbonyls observed in the 13 C nmr spectrum, indicated an octapeptide. The relatively high intensity of the molecular ion (base peak) observed in the EIMS spectrum suggested that the presumed octapeptide might by cyclic. Extensive application of 2-D nmr techniques were next used to determine the identity of the eight amino acid units. The 400 MHz 1 H-nmr spectrum clearly showed the presence of only five (amide protons. By following the spin systems of these protons using 1 H, 1 H-COSY and 1 H, 1 H relayed COSY, these amino acids were determined to be valine, leucine, tyrosine and two isoleucine units. Utilization of 1 H, 13 C-COSY and 1 H, 1 H, 13 C-RELAY showed that the remaining nmr signals consisted of three independent spin systems of the type X-CH-CH 2 -CH 2 -X typical of proline. The eight amino acid units accounted for the observed accurate-mass molecular weight. Actual sequence of the amino acids was ascertained from ID-nOe (nuclear Overhauser effects) experiments as shown below. ##STR5##
In order to further corroborate the proposed structure, positive ion FAB MS/MS was pursued. As shown below, protonation at each proline nitrogen afforded three different linear peptide ions in the mass spectrum noted as a, b and c. All but one of the ions predicted from their fragmentation was also observed, thereby confirming the structure assigned Hymenistatin 1 as shown herein. The absolute configuration of each chiral center was assigned using chiral GC analysis (Chirasil-Val III column) of the peptide hydrolysate following preparation of the N-pentafluoropropionylisopropyl ester derivatives. All of the amino acid units were found to bear the L-configuration.
Hymenistatin 1 peptide sequence determination by FAB ms/ms.
cyclo [Pro a -Pro b -Tyr-Val-Pro c -Leu-Ili-Ile]
Observed mass spectral fragmentation resulting from protonation at proline (indicated by a, b, or c): ##STR6##
To further aid in the understanding of the present invention and not by way of limitation, the following examples are prescribed.
EXAMPLE I
Hymeniacidon sp. was collected (218 kg, wet) and preserved in 2-propanol. The 2-propanol solution was decanted and the sponge was reextracted with 2-propanol. The first extract was reduced to a 50 liter water concentrate under partial vacuum which contained a pale brown suspension which was removed therefrom by centrifugation and decantation leaving a cream colored aqueous phase.
EXAMPLE II
The cream colored aqueous phase produced by Example I was partitioned between methylene chloride (90 liters) and n-butanol (90 liters). Evaporation of solvent from each of the two combined organic extracts gave a very dark brown gel-like solid (180 g, PS ED 50 1.8 μg/mL and T/C 105 at 50 mg/kg) and a pale brown amorphous solid (330 g. PS ED 50 6.1 μg/mL and T/C toxic at >50 mg/kg).
EXAMPLE III
The methylene chloride fraction (180 g) produced according to Example II was disposed in 9:1 methanol-water solution (1 liter) and extracted with hexane (3×1 liter). The methanol-water phase was diluted to 3:2 and extracted with methylene chloride.
The resulting hexane (146 g), methylene chloride (20 g) and 3:2 methanol-water (14 g) fractions were concentrated and aliquots thereof subjected to bioassay. The methylene chloride extract was found to possess significant PS cytostatic activity (PS ED 50 0.26 μg/mL).
EXAMPLE IV
The methylene chloride fraction (20 g) produced according to Example III was dispersed in 3:2 methylene chloride-methanol and thereafter chromatographed on a column of SEPHADEX LH-20 (1.2 kg; 20×120 cm). A further concentration of active material occurred as Fraction A. (l8g, PS ED 50 1.6 μg/mL). Additional partition chromatography on SEPHADEX LH-20 (1.2 kg; 20×120 cm) and elution with 3:1:1 hexane-toluene-methanol produced, inter alia, Fraction B (0.5 g, PS ED 50 2.5 μg/mL) and actual Fraction C (1.64 g, PS ED 50 1.7 μg/mL).
EXAMPLE V
Fraction B and C, obtained from Example IV, were combined and further separated in methanol on a SEPHADEX LH-20 column into nine separate fractions. Among the fractions obtained, a fraction designated D (0.75 g, PS ED 50 3.1 μg/mL) showed an almost single spot on tlc.
EXAMPLE VI
Fraction D obtained from Example V was further purified using a medium pressure (up to 50 psi) liquid chromatography unit with a pre-packed SILICA GEL 60 column (2.5×30 cm) and eluted with 97.5-2.5 methylene chloride-methanol. Hymenistatin 1 was obtained as a colorless, crystalline amorphous solid (49 mg, 3.1×10 -5 % yield) melting at 180°-182° C.
From the foregoing, it is readily apparent that an invention has been herein described and illustrated which fulfills all of the aforementioned objectives in a remarkably unexpected fashion. It is, of course, understood that such modifications, alterations, and adaptations as may readily occur to the artisan confronted with this disclosure are intended within the spirit of this invention which is limited solely by the scope of the claims appended hereto. | A new and demonstratably active cyclo-octapeptide is isolated from the South Pacific Ocean Hymeniacidon sp. and structurally elucidated. The substance, herein denominated Hymenistatin 1, demonstrated utility by inhibiting tumor growth when measured by the National Cancer Institute P388 leukemia cell line (ED 50 =3.5 μg/mL). Hymenistatin 1 has the following structure: ##STR1## | 8 |
CROSS-REFERENCE TO RELATED APPLICATION
[0001] This non-provisional application claims priority to the provisional application for patent Ser. No. 61/072,974 filed Apr. 4, 2008, which is commonly owned by the same assignee.
BACKGROUND OF THE INVENTION
[0002] This product for liquid delivery fragrance samples relates to the manufacture of a fragrance sampler page or piece and more specifically to liquid-delivery type fragrance samplers. These samplers are well known in the industry and are commonly found in magazines, used as retail handouts, or contained in advertising mailers. A unique aspect of the system is retention of a liquid fragrance sample upon the sampler using surface tension of the fragrance in cooperation with the texture of the sampler and without a perimeter weld or gluing of the sampler.
DESCRIPTION OF THE PRIOR ART
[0003] Typically, liquid-delivery type samplers comprise a liquid fragrance contained in a hermetically sealed film envelope which has a heat-sealed, or glued, perimeter so as to contain the liquid fragrance within these samplers without leaking. These samplers are generally manufactured in the form of a label comprising multiple film layers. Generally, the manufacturing process produces the samplers at slow speeds on small-format web or label presses that have been modified to suit the application. Machinery then mechanically or physically attaches the samplers to a carrier page for later incorporation into magazines or other mailings. Further, small stand-alone sampler pieces also provide handouts or flyers in retail establishments.
[0004] The liquid fragrance material carried by the sampler is generally accessed by removing, or pealing away, a laminated cover portion of the sampler. These sample devices provide to fragrance manufactures methods and devices that present a rendition of their products for trial by prospective customers. In addition, the sample pages and pieces include graphics and advertising prose printed thereon, commonly seen in printed advertising media for another viable sales instrument.
[0005] Prior art label-type pieces such as Bootman et al., U.S. Pat. No. 5,391,420, Muchin, U.S. Pat. No. 5,161,688, and, Bishopp, U.S. Pat. No. 5,439,172, teach methods of producing an effective liquid-fragrance advertising device. This type of devices rely upon a perimeter glue band, or heat seal, to prevent capillary action of the fragrance from occurring between the substrate layers of the sampler. Fragrance capillary action arises from the surface tension of the fragrance and the close proximity of the substrates and layers. Fragrance capillary action would cause leakage from within the sampler and onto the sample page, the carrier, or the magazine. Prospective customers avoid fragrances that leak from a sampler and damage a magazine. Leaky fragrance samples also lose their volatile components upon exposure to the atmosphere. The seal also aids in preventing leakage caused by compression loads, which occur with common frequency in sampler pieces that are contained in large stacks of magazines during assembly, mailing, transport, and display.
[0006] The manufacturing operations, necessary to produce these perimeter seals, require continuous process monitoring because even slight process variation can cause the perimeter seals to fail. These products also require a minimum of three expensive, discontinuous auxiliary operations to produce a finished sampler page.
[0007] More particularly, Bootman describes a pressure sensitive label comprising two plies of a film or plastic material: one bottom pressure sensitive ply, a deposit of fragrance material and an overlay of a second ply which traps the fragrance deposit. The sealing is by a perimeter heat seal. The draw back of this product is that the fragrance material is often forced into and through the seal areas under pressure from the stacking forces of many magazines, or inserts, in distribution.
[0008] Then, Muchin builds upon Bootman by introducing a center ply material which has a die-cut window. This window ply is introduced onto the bottom pressure sensitive ply and thus creates a well for the fragrance material. The top, third ply is then added and the result is that stacking forces are distributed on to the widow ply and the fragrance material is exposed to less force that would have lead to seal failures and leakage: a major defect from Bootman.
[0009] A more cost-effective method to produce liquid-delivery sample pages, or pieces, constructs the page from a commercially printable paper substrate and contains the liquid, volatile, fragrance material between layers of the substrates. By following this method, a single manufacturing platform completes the entire printing and assembling process in-line. The paper and other required materials are mounted and processed on the single line, and the finished product exits the end of the manufacturing line for packaging and then shipment.
[0010] Other prior art includes some instances of liquid fragrance delivery devices that are also produced in-line during a single operation. The patent to Charbonneau, U.S. Pat. No. 5,419,958 discloses a paper-based sampler page designed to defeat fragrance pre-release by applying a volatile liquid treatment or coating to the sample application area so as to block the penetration of fragrance oils into the paper.
[0011] This method requires sequential layers of barrier coating and involves the use of huge curing ovens to provide an adequate barrier. Most existing printing lines lack the floor space required for such additions. Therefore, the necessity exists to design and to construct a custom manufacturing line for implementation of this product.
[0012] Further, Charbonneau does not disclose any method that would prevent the fragrance material from leaking out of the sampler. The types of coatings cited by Charbonneau have high susceptibility to surface inconsistencies, known as pin-holes. The pin holes appear from vapor off-gassing during the curing stage of the process. Then the thick coatings that resist the off-gassing cause the paper to curl badly.
[0013] Then the patent to Whitaker et al., U.S. Pat. No. 5,645,161 discloses a multiplicity of construction methods. One embodiment comprises a heat-sealed perimeter that contains the liquid fragrance. Such heat sealing is a slow, cumbersome, and expensive manufacturing method. The maximum speed of the heat-seal unit falls short of the minimum operational speed of present day printing presses leading to a bottle neck of production at the heat seal unit while the presses operate at less an optimum rates. Another embodiment involves equipment that applies a patch of barrier-type film to the moving paper web of a printing press. This operation, too, would also fall behind the minimum operational speed of a modern printing press.
[0014] The patent to Jones et al., U.S. Pat. No. 6,125,614 discloses a method of manufacturing a laminated page comprising a paper substrate carrier and a film substrate barrier layer. This continuous, film-type barrier layer glues to a paper substrate web to provide impermeability to the. film. Then to defeat fragrance material capillary action between the film layers and leakage during compression loads, an additional adhesive is applied to become a perimeter seal on the film layer. Ideally, this secondary glue band requires in-line curing to avoid off-odor detectable by the prospective customer which can occur from interaction between the adhesive and the fragrance material. The fragrance is then printed onto the film, and the area of the page containing the laminated film is then folded over onto itself, forming a pouch, or envelope, containing the fragrance material. The application of the perimeter glue band requires continuous monitoring through visual inspection by workers or automated sensors of the finished pieces as they come along the manufacturing line.
[0015] Another challenge from the laminated, film and paper, construction of Jones, Whitaker, and Charbonneau, exists in the manufacturing scraps and wastes. The paper related recycle waste stream at bindery operations becomes contaminated by the film substrate during magazine edge-trimming operations. This contamination can be avoided by an expensive secondary die-cutting operation that removes the film substrate from the magazine trim-off area. This secondary operation though defeats the original economics of performing an all in-line construction.
SUMMARY OF THE INVENTION
[0016] This sampler contains liquid fragrance within the texture of one or more substrate layers. When a material, such as a liquid, attains a steady state upon a surface, the liquid has reached a state of repose, also called a state of rest or inactivity. In that state, the liquid or other loose, cohesion-less material, comes to rest in a pile of a known geometry defined by its angle of repose which is the maximum angle of slope measured from a horizontal plane. The angle of repose is related to the coefficient of friction of the material.
[0017] The preferred embodiment of the liquid-delivery fragrance sample page or piece has a construction without a liquid tight and a vapor tight, perimeter glue band or heat seal. The liquid-delivery fragrance sampler page comes from easily produced, in-line manufacturing of a commercially printable material, preferably paper, which has an applied barrier coating to defeat permeation by the liquid fragrance material. The material of this invention, preferably paper, provides a substantially irregular, or textured, fragrance sample material mounting and application surface that self creates an occlusive, cohesive seal between the substrate layers when fragrance materials are applied between the layers. The material of the invention provides a self sealing device that retains a fragrance sample placed therein. Then at the place of usage of the sampler, the fragrance sample materials are easily accessed for trial by a prospective customer who opens a fold or removes a die-cut portion on the page of the sampler.
[0018] More particularly in this invention, the opposing, textured substrates of the sampler plies are maintained in close proximity. There, the textured surfaces modify the behavior of the deposited fragrance material so as to defeat its capillary action and, thereby, act to occlude the migration of the fragrance material from its application area out from the sampler. Also, because the textured surface contains the liquid fragrance, the inability of the fragrance to flow in conjunction with its inherent surface tension makes the fragrance material substantially repose and maintain its position within the texture of the barrier coating.
[0019] Numerous objects, features and advantages of the present invention will be readily apparent to those of ordinary skill in the art upon a reading of the following detailed description of the presently preferred, but nonetheless illustrative, embodiment of the present invention when taken in conjunction with the accompanying drawings. Before explaining the current embodiment of the invention in detail, it is to be understood that the invention is not limited in its application to the details of construction and to the arrangements of the components set forth in the following description or illustrated in the drawings. The invention is capable of other embodiments and of being practiced and carried out in various ways. Also, the phraseology and terminology employed herein are for the purpose of description and should not be regarded as limiting.
[0020] Therefore the object of the present invention is to provide a product for liquid delivery fragrance samples that requires no continuous perimeter heat seal or glue band in the fragrance or sample material's containment zone.
[0021] Another object of the product for liquid delivery fragrance samples is to occlude capillary action of the fragrance material by separation of the substrates using the coated substrate's texture.
[0022] Another object of the product for liquid delivery fragrance samples is to substantially fill the textured surface without affecting the position, or repose, or the fragrance sample within the textured surface by compressive loads. The reposed fragrance material remains within the application area's target zone.
[0023] Another object of the product for liquid delivery fragrance samples is to provide the fragrance material's angle of contact in the finished sampler of at least ninety degrees.
[0024] Another object of the product for liquid delivery fragrance samples is to create a cohesive seal between the substrate layers' barrier coating because of the inherent surface tension of the fragrance material, thereby substantially reducing the fragrance material's contact with the atmosphere and thus greatly reducing its ability to evaporate.
[0025] And lastly, another object of the product for liquid delivery fragrance samples is to determine the volume of the sample material contained in the sample application area by the total area of the textured surface and surface tension characteristics of the sample material.
[0026] These together with other objects of the invention, along with the various features of novelty that characterize the invention, are pointed out with particularity in the claims annexed to and forming a part of this disclosure. For a better understanding of the invention, its operating advantages and the specific objects attained by its uses, reference should be had to the accompanying drawings and descriptive matter in which there is illustrated a preferred embodiment of the invention.
BRIEF DESCRIPTION OF THE DRAWINGS
[0027] In referring to the drawings,
[0028] FIG. 1 shows a sampler in plan view;
[0029] FIG. 2 illustrates a detailed depiction of a tight grid, or cross hatch, texture pattern with an application of liquid fragrance material;
[0030] FIG. 3 illustrates a detailed magnified depiction of a quad cell-type texture pattern with an application of liquid fragrance material;
[0031] FIG. 4 illustrates a detailed depiction of a wide grid, or dot matrix-type, texture pattern with an application of liquid fragrance material;
[0032] FIG. 5 illustrates a detailed depiction of a random dot pattern applied to the base coating layer through the use of an atomizer and an application of liquid fragrance material;
[0033] FIG. 6 illustrates a top view of a pattern of concentric shaped ridges of coating material on the base barrier coating layer and an application of liquid fragrance material; and,
[0034] FIG. 7 describes in a detailed view the interaction of liquid fragrance materials with adjoining surface texture.
[0035] The same reference numerals refer to the same parts throughout the various figures.
DESCRIPTION OF THE PREFERRED EMBODIMENT
[0036] The present art overcomes the prior art limitations by assembling a product for liquid delivery fragrance samples where the liquid fragrance remains within the surface texture of a substrate because of a high angle of contact, thus limiting the adverse effects of capillary infiltration of the fragrance into the material of the invention. The high angle of contact of the fragrance sample in relation to the material of the present invention prevents wetting of the sample into the material. The present invention utilizes a highly hydrophobic systems that induces an angle of contact exceeding ninety degrees. The present invention 10 begins with the components of a fragrance formulation selected by a fragrance house or manufacturer. The fragrance formulation is then rendered into a liquid for placement upon a sampler, or piece, as in FIG. 1 where the preferred embodiment is shown opened. The printable paper page, sheet of material, or substrate 1 , has a generally rectangular shape where the longitudinal axis is longer than the lateral axis. In this figure, the longitudinal axis is oriented upright. The substrate has a fold line, as at 2 , slightly off center to allow for covering the fragrance sample and the application of adjacent printing. The fold line divides the substrate into a base 1 a to the left of the fold line and a cover 1 b to the right of the fold line. Alternatively, the cover may be a hinged portion of the base that folds upon a portion of the base. In a further alternate embodiment, the cover and the base may be of separate sheets of material that overlay at least a portion of one sheet. Mutually spaced apart from the fold line 2 and in mutual registration, the substrate has two ultraviolet light cured, cationic barrier-type coated surfaces, as at 3 on the left or base 1 a and as at 4 on the right or the cover 1 b, that come into registered contact when the cover is folded along the fold line 2 upon the base. The coated surface 3 , or section of barrier coating, has a substantially smooth surface. In contrast, the opposite coated surface 4 includes a textured surface of known geometry applied upon a barrier coating, as later shown in FIGS. 2-5 , and an application of liquid fragrance sample material 5 within the perimeter of the textured surface. Though a sample material is described broadly, the sample includes lipstick, liquid cosmetics, liquid fragrances, substantially gelled fragrances, and liquid fragrances with chemically altered viscosity and surface tension. The liquid fragrances include various additives that manipulate the viscosity and surface tension of the fragrance solution without affecting its scent. Then an enlarged depiction of the coated surface 4 , or textured coating section, appears in FIGS. 2-6 .
[0037] The liquid fragrance sample may undergo modification of its viscosity in various ways. Such modifications utilize fragrance oils or other fluids to change the resulting viscosity of the modified fragrance solution. Typically, fragrance oil has a viscosity range of about 2 to about 12 centipoise. However, the type of applicator or dispensing equipment may require thickening of the liquid, that is a higher viscosity, for proper passage of the fragrance liquid through the equipment. Most equipment operates upon liquids having a viscosity between 40 centipoise and 2400 centipoise, however, liquid viscosity in the range of 200,000 centipoise are still accommodated. The liquid fragrance of modified viscosity includes a blend of materials, or the addition of rheology modifiers, emulsions, suspensions, reacted materials, and other forms of thickened liquids. The liquid fragrance of modified viscosity may or may not have adhesive qualities.
[0038] The Applicants foresee modifying the liquid fragrance's viscosity using various components. Those components include blends of cellulose gums, cellulose derivatives, carboxymethylcellulose, sodium carboxymethylcellulose, hydroxypropylcellulose, hydroxyethylcellulose, methylcellulose, ethylcellulose or ethycell; vegetable gums, xanthan gum, acacia gum; alginates, carrageenan, alcogum; silicones, versagels, silicone fluid 200; clays, veegum, bentone gel, silicas, untreated fumed silica or Cabosil® M-5 from Eager Plastics of Chicago, Ill., specially treated fumed silica or Cabosil®TS-720, TS-630; surfactants, sodium lauryl sulfate, ammonium lauryl sulfate; fillers, calcium polycarbophil; emulsions, polyvinyl alcohol or Celvol® from Celanese Corp. of Dallas, Tex.; and suspensions, acrylic acid derivatives such as Carbopol® 940 and Ultrez® 10 from Lubrizol Corp. of Wickliffe, Ohio. One example of medication adjusts the viscosity of fragrance oil by adding ethycell at the rate of five percent by weight and mixing the solution at room temperature under high shear for five hours. This modification produces a fragrance oil with its viscosity increased to the range of 1700 to 1900 centipoise.
[0039] In the operations of this invention, the textured coating has the cosmetic sample locating within its interstices. Then mutually parallel barrier coatings layer upon and confront the textured coating. The sample remains with the textured coating because of stilting and its repose while the textured coating becomes effectively sealed by the adjacent barrier coatings. This layered arrangement of textured coating and barrier coating does not require a perimeter seal by heat or other welding methods.
[0040] Generally, the textured coating section has a pattern of spaced apart cells or a plurality of pockets. The sample page 1 also has a plurality of means to adhere the invention into a closed form including non-permanent adhesive applications, as at 6 , in a pattern upon the cover 1 b that maintain the barrier surfaces 3 and 4 in close proximity when the cover 1 b is closed upon the base 1 a as at the end of manufacturing, during shipment, and through the mail. The adhesive applications may include a pressure sensitive adhesive activated during manufacturing when the textured coating section is closed upon the barrier coating section and a repositionable glue that adheres the material of the device to itself temporarily but allows for ready separation of the parts of the device or the device from a mailpiece. The adhesive applications, 6 , keep the sampler 1 closed until the cover 1 b is opened from the base 1 a by the prospective consumer. Additionally, either coated surface, 3 , 4 , or the sheet of material may have a further application of pressure sensitive adhesive that activates upon insertion of the invention into a printed material. This usage of adhesive secures the invention, when closed, upon a page or a card or into a magazine or other material as part of a consumer mailing campaign.
[0041] Alternatively, the textured coating section and the barrier coating section are located upon separate. sheets of material, such as select papers. Each sheet of material then has a barrier coating applied thereto and one sheet has the textured section applied upon its barrier coating. Though on separate sheets. the textured coating section registers with the barrier coating section of another sheet so that the individual pieces of texture retain the liquid fragrance sample within the spaces of the textured surface as later shown in FIG. 7 .
[0042] The barrier coating, or base coat, of the invention begins with an existing low odor, ultraviolet curable, cationic type varnish. Such a varnish includes RAD-KOTE product number K261 from Actega Radcure of Wayne, N.J. This varnish has a viscosity of approximately 375 centipoise. The low odor attribute of this varnish makes it preferable over coatings from other manufacturers. The barrier coating is applied on to a printed web of material using a flexographic coater with a Cyrel type printing plate. The printing plate has a smooth finish and is sized to meet the dimension of the desired application. Generally, the barrier coating is applied to the web of material in a thickness of about 0.3 to about 0.6 mils, depending on the surface finish or porosity of the web of material, commonly paper or substrate. An about 0.3 to about 0.4 mil thick application of base coat is effective on a high quality, smooth finish paper which is used in commercial printing. The coating then undergoes curing at an ultraviolet light curing station mounted directly after the flexographic coater. The intensity of ultraviolet light used relates to the desired operation speed of the press. Generally, printers provide approximately 100 watts of ultraviolet light per every 100 feet per minute of press web speed. As an example, a press running at 1000 feet per minute calls for 1000 watts of ultraviolet light curing capability.
[0043] The present invention also provides an embodiment where the prospective customer accesses the sample of fragrance through a die cut opening. The die cut opening can be in the textured coating section, the opposite barrier coating section, or both the textured coating section and the barrier coating section. In usage, the textured coating section has the sample of fragrance deposited upon it and then folded upon the barrier coating section with the die cut opening upwards. The prospective customer then removes the textured coating section within the die cut to test the fragrance.
[0044] Then FIG. 2 depicts a detailed view of a tight grid, or cross hatch, texture pattern upon the coated surface 4 . This pattern has lines intersecting at right angles with the lines of thinner width than the squares of substrate between adjacent lines. This pattern provides a suitable application surface for liquid fragrance sample material, as at 5 , along the thin lines between the squares of substrate material.
[0045] The texture coating is preferably a low odor, ultraviolet curable, cationic type adhesive. Such an adhesive includes RAD-KOTE product number K6004B from Actega Radcure of Wayne, N.J. This adhesive has a viscosity of approximately 825 centipoise. The Applicants prefer this adhesive for its ability to build height to the texture, as it possesses a greater viscosity and solids content than what is used for the base coat. Though described as an adhesive, the present invention has the adhesive cured immediately in a pattern as later shown that builds the texture of the invention.
[0046] The texture coating is also applied to the material, paper, or substrate, using a flexographic coater with a Cyrel type printing plate followed by immediate curing at an ultraviolet station as previously described. This printing plate though has a raised, or negative image, of the desired texture pattern in the appropriate size for the desired product. Generally, the texture coating is applied in a thickness ranging from about 0.25 mils to about 2.5 mils depending on the amount of fragrance loaded into the present invention. The Applicants prefer a thickness in the range of about 0.5 miles to about 1.25 mils. As an example of single sided texture delivery device includes a one square inch fragrance fluid application upon a 30 line per inch grid texture where the grid has a 1.0 mil height. This example yields a payload of approximately 0.27 fluid drams or about 0.1 milliliter. The present invention also includes textured coating upon both surfaces which doubles the fragrance payload.
[0047] Alternatively, the liquid fragrance material is applied by a flexographic coater as previously described. This printing plate though is made of a soft, closed cell foam material, such as Poron®. These plates, or pads, possess a smooth surface and a low memory attribute that enhances application repeatability, usually for adhesive application.
[0048] FIG. 3 illustrates a detailed view of an alternate embodiment of the texture pattern as a quad cell-type pattern also upon the coated surface 4 . This pattern has individual cells, of substrate material, with rounded corners where the cells are oriented at a forty five degree angle to the edges of the product sampler. The application of liquid fragrance material, as at 5 , generally occupies the diamond like shapes between the cells in this figure.
[0049] FIG. 4 shows a detailed view of a dot matrix-type texture pattern upon the coated surface 4 . Similar to FIG. 2 , this pattern also has lines at right angle intersections with the lines having similar width to the squares of substrate between adjacent lines. This pattern has a suitable application surface for liquid fragrance sample material, as at 5 , along the wider lines between the squares of substrate material.
[0050] FIG. 5 provides another detailed view but of a random dot pattern of the base coating layer applied to the substrate as the coated surface 4 through the use of an atomizing device. Alternatively, the random dot pattern arises upon mixing a fine aggregate particle material, such as nylon spheres of a certain diameter, into the barrier coating material and applying the mixture upon the substrate to create texture that secures an application of liquid fragrance material, as at 5 . In a further alternate embodiment, a textured barrier film applied to the cover forms the coated surface 4 . In another alternate embodiment, mechanically altered, or distressed, coating film applied to the cover makes the textured coating section. The textured coating section may also have porosity that defines a pattern of texture for retaining liquid fragrance material.
[0051] And then, FIG. 6 shows a detailed view of a pattern of concentric shaped ridges of coating material on the base barrier coating layer, or coated surface 4 . The ridges, or surfaces, generally follow the shape of the perimeter of the sampler product and each ridge is spaced at an interval inwardly from the previous ridge. The interval, or spacing, between adjacent ridges retains an application of liquid fragrance material, as at 5 , upon the sampler product. In alternate embodiment, the outermost ridge may also be a glue band that seals the two surfaces together thus preventing contamination of the fragrance sample therein.
[0052] Following the description of the various patterns upon the coated surface 4 , FIG. 7 shows the interaction of a liquid fragrance sample with the surface texture in a pattern similar to that shown in FIG. 4 . This view is highly magnified, generally showing individual droplets of fragrance secured within the texture, particularly its surface features. The paper of this invention provides a textured mounting surface, as at 4 , to which is applied fragrance material, as at 5 , here shown between individual cells of texture, as at 4 . Opposite the mounting surface 4 , the invention has a smooth surface 3 onto which the mounting surface abuts. The individual textures of the mounting surface contact the smooth surface and seal the gaps between individual textures. The individual textures modify the behavior of the deposited fragrance material, such as at 5 between two adjacent textures 4 , so as to defeat its capillary action. The textured surface thus occludes the migration, or flow, of the fragrance material from its application location through the smooth and the textured surfaces as at 3 , 4 and then out of the product sampler. The present invention achieves stilting between the cover and the mounting surface. In an embodiment with two separate films as the cover and mounting surface, the separate films with the appropriate surface coatings and textures avoid or retard the capillary infiltration of a liquid cosmetic into the fibers of the sampler. Further, because the textured surface contains the liquid fragrance, the inability of the fragrance to flow along with its inherent surface tension causes the fragrance material to substantially repose and remain within its locations inside the texture of the barrier coating supplied upon the textured surface 4 . Thus, the mounting surface and the smooth surface create an occlusive, cohesive seal between the surfaces at each location where fragrance materials are applied thus removing the need for any perimeter seal of the product sampler.
[0053] In an alternate embodiment, two opposed textured surfaces, such as 4 , can be used. The high points of each textured surface abut each other and form a liquid retaining seal. Preferably, the two opposed textured surfaces utilize raised cross hatch patterns that seal against each other.
[0054] From the aforementioned description, a product for liquid delivery fragrance samples has been described. The sampler product is uniquely capable of retaining a liquid fragrance sample upon a substrate within a folded cover and without a perimeter adhesive or heat seal. The sampler product may be manufactured from many materials, including but not limited to, paper, cardstock, paperboard, polymers, ferrous and non-ferrous metal foils and their alloys, and composites. | The product for liquid delivery fragrance samples lacks a liquid tight and a vapor tight, perimeter glue band or heat seal. The product comes from easily produced, in-line manufacturing of a commercially printable paper which has an applied barrier coating to defeat permeation by the liquid fragrance material. The product has a substantially irregular, or textured, fragrance sample material mounting and application surface that creates an occlusive, cohesive seal between the substrate layers when fragrance materials are applied. The opposing, textured substrates of the product are in close proximity where the textured surfaces defeat the capillary action of the fragrance sample, and thereby occlude the migration of the fragrance sample out from the product. Also, the inability of the fragrance to flow in conjunction with its inherent surface tension makes the fragrance sample substantially repose within the texture of the barrier coating. Then for usage, the fragrance sample is accessed by a prospective customer who opens a fold or removes a die-cut portion. | 0 |
CROSS-REFERENCE TO RELATED APPLICATION
This application claims priority to and the benefit of Korean Patent Application No. 10-2007-0131600 filed in the Korean Intellectual Property Office on Dec. 14, 2007, the entire contents of which are incorporated herein by reference.
BACKGROUND OF THE INVENTION
(a) Field of the Invention
The present invention relates to a fuel system for a liquefied petroleum injection (LPI) engine, and more particularly to a fuel system for an LPI engine integrally provided with a fuel pump such that the fuel system has less components and manufacturing cost of the fuel system is reduced.
(b) Description of the Related Art
An LPI engine has high power and low emission of pollutants, and alleviates problems of conventional liquefied petroleum gas (LPG) engines such as environmental pollution, low power, and low quality.
An LPI engine injects high pressure liquefied fuel with an injector. That is, a fuel pump is mounted in a fuel tank and supplies fuel to the injector through a fuel line.
Power performance of an LPI engine is substantially the same as a gasoline engine, and fuel consumption and acceleration performance of an LPI engine is good. In addition, startability of an LPI engine is remarkably enhanced.
A supply pipe is mounted between the fuel pump and the injector, and a recovery pipe is mounted between the injector and the fuel tank. Fuel remaining in a combustion process in an engine is recovered to the fuel tank through the recovery pipe. A return valve (check valve) is mounted at the recovery pipe.
According to a conventional fuel system for an LPI engine, noise may occur at the return valve when mixture of liquefied and gaseous fuel is recovered.
The above information disclosed in this Background section is only for enhancement of understanding of the background of the invention and therefore it may contain information that does not form the prior art that is already known in this country to a person of ordinary skill in the art.
SUMMARY OF THE INVENTION
The present invention has been made in an effort to provide a fuel system for an LPI engine having advantages of reducing noise when liquefied and gaseous fuel is recovered.
In addition, the present invention has been made in an effort to provide a fuel system for an LPI engine having further advantages that fuel recovered to a fuel tank is easily supplied to an engine.
A fuel system for an LPI engine according to an exemplary embodiment of the present invention may include: a recovery pipe wherein liquefied fuel mixed with gaseous fuel is recovered therethrough; a reservoir wherein an end portion of the recovery pipe is inserted therein and separates the liquefied fuel from the mixture of the liquefied fuel and the gaseous fuel; a supply pipe wherein an end portion the supply pipe is positioned in the reservoir; and a fuel pump disposed in the reservoir and supplying LPI fuel while the liquefied fuel separated from the mixture of the liquefied fuel and the gaseous fuel is pumped back through the supply pipe by the fuel pump.
The fuel system may further comprise a cover including a first recovery hole and a supply holes wherein the cover substantially encloses an upper portion of the reservoir and the end portion of the recovery pipe is configured to be connected with the reservoir through the first recovery hole and the end portion of the supply pipe is configured to be connected to the fuel pump through the supply hole.
The cover of the fuel system may include at least a gas hole on the cover to release gas.
The first recovery hole of the fuel system may be configured to include a gap between an inner circumference of the first recovery hole and the recovery pipe sufficiently enough to release the gas and/or the supply hole is configured to include a gap between an inner circumference of the supply hole and the supply pipe sufficiently enough to release the gas.
The fuel system of the present invention as an exemplary embodiment may include a first pathway formed in a longitudinal direction of the reservoir from a lower portion of the reservoir, and the liquefied fuel mixed with the gaseous fuel is moved upwardly through the first pathway.
The first pathway may be formed by a partition and a portion of the interior surface of the reservoir along the longitudinal direction of the reservoir.
The fuel system of the present invention as an exemplary embodiment may include a second pathway is connected between the end portion of the recovery pipe and a lower portion of the first pathway, and positioned at the lower portion of the reservoir.
The end portion of the recovery pipe and one end of the second pathway may be connected by a connector opened toward an tipper direction to receive the end portion of the recovery pipe.
The fuel system of the present invention as an exemplary embodiment may include a reservoir cup mounted in the reservoir, wherein a lower surface of the reservoir cup is spaced with a predetermined height from the lower portion of the reservoir by a retainer of the reservoir cup and provided with a groove corresponding to the first pathway and a second recovery hole through which the recovery pipe passes.
The liquefied fuel mixed with the gaseous fuel may be spouted upwardly over the reservoir cup through the first pathway, and thereby the liquefied fuel is separated from the mixture of the liquefied fuel and the gaseous fuel by weight.
The reservoir cup may further include a rim wherein the rim supports the reservoir cup against the reservoir and prevents the liquefied fuel separated from the mixture from overflowing the lower surface of the reservoir cup.
The rim of the reservoir cup may be positioned under or the same level of top portion of the first pathway and configured to be positioned substantially at a center of the reservoir cup and at least a mounting bracket having at least an inlet hole is formed at a upper portion of the retainer to mount the fuel pump and collect through the inlet hole the liquefied fuel separated from the mixture.
As an exemplary embodiment of the present invention, the LPI fuel sucked through a suction hole may be pumped to the supply pipe and a part of the LPI fuel sucked through the suction hole may be merged into the liquefied fuel mixed with the gaseous fuel in the second pathway.
The above features and advantages of the present invention will be apparent from or are set forth in more detail in the accompanying drawings, which are incorporated in and form a part of this specification, and the following Detailed Description of the Invention, which together serve to explain by way of example the principles of the present invention.
BRIEF DESCRIPTION OF THE DRAWINGS
The above and other features of the present invention will now be described in detail with reference to certain exemplary embodiments thereof illustrated the accompanying drawings which are given hereinbelow by way of illustration only, and thus are not limitative of the present invention, and wherein:
FIG. 1 is a perspective view of a fuel system for an LPI engine according to an exemplary embodiment of the present invention;
FIG. 2 is an exploded perspective view of a fuel system of an LPI engine according to an exemplary embodiment of the present invention;
FIG. 3 is a perspective view of a reservoir cup according to an exemplary embodiment of the present invention;
FIG. 4 is a perspective view of a reservoir according to an exemplary embodiment of the present invention; and
FIG. 5 is a cross-sectional view taken along a line I-I of FIG. 2
It should be understood that the appended drawings are not necessarily to scale, presenting a somewhat simplified representation of various preferred features illustrative of the basic principles of the invention. The specific design features of the present invention as disclosed herein, including, for example, specific dimensions, orientations, locations and shapes will be determined in part by the particular intended application and use environment.
In the figures, reference numbers refer to the same or equivalent parts of the present invention throughout the several figures of the drawing.
<Description of Reference Numerals Indicating
Primary Elements in the Drawings>
100:
fuel system
105:
recovery pipe
110:
supply pipe
115:
reservoir
120:
cover
130:
first recovery hole
140:
supply hole
205:
reservoir cup
210:
second recovery hole
215, 215a, 215b:
partition
220:
first pathway
225:
mounting bracket
230:
lower surface
250:
rim
260:
mounting hole
263:
retainer
265:
inlet hole
300:
groove
400:
connector
405:
second pathway
500:
recovered fuel
505:
sucked fuel
520:
suction hole
DETAILED DESCRIPTION OF THE EMBODIMENTS
Hereinafter reference will now be made in detail to various embodiments of the present invention, examples of which are illustrated in the accompanying drawings and described below. While the invention will be described in conjunction with exemplary embodiments, it will be understood that present description is not intended to limit the invention to those exemplary embodiments. On the contrary, the invention is intended to cover not only the exemplary embodiments, but also various alternatives, modifications, equivalents and other embodiments, which may be included within the spirit and scope of the invention as defined by the appended claims.
Hereinafter, referring to the accompanying drawings, a fuel system for an LPI engine according to an exemplary embodiment of the present invention will be described in detail.
FIG. 1 is a perspective view of a fuel system for an LPI engine according to an exemplary embodiment of the present invention.
As shown in FIG. 1 , a fuel system 100 for an LPI engine includes a supply pipe 110 , a recovery pipe 105 , a reservoir 115 and a cover 120 . A first recovery hole 130 and a supply hole 140 is configured to receive supply and recovery pipes 105 and 110 respectively and through the first recovery hole 130 , the recovery pipe 105 is inserted into the reservoir 115 and through the supply hole 140 , the supply pipe 110 is inserted into the reservoir 115 .
A fuel pump (referring to FIG. 5 ) is mounted in the reservoir 115 .
According to the present exemplary embodiment, the fuel pump may be a brush-type motor or a brushless DC motor.
The brush-type motor has a simple structure and is inexpensive, but has drawbacks such as occurrence of cavitations and low durability.
The brushless DC motor has a long life, but has a complex structure and is expensive. The fuel pump mounted in the reservoir is well known to a person skilled in the art so a detailed description will be omitted.
FIG. 2 is an exploded perspective view of a fuel system of an LPI engine according to an exemplary embodiment of the present invention.
As shown in FIG. 2 , the fuel system 100 includes the reservoir 115 and a reservoir cup 205 .
The reservoir cup 205 is mounted in the reservoir 115 . The reservoir cup 205 comprises a rim 250 , a retainer 263 , a second recovery hole 210 , a groove 300 and a lower surface 230 . The retainer 263 comprises one-side opened mounting hole 260 formed at an upper portion of the retainer 263 and positioned substantially at a center portion of the power surface 230 of the reservoir cup 205 . The lower surface 230 of the reservoir cup 205 is spaced from a lower portion of the reservoir 115 with a predetermined height by the retainer 263 .
The fuel pump (referring to FIG. 5 ) is mounted in the retainer 263 and receives liquefied fuel separated from a mixture of the liquefied fuel and gaseous fuel as explained later in detail.
A partition 215 is formed at a portion of an interior surface of the reservoir 115 and complimentarily supported by the groove 300 of the reservoir cup 205 .
In addition, the second recovery hole 210 is formed at a portion of the lower surface 230 of the reservoir cup 205 and the recovery pipe 105 is configured to be inserted into the second recovery hole 210 of the reservoir cup 205 after the recovery pipe 105 passes through the first recovery hole 130 formed at the cover 120 . Therefore, the mixture of liquefied and gaseous fuel recovered through the recovery pipe 105 is moved to a lower portion of the reservoir 115 .
The mixture of liquefied and gaseous fuel moved to the lower portion of the reservoir 115 is flown through a second pathway 405 positioned at the lower portion of the reservoir 115 and spouted upwardly through a first pathway 220 formed by the partition 215 .
FIG. 3 is a perspective view of a reservoir cup according to an exemplary embodiment of the present invention.
As shown in FIG. 3 , the second recovery hole 210 , the groove 300 , and the retainer 263 are formed at the reservoir cup 205 as explained above.
The second recovery hole 210 is formed at the lower surface 230 of the reservoir cup 205 , and the groove 300 has a shape corresponding to the partition 215 formed at the interior surface of the reservoir 115 .
FIG. 4 is a perspective view of a reservoir according to an exemplary embodiment of the present invention.
As shown in FIG. 4 , a connector 400 , a second pathway 405 and the partition 215 are formed at a lower portion of the reservoir 115 .
The connector 400 connects one distal end portion of the recovery pipe 105 and one end of the second pathway 405 . The other end of the second pathway 405 is connected with a distal end portion of the first pathway 220 . The mixture of liquefied and gaseous fuel recovered through the recovery pipe 105 passes through the second pathway 405 into the first pathway 220 .
The partition 215 comprises a first partition 215 a and a second partition 215 b forced at an interior surface of the reservoir 115 and the first pathway 220 is configured to be enclosed by a portion of the interior surface of the reservoir 115 , the first partition 215 a , and the second partition 215 b.
The mixture of liquefied and gaseous fuel recovered through the recovery pipe 105 passing through the second pathway 405 is spouted upwardly through the first pathway 220 .
Once the mixture of liquefied and gaseous fuel is spouted upwardly through the first pathway 220 , the liquefied fuel is separated from the mixture of the liquefied fuel and gaseous fuel by gravity. Then, the separated liquefied fuel flows over the rim 250 of the reservoir cup 205 . Accordingly, the rim 250 of the reservoir cup 205 functions as preventing the separated liquefied fuel from overflowing the reservoir cup 205 , reserving the liquefied fuel until flowing into the retainer 263 of the reservoir cup 205 to make the flown liquefied fuel stable and thus reduces occurrence of cavitations in the separated liquefied fuel.
The liquefied fuel reserved temporarily on the lower surface 230 of the reservoir cup 205 flows into the retainer 263 through at least an inlet hole 265 formed at mounting brackets 225 as show in FIG. 3 . The mounting brackets 225 are formed along a circumference of a mounting hole 260 positioned on a upper portion of the retainer 263 .
The gas separated from the mixture may be released through the first recovery hole 130 and the supply hole 140 of the cover 120 . In another embodiment of the present invention, the cover 120 may have at least a gas hole (not shown) to release the gas more effectively.
Particularly, according to the present exemplary embodiment, noise occurring in separating the liquefied fuel from the mixture of the liquefied fuel and gaseous fuel may be reduced while the recovered fuel passes through the recovery pipe 105 , the connector 400 , the second pathway 405 , and the first pathway 220 . Furthermore, as shown in FIG. 1 , since the cover 120 covers an upper portion of the reservoir 115 , noise may further reduced.
FIG. 5 is a cross-sectional view taken along a line I-I of FIG. 2 .
As shown in FIG. 5 , the recovery pipe 105 penetrates the cover 120 through a first recovery hole 130 (shown in FIG. 1 ) and the reservoir cup 205 through the second recovery hole 210 (shown in FIG.3 ), and is connected to the connector 400 positioned at the lower portion of the reservoir 115 .
In an embodiment of the present invention, a sucked LPI fuel 505 sucked through a suction hole 520 is moved to the fuel pump 510 through a passageway (not shown) positioned at the lower portion of the reservoir 115 . Then the sucked LPI fuel 505 is supplied to the injector by the fuel pump 510 through the supply pipe 110 .
In another embodiment of the present invention, a part of the sucked LPI fuel 505 sucked through the inlet hole 520 may be bifurcated to the second pathway 405 to join the recovered fuel 500 already moved downwardly through the recovery pipe 105 , and then spouted upwardly through the first pathway 220 formed by the partition 215 as explained above.
The mixture of liquefied and gaseous fuel is moved to a space between the lower surface 230 of the reservoir cup 205 and the cover 120 through the first pathway 220 . The liquefied fuel is separated by gravity force from the mixture of the liquefied fuel and gaseous fuel at the space.
As described above, since one end of the recovery pipe is mounted in a reservoir enclosed by a cover, noise may be easily reduced according to an exemplary embodiment of the present invention.
In addition, since a separator that separates liquefied fuel from the mixture of the liquefied fuel and gaseous fuel is integrally formed with the fuel pump, assembly efficiency of a fuel system may be improved and volume of the fuel system may be reduced.
While this invention has been described in connection with what is presently considered to be practical exemplary embodiments, it is to be understood that the invention is not limited to the disclosed embodiments, but, on the contrary, is intended to cover various modifications and equivalent arrangements included within the spirit and scope of the appended claims. | A fuel system for an LPI engine according to an exemplary embodiment of the present invention may include a reservoir disposed in a fuel tank, a recovery pipe inserted in the reservoir, and a fuel pump disposed in the reservoir and supplying LPI fuel, wherein liquefied fuel mixed with gaseous fuel recovered through the recovery pipe is separated in the reservoir and the liquefied fuel is pumped again by the fuel pump. | 5 |
BACKGROUND OF THE INVENTION
[0001] 1. Field of the Invention
[0002] This invention relates to a device for the aquatic farming of molluscs and in particular mussels.
[0003] Historically, like other marine life, mussels have been harvested from the wild, but diminishing stocks, greater demand and the need for a high quality produce have resulted in the growth of a mussel aquaculture industry.
[0004] 2. Discussion of the Prior Art
[0005] Existing mollusc farming devices include a cage-like enclosure with a series of trays, which are seeded with immature molluscs. The enclosure is lowered into the water and left in place until the molluscs mature.
[0006] A much simpler and less expensive method of forming mussels is to seed a weighted rope, which is lowered into the water. The mussels remain attached to the rope as they develop, and are easily harvested by winching up the rope and feeding it through a device for stripping the mussels from the rope. This approach to mussel farming suffers from two serious drawbacks: firstly, mussels are sensitive to changes in water temperature and may detach from the rope if the temperature varies too much over the growing season, and secondly, the small surface area of a rope limits the number of mussels which can be grown on one rope. A device that solves both of these problems would significantly increase the yield and result in a positive economic benefit.
[0007] One attempt to increase the yield of a mussel farming rope is disclosed by Canadian Patent Application 2,130,999 (Hitchins et al) published on Sep. 2, 1993. The inventors propose a funnel-shaped, mesh net to be placed at discrete intervals along a rope to provide support and habitat for the mussels. Several obvious problems are anticipated with the use of such a net, including difficulty in attaching the nets to the rope, and the strong likelihood of entanglements.
GENERAL DESCRIPTION OF THE INVENTION
[0008] An object of the present invention is to provide a device to be used with the rope method of farming mussels which will increase crop yields by providing a greater surface area for attachment and growth of the mussels.
[0009] Another object of the invention is to provide a device that will reduce the loss of mussels by detachment from the mussel rope due to water temperature.
[0010] A further object of the invention is to provide a device, which is easy to use and to attach to a mussel farming rope.
[0011] Accordingly, the invention relates to a mollusc aquaculture device comprising a planar body; an aperture in said body for receiving a rope and a clip in said aperture connected to said body for securing the body at a fixed location on the rope whereby a rope can be inserted through the body into engagement with the clip to affix the body to the rope.
BRIEF DESCRIPTION OF THE DRAWINGS
[0012] The invention is described hereinafter in greater detail with reference to the accompanying drawings, which illustrate preferred embodiments of the invention, and wherein:
[0013] [0013]FIG. 1 is a perspective view from above of an aquacultural device in accordance with the invention;
[0014] [0014]FIG. 2 is a bottom view of the aquaculture device of FIG. 1;
[0015] [0015]FIG. 3 is a side view of the aquaculture device of FIGS. 1 and 2.
[0016] [0016]FIG. 4 is a top view of a second embodiment of the aquacultural device of the present invention;
[0017] [0017]FIG. 5 is a side view of the device of FIG. 4;
[0018] [0018]FIG. 6 is a top view of a third embodiment of the aquacultural device of the present invention;
[0019] [0019]FIG. 7 is a side view of the device of FIG. 6;
[0020] [0020]FIG. 8 is a top view of a fourth embodiment of the aquacultural device of the present invention,
[0021] [0021]FIG. 9 is a side view of the device of FIG. 8;
[0022] [0022]FIG. 10 is a top view of a fifth embodiment of the aquaculture device of the present invention in the open condition;
[0023] [0023]FIG. 11 is a top view of the device of FIG. 10 in the closed or use position;
[0024] [0024]FIG. 12 is a cross section taken generally along line 12 - 12 of FIG. 10;
[0025] [0025]FIG. 13 is an isometric view of a latch used in the device of FIGS. 10 to 12 ;
[0026] [0026]FIG. 14 is a top view of the latch of FIG. 13;
[0027] [0027]FIG. 15 is a cross section taken generally along line 15 - 15 of FIG. 14;
[0028] [0028]FIG. 16 is a perspective view of a sixth embodiment of the device of the present invention;
[0029] [0029]FIG. 17 is a top view of a seventh embodiment of the device of the present invention; and
[0030] [0030]FIG. 18 is an isometric view of a latch used in the device of FIG. 17.
DESCRIPTION OF THE PREFERRED EMBODIMENT
[0031] Referring to FIGS. 1 to 3 , a first embodiment of the aquacultural device includes a disc-shaped, planar body generally indicated at 1 , which is reinforced by a flange 2 , which extends upwardly and downwardly from the periphery of the body 1 . The body 1 is further reinforced by top and bottom ribs 3 and 4 , respectively extending radially between the flanges 2 and the sides of a generally bell-shaped aperture 5 in the center of the body 1 . Additional, arcuate reinforcing ribs 7 (FIG. 2) are provided on both the top and bottom of the body 1 . A slot 8 extends between the outer periphery of the body 1 and a straight end 9 of the aperture 5 , so that a rope 10 (FIG. 1) can be introduced into the aperture. It will be noted that the flange 2 continues along the sides of the slot 8 and around the interior of the aperture 5 . A cylindrical clip 12 is provided in the aperture 5 for securing the body 1 to the rope 10 . The clip 12 is slightly smaller in diameter than the rope 10 for gripping the latter.
[0032] As best shown in FIG. 3, the clip 12 is taller than the flange 2 , providing a large rope gripping surface. The clip 12 is connected to the body 1 on the side of the aperture 5 opposite the slot 8 by an arm 14 , which is reinforced by gussets 15 (FIG. 2).
[0033] The side of the clip 12 facing the slot 8 includes an opening bordered by outwardly diverging, resilient arms 17 , which guide the rope 10 into the clip. Reinforcing flanges 18 extend around the middle of the clip 12 from the gussets 15 to the arms 17 . During insertion of a rope 10 into the clip 12 , the arms 17 flex outwardly into generally V-shaped recesses 20 at the outer, slot end of the aperture 5 , and then return to the rest position (FIG. 2) in which the rope is clamped in the clip.
[0034] It will be appreciated that, in its simplest form, the device of FIGS. 1 to 3 need not include a slot 8 . By making the aperture containing the clip 12 sufficiently large, a rope 10 can be threaded through the body 1 and then pressed into the clip 12 .
[0035] Because most embodiments of the invention have several features in common, in the following description of FIGS. 4 to 11 , the same reference numerals are used to identify elements which are the same or similar to elements shown in FIGS. 1 to 3 .
[0036] Referring to FIGS. 4 and 5, in a second embodiment of the invention, the aperture 5 and the slot 8 more or less define one continuous opening in one side of the body 1 . The inner end of the aperture 5 is defined by a semicylindrical wall 21 , which is integral with the body 1 . The outer, slot end of the clip 12 is defined by the diverging inner ends 22 of a pair of resilient arms 23 . The arms 23 extend inwardly from the outer ends of the slot 8 (i.e. the sides of the outer end of the slot), converging through most of their length, and then being substantially parallel proximate their inner ends 22 . The inner ends 25 of the sides of the slot 8 diverge, leaving room for the arms 23 to move apart when a rope 10 is pressed into the slot. Once the rope 10 enters the aperture 5 , the arms 23 spring back to their rest positions (FIG. 4) to lock the body 1 on the rope.
[0037] The embodiment of the invention illustrated in FIGS. 6 and 7 is virtually identical to that of FIGS. 4 and 5, except that the inner ends 26 of the arms 23 and the inner ends 27 of the sides of the slot 8 , respectively are arcuate.
[0038] With reference to FIGS. 8 and 9, in a fourth embodiment of the invention, the outer side of the clip is defined by the straight inner end 29 of a resilient, L-shaped arm 30 . The arm 30 extends inwardly from one side of the outer end of the slot 8 , and functions in essentially the same manner as the arms 23 (FIGS. 6 and 7) to retain a rope 10 in the aperture 5 . A recess 32 in one side of the inner end of the slot 8 adjacent the aperture 5 receives the inner end 29 of the arm 30 when the latter is displaced during insertion of a rope 10 into the aperture 5 . Once the rope enters the semicylindrical inner end 21 of the aperture 5 , the arm 30 springs back to the rest position (FIG. 8).
[0039] In use, a plurality of the devices are placed at spaced apart locations on a rope suspended in the water. The bodies 1 provide support for immature mussels as they are growing, and reduce the risk of detachment of the molluscs from the rope.
[0040] A fifth embodiment of the invention ( FIGS. 10 to 15 ) includes a disc-shaped body 34 defined by two semi-circular sections 35 and 36 , which are joined on one side by a hinge 37 defined by a thin area of the flange 2 . The flange 2 continues around the periphery of each section 35 and 36 . A plurality of pins or spears 39 extend inwardly from the semicircular central portions 40 of the flange 2 for penetrating a mesh bag 41 , whereby the disc is securely attached to the bag 41 . A plurality of bags 41 and bodies 34 are suspended from a rope (not shown) for growing mussels.
[0041] The two sections 35 and 36 of the body 34 are locked together by a latch indicated generally at 42 (FIG. 11). As best shown in FIGS. 13 to 15 the latch 42 includes a rectangular cross section, arrow-shaped bolt 44 on one section 35 of the body for sliding through a notch 45 in the other section 36 of the body 34 . When the sections 35 and 36 of the body 34 are closed, the bolt 44 enters a loop 47 in a recess 48 in the section 36 . During entry, the resilient head 49 of the bolt 44 is deformed, and then springs back to its original shape to lock the sections 35 and 36 together.
[0042] A pair of alignment pins 51 (FIGS. 10 and 11) also extend outwardly from the straight side of the section 35 . The pins 51 are similar to the bolt 44 , but do not include heads. When the sections 35 and 36 are closed, the pins 51 slide through notches 52 into loops 47 in recesses 48 in the section 36 .
[0043] Referring to FIG. 16, a sixth embodiment of the device of the present invention, which is similar to the device of FIGS. 1 to 3 , includes a hollow, circular body indicated generally at 55 . The body 55 is defined by three concentric rings 56 , 57 and 58 interconnected by radially extending ribs 60 . The inner ends of the ribs 60 support a wall 61 defining a bell-shaped aperture similar to the aperture 5 in the body 1 (FIG. 1). A slot 62 extends between the outer ring 56 and the straight end 63 of the wall 61 for introducing a rope 10 into the central aperture.
[0044] A cylindrical clip 65 is provided in the aperture for securing the body 55 on the rope 10 . The clip 65 is connected to the wall 61 by an arm 66 . Access to the clip 65 is gained via an opening in one side of the wall 61 , which is bordered by outwardly diverging, resilient arms 67 . As in the case of the first embodiment of the invention, when a rope 10 is slid into the slot 62 , the arms 67 are forced apart so that the rope enters the aperture, and then the arms return to the rest position (FIG. 16) so that the wall 61 grips the rope 10 .
[0045] The embodiment of the invention shown in FIGS. 17 and 18 is similar to that of FIGS. 10 to 12 , except that the two sections 70 and 71 of the body are hollow, i.e. they are defined by concentric, semicircular bars 72 , 73 , 74 and 75 interconnected by a plurality of radially extending ribs 76 , and straight inner walls 77 and 78 which abut when the body is closed. The sections 70 and 71 are interconnected by a thin hinge 79 . Pins or spears 80 extend inwardly from the semicircular central areas of the walls 77 and 78 for penetrating a mesh bag 41 , whereby the body is securely attached to the bag.
[0046] The two sections 70 and 71 are locked together in the closed position by three similar latches indicated generally at 81 (FIG. 18). Each latch 81 includes an arrow-shaped bolt 82 extending outwardly form the inner wall 77 of the body section 70 . The head 83 of the bolt 82 includes a longitudinally extending notch 84 in the free end thereof, facilitating flexing of the head during insertion of the head through a notch 86 in the inner wall 78 of the body section 71 , and through a tapering loop or sleeve 87 on the section 71 .
[0047] Referring to FIG. 18, the outermost loop 87 projects upwardly from a plate 88 , which extends from the bottom of the wall 78 . Ribs 90 and 91 extend between the bars 72 and 73 , and the sleeve 87 and the plate 88 , respectively.
[0048] The last embodiment of the invention is used in the same manner as the embodiment shown in FIGS. 10 and 11. The sections 70 and 71 are locked together so that the spears 80 penetrate a mesh bag 41 . The spears 80 can also be used to penetrate a rope for holding the body on a rope. A plurality of bodies are mounted on a bag 41 in this manner, and a plurality of bags are suspended at spaced apart locations from a rope for supporting molluscs. | Mussels are commonly grown on ropes which have been seeded with immature molluscs. Past techniques for farming mussels have suffered from low product yields because of the low surface area of a mussel rope, and mussel detachment from the rope. Existing devices for solving these problems are cumbersome and difficult to use. The present invention solves the problems by providing a mussel farming device including a planar body with a slot in one side thereof for receiving a rope or mesh bag, an aperture at the center of the body, and a clip in the aperture for attaching the body to the rope or bag. A plurality of such devices are attached to a rope or bag at intervals along its length, thereby providing a large surface area for mussel attachment and creating stable platforms on which the mussels can mature. | 8 |
This is a Continuation of application Ser. No. 309,565, filed Oct. 8, 1981, now abandoned.
BACKGROUND OF THE INVENTION
The present invention relates to composite panels for use in the construction industry. As is well known in the art, composite panels have been widely used in the formation of walls and roofs to incorporate heat insulation therein. Known composite panels comprise a core of foamed plastic materials with outer protective skins of, e.g. aluminum foil. Many different foamed plastic materials have been used for the core and the choice of a particular plastic will depend on cost and the physical and thermal insulation properties required. It is an object of the present invention to provide a novel panel comprising a unique facing skin, which imparts considerable physical improvement and protection to the product, a unique plastic foam, and a method of manufacture which facilitates adhesion of the facing skin to that core.
It is a further object of the present invention to provide a new and improved composite building panel. In particular, the present invention provides a composite building panel with significantly improved dimensional stability coupled with increased mechanical strength.
SUMMARY OF THE INVENTION
According to one aspect of the present invention, there is provided a composite building panel comprising a core of rigid foamed plastic material, such as an isocyanurate foam, having secured to its front and back surfaces facing skins, each said facing skin comprising an outer surface of this aluminum foil bonded to a non-woven mat of randomly oriented glass fibers. The core of foamed material is formed in situ between two spaced-apart facing skins using techniques well established in this art. Because the glass fiber mat is non-woven and is a relatively open structure, the foam, as it is formed, expands into and through the mat which ensures adhesion of the outer skin to the foam core, increasing the adhesion of the foil to glass mat.
The glass fiber mat may be formed using conventional wet forming equipment in which the wetted glass mat is formed in the presence of a binder. The weight of glass fiber may be in the region of between about four and thirty pounds per 1,000 square feet, and preferably between about seven and fifteen pounds per 1,000 square feet, depending on the particular type of application of the material. An organic resin binder is used in the formation of the glass mat. The diameter of the glass fibers range between about 6 and 16 microns. The glass fibers are relatively short, having a nominal length between about 1/4 of an inch and 1 inch.
In known composite panels employing facing skins of aluminum foil, the aluminum foil has been a "full hard" temper (non-annealed) foil of about 0.0010 to 0.0015 inch thickness. This foil is difficult to cut during fabrication, and where it is cut, jagged edges remain which are a substantial hazard to the safety of the personnel using the material on the construction site. Moreover, this full hard foil is difficult to process without damaging its surface, i.e., without causing it to wrinkle. As the foil is usually over-printed with technical or commercial information, wrinkling produces an unsatisfactory final product. The danger of users being cut by jagged edges could be avoided by using dead soft aluminum foil of 0.001 inch thickness, but such foil would not have sufficient tensile strength for production purposes, nor would the resultant composite board have sufficient mechanical strength in use.
Further problems have been experienced with full hard aluminum foil covered panels which are easily punctured due to the brittleness of the foil. A panel of this type of foam insulation with a punctured surface will lose insulation value in the area of the puncture quite rapidly. A further problem that has been experienced is the dimensional stability of the prior art composite panels which have exhibited considerable variation in size under the varying conditions of temperature and humidity to which they are exposed in use. This has proved a particularly severe problem in the case of panels used for roofing purposes. In this connection, it has been proposed to improve dimensional stability by forming the core around an ordered array of long, straight, particles of glass fibers, (see U.S. Pat. Nos. 4,028,158 and 4,118,533, to Hipchen, et al.).
Embodiments of the invention employing aluminum foil in the skin have produced an improved fire resistant board, which can be formulated so as to provide a tough, lightweight roof insulation which offers several superior fire resistance ratings. The material in this preferred form comprises outer surfaces of dead soft, fully annealed aluminum foil of approximately 0.0003 to 0.0008 inch (0.0076 mm to 0.025 mm) thickness, with the preferred range being 0.0005 inch to 0.0008 inch (0.0127 mm to 0.025 mm).
The bonding of the glass mat to the aluminum foil imparts considerable surface strength to the foil, greatly improving the overall puncture resistance and resistance to wrinkling. In addition, the glass mat increases the resistance of the board to bending, that is to say, it increases the flexural strength of the composite board. Moreover, the intimate engagement between the foam core and the mat, substantially reduces changes of dimension of the foam which might otherwise occur at extremes of humidity and temperatures. Moreover, since the aluminum is essentially adhered directly to the core, potential delamination problems are avoided.
According to another aspect of the invention, the unique plastic foam core is produced using a polymeric isocyanate which is reacted with itself to form trimer rings and also with a polyester/polyether polyol to form urethane linkages: the resultant plastic foam has unusually low flammability characteristics. The polyether polyol is obtained by alkyloxidation of either plain sucrose, or an amine-sucrose blend with propylene oxide and capped, or chain-terminated, with ethylene oxide. The polyester polyol is obtained from transesterification of dimethylterephthalate process side-streams with various glycols, including diethylene glycol. The polyol blend is comprised of between about 40%-60% dimethylterephthalate/glycol based polyester polyol mixed with between about 60%-40% alkyloxylated sucrose based polyether polyol. The alkyloxylated sucrose polyol provides compatability with the chlorofluorocarbon blowing agent. The polyester polyol provides superior char formation and fire retardancy.
The final relative percentage of isocyanurate trimer rings formed as compared to urethane linkages is controlled by the ratio of chemical equivalents of -NCO (isocyanate) groups to -OH (hydroxyl) groups as well as the catalyzation employed. The plastic core of the present invention may have an isocyanate- to hydroxyl- group ratio in the range of between about 1.8:1 to 6.0:1 and is preferably about 4.0:1.
Composite panels based on an isocyanurate core have been proposed in U.S. Pat. Nos. 4,204,019 to Parker, and 3,903,346 and 3,940,517, both to DeLeon. However, there is no suggestion in any of these Patents of using a polyester/ polyether polyol as the urethane modifier to the isocyanurate. The excellent physical properties of the present foam are not produced using the Parker components, nor the technology described in these U.S. Patents.
DESCRIPTION OF THE DRAWING
The inventions will now be described in more detail with reference to the accompanying drawings in which:
FIG. 1 shows a cross-section through a first insulating panel embodying the invention, and the thickness of the two-ply skins being much enlarged for the purpose of illustration.
DETAILED DESCRIPTION OF THE INVENTION
Referring to FIG. 1, a lightweight roof insulation panel is shown comprising an isocyanurate foam core 11 covered on its upper and lower surfaces by a two-ply skin 13. The skin 13 comprises an inner mat 15 of randomly arranged glass fibers and an outer layer 17 of aluminium foil. The glass fiber mat 15 is fabricated by wet forming the glass fiber mat using glass fibers with diameters between about 6 and 16 microns and between about 1/4 of an inch and 1 inch in length. The wet processing is carried out on a conventional wet forming machine in the presence of an organic resin binder. Thereafter, the two-ply skin 13 is fabricated by adhesion lamination using a conventional casein-latex, polyvinylidene-butadiene, a PVdC-polystyrene copolymer latex emulsion, or a similar type adhesive, to the desired aluminum foil. The aluminum foil used is a dead soft, fully annealed foil approximately 0.0003 inches to 0.0008 inches thick.
The resultant two-ply skin material is then used as upper and lower facing sheets in the continuous formation of laminated boards by in situ foaming of the isocyanurate, using techniques well known in the art and the novel formulation of the present invention.
The foam core is produced from a two component mixture comprised of a polyisocyanate (A component) and a polyol blend (B component) using high pressure impingement mixing techniques. Low pressure mixing equipment could also be used. One of the advantages of this invention is that a polyisocyanurate foam is produced without adding any other material to the polyisocyanate (A component). In the previously referred to isocyanurate core foam patents, U.S. Pat. Nos. 4,204,019, 3,903,346 and 3,940,517, some further component has to be added to the A component blend to produce the polyisocyanurate foam. The advantage of the present invention, therefore, is that existing commercial equipment which has a mixing ratio of 1 to 1 can be used. Therefore, in all discussions following it is understood that the polyisocyanate (A component) is used neat without any mixing or further dilution.
The polyol blend (B component) can be made up in the normal urethane blending fashion which includes adding to the polyol a fluorocarbon blowing agent. The preferred agent is trichlorofluoromethane, CC13F, but other suitable agents such as trichlorotrifluoroethane, CC12FCC1F2, methylene chloride, or water may be used. These various blowing agents can be obtained from DuPont of Wilmington, Del., Allied Chemical Corporation of New York, N.Y., and Kaiser Chemical Company of Oakland, Calif. The blowing agents may be stabilized with an acid scavenger such as monomeric styrene or alloocimine. The polyol blend (B component) also contains a surfactant, which is preferably a silicone-containing polymeric surfactant more preferably from the generic family of polydimethylsiloxane polyoxyalkylene block copolymers.
Another advantage of the present invention is that a surfactant containing hydroxyl (-OH) groups may be used, which increases the range of products from which the surfactant may be selected. Such products are DC-193 from Dow Corning of Midland, Mich., L-5420 from Union Carbide of New York, N.Y., and P-9475 from Pelron Corporation of Lyon, Ill. In the prior art systems, a non-hydrolizable, non-reactive surfactant, i.e, one which does not contain significant -OH groups, must be used, since the surfactant will be added to the A component.
Another component of the polyol blend is the catalyst system which must promote both the urethane reaction and the trimerization reaction of polyisocyanate. It has been discovered that the catalyst system must have both the properties of a tertiary amine and also the properties of an organic salt such as quaternary ammonium compound or else a metal carboxylate salt, such as potassium 2-ethylhexoate or potassium acetate. The preferred organic metal salt is potassium 2-ethylhexoate. This material can be purchased from Mooney Chemicals Incorporated of Cleveland, Ohio with the trade name potassium Hex-Cem 977 which contains 15% potassium in a carrier of diethylene glycol. Another organic compound which can be used as the co-catalyst is a quaternary ammonium compound such as Dabco TMR catalyst produced by Air Products and Chemicals Company of Allentown, Pa. These amine salts are suspended in glycols. The quaternary ammonium salt catalyst provides both the necessary amine content as well as the metallic salt catalytic activity. When the metal carboxylate is used, however, it must have with it a amine catalyst such as 2, 4, 6, trisdimethylaminomethylphenol. This catalyst is sold by the trade name of DMP-30 produced by Rohm & Haas Company of Philadelphia, Pa., P-9529 produced by Pelron Corporation of Chicago, Ill., and EH-300 produced by Thiokol Chemical Corporation of Trenton, N.J. All of these catalyst components must be used in an amount which will promote the reaction required. Typically the amounts to be added are between 0.5% and 3.5% of the polyol blend (B component). A key ingredient in the polyol blend is the unique blend of the polyether polyol and the polyester polyol. The polyester polyol is made from a derivative of the dimethlyterephthalate process. This ester is then transesterified with a glycol, such as diethylene glycol, to produce a compound with an average hydroxyl functionality of between 2.0 and 2.5. Other compounds present which also engage in the transesterification reaction include the aromatic polyesters derived from polycarbomethoxy-substituted diphenyls, polyphenyls and benzyl esters of the toluate family. Such a product may be purchased from Hercules Incorporated, Wilmington, Del. under the trade name TERATE. Preferably TERATE 202 or 203 is used in compounding the base polyol. The other part of the polyol compound consists of a highly alkyloxylated sucrose base polyol. In the past, most alkyloxylated sucrose polyols have had hydroxyl numbers in the range of about 480 to 530. These have produced compounds with rather high viscosities. To overcome the high viscosity of the polyester polyol, it is advantageous to carry the alkyloxylation of the sucrose to a higher level producing lower hydroxyl numbers. This processing tends to lower the viscosity as well as increasing the solubility of this polyol blend in CFC-11.
Examples I and II below are specific examples of component mixtures which can be used to produce the foam core of this invention. Example I produces a -NCO to -OH ratio of 4:1. This ratio is known as a 4 index (or a 400 index. Example II produces an active isocyanate to active hydroxyl ratio of 2:1 to produce a 2 index foam.
EXAMPLE I
(4 Index Foam)
______________________________________ Parts by Weight______________________________________A ComponentPolyisocyanate 189(Rubinate M)B ComponentPolyol 62.5(BM 361-L)Blowing Agent 32.3(K-11B2)Surfactant 2.2(DC-193)Metal Carboxylate 2.3(Hex-Cem 977)Amine, 2, 4, 6, -tris 0.7(dimethylaminomethyl)phenol DMP-30, of Rohm& Haas Company.B Component Subtotal 100TOTAL: 289______________________________________
EXAMPLE II
(2 Index Foam)
______________________________________ Parts by Weight______________________________________A ComponentPolyisocyanate 102(Rubinate M)B ComponentPolyol 67.5(BM 361-L)Blowing Agent 28.0(K-11B2)Surfactant 1.5(DC-193)Metal Carboxylate 2.3(Hex-Cem 977)Amine 0.7(DMP-30)B Component Subtotal 100TOTAL: 202______________________________________
To produce the foam, using the components of either Example I or Example II, the five ingredients of the B component are pre-mixed in a closed vessel at room temperature for at least fifteen minutes. The A component and the mixed B component is then passed, with the A component, through heat exchangers to maintain a temperature of between about 60°-80° F. and preferably in the 70°-75° F. range. The components are then mixed and deposited for foam formation using commercially available equipment, for example, that produced by the Hennecke Machinery Division of Mobay Chemicals. Using such equipment, the laminate board is produced by depositing the mixed A and B components between two spaced-apart continuous webs of the above described two-ply skin material on a laminator having two parallel conveyor belts. A suitable laminator is produced by the Hennecke Machinery Division of Mobay Chemicals. The laminator air and belt temperatures should be between about 120°-200° F. and preferably in the range of 150°-180° F. The resultant board laminate is cut to the desired width and length. Because of the relative lack of hardness of the aluminium foil, as compared with the 0.001 to 0.0015 inch thick foil hitherto used in aluminum foil covered boards, the boardstock which results can be trimmed without the formation of sharp edges which have, heretofore, endangered the safety of construction personnel using the products.
Board produced according to the above described specification and method exhibit excellent dimensional stability and fire resistance, as shown by the ASTM E-84 Flame Spread, the ICBO Room Corner fire test, and the Factory Mutual Calorimeter fire testing. In certain roof construction, the boards are approved for use in attaining the best fire ratings, such as Factory Mutual Class I steel roof deck constructions, or Underwriting Laboratories, Inc., Outline #1256 and Standard #790.
Insulating board produced as described above has been designed specifically for single-ply membrane roofs, but could be used for hot asphalt mopped, built-up roofs, due to its superior surface strength. It can be used directly over steel roof decks without additional gypsum or perlite fire rated base layers. In use, the board can be secured to the roofing deck using hot steep asphalt, cold adhesive or mechanical fasteners. In the case of metal decks, mechanical fasteners would be most appropriate. A superior roof insulation job at the lowest possible cost is obtained using the above described insulating board and a single-ply membrane. Moreover, since the insulating panel is foil covered, a slip sheet may not be required between the insulation and the single-ply membrane.
In addition to the particularly advantageous product obtained using the unique core material in combination with the unique facing material as described above, the present invention also encompasses the use of the unique core with other facing materials. For example, the core 11 above can be bonded on one board side to a facing skin of 0.001 inch aluminum foil which has been properly prepared with an organic coating, and to the unique two-ply aluminum foil/fiber glass material on the other board side. This board has cost advantages over the product with foil/glass on both sides, but the physical properties of the product with glass/foil skin on both sides are better. Similarly, if damage resistance is not as important, useful board can be produced by laminating 0.001 inch aluminum foil to both sides of a core produced as the core 11 described above. | A composite panel for use in the construction industry includes a core of foamed plastic material and a skin on at least one of its faces comprised of a two-ply material consisting of aluminum foil bonded to a mat of randomly oriented glass fibers into which the foam core has been expanded.
The core material comprises the rection product of isocyanurate and polyester/polyether polyol with the isocyanurate in sufficient excess to form trimmer rings and to react with the polyol to form urethane linkages.
Panels formed of the core material and the two-ply skins have excellent thermal insulation and fire retardant properties and the skins have excellent mechanical strength. | 1 |
BACKGROUND OF THE INVENTION
The invention relates to an apparatus for detecting leakages in structural members.
The detection of leakages in structural members is absolutely necessary both in quality inspection in manufacture and also in operation. The detection of leakages in structural members which are used in an environment with low or excess pressure is particularly critical.
Processes and apparatuses for leakage detection which are nowadays customary and are used in particular in manufacture are either expensive, difficult to operate, too imprecise or use toxic media for the detection of leakages, which is problematical because of the danger to service personnel and the environment.
SUMMARY OF THE INVENTION
The object of the present invention is therefore to create an apparatus for the detection of leakages in structural members which is relatively cheap, can be operated easily, in an environmentally friendly manner and without danger to the service personnel and also operates without contact and precisely.
This object is achieved with an apparatus which in accordance with the invention comprises a device for conveying gas through the structural element to be tested, a camera having a narrow band filter characteristic substantially matched to the spectral properties of the gas and a device connected to the camera for processing and displaying the recorded image of the structural member to be tested.
The apparatus specified by the invention, which is particularly suitable for testing hollow structural members, offers a clear detection and localization of leakage points on the basis of the optical detection and the subsequent opto-electronic image processing. Thus the apparatus according to the invention operates in a particularly precise manner. Moreover the apparatus specified by the invention is easy to operate as it works without contact and can be easily adapted to any change in the test environment. Finally the apparatus according to the invention operates in an environmentally friendly manner, and moreover there is no danger to service personnel, as a gas generally recognized as being safe may be used. The advantages mentioned are achieved in accordance with the invention by making absorption operations of gases emerging at a leakage point of the test piece visible with the help of a camera, which comprises a narrow band filter substantially matched with the spectral properties of the gas or corresponding filter properties. As in accordance with the invention the sensitivity of the camera is precisely limited to the absorption bands of the test gas to be detected, a high radiation contrast between the escaping gas and its environment or its background can be achieved.
The optical detection of the gas escaping at leakage points can be further intensified with light by an illumination device for the illumination of the structural member to be tested, with the wave length of the light being substantially matched to the spectral properties.
The apparatus preferably operates in the infrared range.
CO 2 , N 2 O or SF 6 , for example, is expediently used as a gas generally recognized as safe in the previously encountered definition.
The gas conveying device comprises a flowmeter for the quantitative assessment of the leakage point.
The gas conveying device expediently conveys the gas under pressure through the structural member to be tested.
The structural member to be tested and the camera may preferably moved in relation to one another for the most complete detection possible from all perspectives.
BRIEF DESCRIPTION OF THE DRAWINGS
A preferred exemplified embodiment of the invention is explained in further detail below by means of the attached drawing, in which a schematic block diagram of a preferred design of the apparatus for detecting leakages is represented.
DETAILED DESCRIPTION
As can be seen from the attached drawing, a gas conveying device 2 is provided, which inter alia comprises a flowmeter 4 and also a container 6 with a test gas. CO 2 , SF 6 or N 2 O is preferably used as the test gas. The gas conveying device 2 also comprises a hose, a pipe or another connection means through which the test gas is conveyed into the test piece 8, which in the attached drawings is indicated by the arrow 9.
An illumination device 10, which comprises a quartz projector for example, is also provided. The test piece 8 is irradiated during the test operation by means of the illumination device 10.
A photographic device 12 comprises an infrared camera 14, which preferably operates in the wavelength range of from 1 to 5 μm 8 to 12 μm. The infrared camera 14 is provided with a narrow band filter adapted to the test gas, by which the generally broad band spectral sensitivity of the camera 14 is precisely limited to the absorption bands of the test gas to be detected. If CO 2 , for example, is used as the test gas, the infrared optics should be adapted by the filter to a central wavelength of 4.26 μm. The same also applies for the illumination device, which should preferably produce infrared light with an effective wavelength of roughly 4 μm.
At this juncture it should be pointed out that instead of a filter the infrared optics of the camera 14 may alternatively also be designed so that it possesses the required filter properties itself.
The use of the apparatus described is likewise not limited to infrared. The use of electromagnetic radiation of other wave lengths also appears possible. Furthermore any other detector may be used instead of an optical camera to detect light.
The optical detection device 12 also comprises an integrated or removed image processing device 16 for producing optimal picture quality in black/white or colour and also for the automatic detection of the test gas escaping from a leakage point and the determination of the origin of the leakage by variance comparison or image evaluation adapted to the situation.
A monitor 18 for representing the test piece and the test result with the cloud of gas escaping from the test piece is connected to the image detection device 12.
A data logging device 20 is also provided, which is connected to the data processing device 16 and the flow meter 4 and comprises interfaces for telecommunication and data banks.
The course of the test operation using the apparatus represented is described below.
The test gas contained in the container 6 of the gas conveying device 2 is conveyed into the test piece 8 via corresponding hoses, pipes or other connecting means. This normally occurs under pressure, with the test pressure being adapted to the test piece specifications.
For the opto-electronic recording of the test piece 8 and possible leakage sits, the infrared camera 14 is guided either manually or automatically around the test piece 8 or the test piece 8 itself is moved in front of the camera. The illumination device 10 is either mounted on the camera 14 or is disposed in the vicinity thereof in order to illuminate the test piece 8 with infrared light in the picture detail to be recorded by the camera 14.
The generally wide band spectral sensitivity of the infrared camera 14 is precisely restricted in the aforementioned manner to the absorption bands of the test gas to be detected, so that the highest possible radiation contrast between the escaping cloud of gas 22 and its environment or respectively the background is guaranteed. The radiation contrast is assisted by the external illumination by means of the illumination device 10, which in addition to the thermal characteristic radiation of the test piece under consideration increases the radiation intensities via the detection sensitivity threshold of the camera 14 increased by the filter. This infrared image recorded by the camera 14 is visible as a result of absorption and emission phenomena in the test gas 22.
All images recorded by the camera 14 or alternatively only the images with the leakage sites, which are made visible in the infrared image by escaping test gas 22, are processed, stored and if necessary evaluated by the data processing device 16 and can be represented on the monitor 18. The image representation on the monitor may be in black/white or in colour, preferably in "false colour", with it being possible to mark the cloud of test gas escaping at the leakage point.
The data relating to the recorded images is further processed and transmitted in the data logging device 20, and any leakage points detected may be marked in a special way, for example.
The flow meter 4 is used for the quantitative evaluation of the leakage site, and its measured values are also processed and transmitted by the data logging device 20. | An apparatus for detecting leakages in structural members (8) is disclosed. The apparatus includes a device (2) for conveying gas through the structural member (8) to be investigated, a camera (14) having a narrow band filter characteristic matched to the spectral absorption of the gas and a device (16, 18) connected to the camera (14) for processing and displaying the recorded image of the structural member (8) to be investigated. | 6 |
CROSS REFERENCES TO RELATED APPLICATIONS
This application is a Continuation of application Ser. No. 12/620,667, filed Nov. 18, 2009, and is expressly incorporated herein by reference. The entire disclosure of Japanese Patent Application No. 2008-314469, filed Dec. 10, 2008, is expressly incorporated herein by reference.
BACKGROUND
1. Technical Field
The present invention relates to a recording apparatus such as a facsimile machine or a printer, and more particularly, to a recording apparatus including a drier for accelerating the drying of a recordable medium.
2. Related Art
Hereinafter, a printer will be described as an example of a recording apparatus. In particular, as described in Japanese Patent No. 3075329, there is provided a printer for heating a recording sheet by a heater, evaporating moisture included in the recording sheet, and exhausting air including moisture by an exhauster. JP-A-2002-292841 discloses a printer including a drier for drying an ink landing on a sheet by ejecting hot air onto the sheet.
Even when the heater and the exhauster are included in order to accelerate the drying of the sheet as in the printer described in Japanese Patent No. 3075329 or even when hot air is ejected onto the sheet as in the printer described in JP-A-2002-292841, turbulence (turbulent flow) of air stream occurs at the periphery of the sheet. If the turbulent flow occurs at an end of the sheet, floating (curling) of the end of the sheet occurs and thus recording quality may deteriorate. Such a technical problem is not sufficiently considered in the existing printers including the printers of Japanese Patent No. 3075329 and JP-A-2002-292841.
SUMMARY
An advantage of some aspects of the invention is that suitable recording quality is attained by preventing turbulence of air stream from occurring at an end of a sheet and preventing the end of the sheet from floating (curling).
According to an aspect of the invention, there is provided a recording apparatus including: a recording unit for performing recording on a recordable medium; a transportation unit transporting the recordable medium; and a drier accelerating the drying of the recordable medium by ejecting gas onto the recordable medium, wherein the drier is configured such that the ejection range of the gas in a direction perpendicular to the transportation direction of the recordable medium is changeable.
According to the present aspect, since the recording device includes the drier accelerating the drying of the recordable medium by ejecting the gas onto the recordable medium and the drier is configured such that the ejection range of the gas in the direction (hereinafter, referred to as “the width direction of the recordable medium”) perpendicular to the transportation direction of the recordable medium is changeable, the ejection range can be adjusted according to the width of the recordable medium.
That is, for example, if the ejection range is large with respect to the width of the recordable medium, turbulent flow occurring in the side end of the recordable medium and thus the side end is apt to float (curl). However, since the ejection range can be adjusted according to the width of the recordable medium, it is possible to prevent the side end of the recordable medium from floating (curling) by the turbulent flow. In addition, it is possible to prevent the temperature of the heated recordable medium from being reduced by the turbulent flow.
The drier forms air stream from the center to the side end of the recordable medium in the direction perpendicular to the transportation direction of the recordable medium.
By this configuration, since the drier forms the air stream from the center to the side end of the recordable medium in the direction perpendicular to the transportation direction of the recordable medium, the gas escapes outwardly straight. Accordingly, it is possible to efficiently prevent the side end of the recordable medium from floating (curling) by the gas ejected from the drier.
In addition, after the gas is ejected onto the recordable medium, it is possible to reduce the distance of the gas moved to the outside of the recordable medium. Accordingly, when moisture is emitted from the recordable medium, it is possible to rapidly separate air including moisture from the recordable sheet, to suppress air including moisture from being moved to the downstream side even when the recordable sheet is transported at a high speed, and to prevent the recording unit (for example, an ink jet recording head) or the peripheral configuration thereof from bedewing with certainty.
In an air ejection port of the drier, a shutter member covering both sides of an ejection port in the direction perpendicular to the transportation direction may be displaceably provided in the direction perpendicular to the transportation direction, and the shutter member may be displaced such that the ejection range is changed.
By this configuration, since the shutter member which is displaceable in the width of the recordable medium is displaced such that the ejection range is changed, it is possible to configure the drier, in which the ejection range is changed, with low cost.
The drier may include a plurality of blast sources in the direction perpendicular to the transportation direction, and at least some of the plurality of blast sources may be displaced in the direction perpendicular to the transportation direction such that the ejection range is changed.
By this configuration, since the plurality of blast sources is included, at least some of the blast sources are displaceable in the width direction of the recordable medium. Since the blast sources are displaced such that the ejection range is changed, it is possible to adjust the gas ejection strength of the blast sources. Accordingly, it is possible to prevent the side end of the recordable medium from floating with more certainty, that is by setting the gas ejection strength from the blast sources disposed at the end of the recordable medium in the width direction to be strong.
BRIEF DESCRIPTION OF THE DRAWINGS
The invention will be described with reference to the accompanying drawings, wherein like numbers reference represent like elements.
FIG. 1A is a side view showing the main portions of a printer according to a first embodiment of the invention and FIG. 1B is a plan view thereof.
FIG. 2 is a cross-sectional view of a drier (first embodiment).
FIG. 3 is a cross-sectional view of a drier (second embodiment).
FIG. 4 is a cross-sectional view of a drier (third embodiment).
FIG. 5 is a cross-sectional view of a drier (fourth embodiment).
FIG. 6A is a side view showing the main portions of the printer according to the first embodiment of the invention, and FIG. 6B is a side view showing the main portions of a printer according to a fifth embodiment of the invention.
DESCRIPTION OF EXEMPLARY EMBODIMENTS
Hereinafter, the embodiments of the invention will be described with reference to the accompanying drawings. FIG. 1A is a side view showing the main portions of an ink jet printer (hereinafter, referred to as a “printer”) 1 as a recording apparatus according to a first embodiment of the invention, FIG. 1B is a plan view thereof, FIG. 2 is a cross-sectional view of a drier 12 A (first embodiment), FIG. 3 is a cross-sectional view of a drier 12 B according to another embodiment (second embodiment), FIG. 4 is a cross-sectional view of a drier 12 C according to another embodiment (third embodiment), FIG. 5 is a cross-sectional view of a drier 12 D according to another embodiment (fourth embodiment), FIG. 6A is a side view showing the main portions of the printer 1 according to the first embodiment of the invention, and FIG. 6B is a side view showing the main portions of a printer 1 ′ in which a transportation unit is replaced with another embodiment.
In addition, hereinafter, a direction (a vertical direction of FIG. 1B and a horizontal direction of FIGS. 2 to 5 ) perpendicular to a sheet transportation direction (a horizontal direction of FIGS. 1A and 1B ) is referred to as a “sheet width direction”, for convenience of description.
First Embodiment
Hereinafter, a first embodiment of the invention will be described with reference to FIGS. 1 and 2 .
The printer 1 according to the present embodiment is a so-called line head type high-throughput ink jet printer including an ink jet type recording head (recording unit) 10 with a length covering a sheet width, and ejects inks from the recording head 10 while moving a recording sheet P as an example of a recordable medium in a sheet transportation direction so as to execute recording, without reciprocally moving an ink ejecting head in the sheet width direction.
In more detail, the printer 1 has a gate roller 7 on the upstream side of a transportation unit 2 . By the gate roller 7 , skew is eliminated before feeding the recording sheet P to the transportation unit 2 and the recording sheet P is then fed to the transportation unit 2 disposed on the downstream side.
A transportation belt 3 which forms a transportation surface for transporting the recording sheet P and the transportation unit 2 including a plurality of rollers (a driving roller 4 and driven rollers 5 and 6 ), around which the transportation belt 3 is wound, are provided on the downstream side of the gate roller 7 . The transportation belt 3 has a plurality of suction holes 3 a . The recording sheet P is sucked by a suction device 8 through the suction holes 3 a (in a direction denoted by an arrow of FIG. 1A ), and is transported in a transportation direction with certainty.
The recording head 10 for ejecting inks is provided at a position facing the transportation surface of the transportation belt 3 . In the recording head 10 , a plurality of heads 10 a is arranged in a zigzag shape in the sheet width direction. In each of the heads 10 a , ink nozzles (not shown) of respective colors such as yellow, magenta, cyan and black are arranged so as to be shifted from each other in each of the colors in the transportation direction of the recording sheet P. The inks are supplied from ink tanks (not shown) of the respective colors to the ink nozzles (not shown) through ink supply tubes (not shown).
A necessary amount of ink droplets is ejected from the ink ejecting nozzles such that minute ink dots are formed on the recording sheet P. This operation is performed with respect to the respective colors and thus recording is completed by once passing the recording paper P sucked to the transportation belt 3 .
Next, the drier 12 A is provided in the vicinity of the upstream side of the recording head 10 . The drier 12 A, which includes a blast fan 18 and a heater 19 , introduces outdoor air into the apparatus, heats the outdoor air to hot air (dried air), and sends the hot air to the inside of a case 13 through a taking-in port 16 of the case 13 as shown in FIG. 2 .
The hot air is ejected from an ejection port 17 a formed in the lower portion of the case 13 toward the recording sheet P so as to increase the temperature of the recording sheet P and evaporate residual moisture such that the drying after the inks are ejected is accelerated. In FIG. 2 , the arrows denote the flow directions of the hot air in the respective portions.
Blades 20 functioning as a shielding member are provided on the transportation-direction upstream and downstream sides of the ejection port 17 a . By the blades 20 , the hot air ejected from the ejection port 17 a is shielded so as not to be leaked in the sheet transportation direction and more particularly to the side (downstream side) of the recording head 10 .
Accordingly, air including moisture emitted from the recording sheet P is not moved to the side of the recording head 10 or the movement thereof is reduced so as to prevent the recording head 10 or the peripheral configuration thereof from bedewing. If air including moisture flows in an opposite direction (upstream direction) of the recording head 10 , the moisture may be absorbed by the recording sheet P again, but such a problem can be prevented.
A deflector 15 for spreading the received hot air in the sheet width direction is provided in the case 13 , and a plurality of louvers (louver boards) 14 A for regulating the ejection direction of the hot air is provided on the lower side thereof along the sheet width direction. An angle (hereinafter, referred to as an “inclined angle”) between the board surface of each of the louvers 14 A and the recording surface of the recording sheet P is substantially set to 90° such that the hot air is linearly ejected from the ejection port 17 a onto the recording surface of the recording sheet P.
The drier 12 A includes exhaust ports 17 b in both ends thereof in the sheet width direction, in addition to the ejection port 17 a . The flow rate of the hot air ejected from the ejection port 17 a may be easily adjusted (reduced) by the exhaust ports 17 b . In addition, a throttle (not shown) for adjusting the size of the opening of each of the exhaust ports 17 b is provided such that the flow rate of the hot air ejected from the ejection port 17 a can be adjusted with higher accuracy.
In addition, since the exhaust ports 17 b disposed outside the sheet side end of the recording sheet P which are supposed to be used with a largest sheet width (are disposed outside the transportation belt 3 ) and are opened toward the outer direction of the sheet side end, it is possible to prevent turbulent flow of the hot air exhausted from the exhaust ports 17 b from occurring at the peripheral end of the sheet and thereby prevent the sheet side end from floating (curling) by the turbulent flow.
Next, movable plates (shutter) 21 for covering the ejection port 17 a are provided on both sides of the ejection port 17 a in the sheet width direction. The movable plates 21 are slidably provided in the sheet width direction, and the hot air ejection range from the ejection port 17 a can be adjusted according to the width dimension of the recording sheet P.
That is, if the width of the recording sheet P is large, the movable plates 21 are moved in the outer direction and, if the width is small, the movable plates 21 are moved in the center direction, such that the adequate hot air ejection range suitable for the width of the recording sheet P can be set. For example, the hot air ejection range may correspond to the width of the recording paper P. Accordingly, it is possible to prevent the turbulent flow of the hot air from occurring in a region deviating from the end of the sheet and to prevent the sheet side end from floating (curling) by the turbulent flow with certainty. In addition, it is possible to prevent the temperature of the preheated sheet (the recording sheet P is heated before recording) from being lowered by the turbulent flow.
Although one hot air drier 12 A (ejection port 17 a ) is included in the above-described first embodiment, a plurality of hot air driers may be disposed on the sheet transportation direction such that the drying is accelerated by the plurality of hot air driers 12 A (ejection ports 17 a ). In this case, the blade 20 interposed between two hot air driers 12 A (ejection ports 17 a ) may be omitted.
Second Embodiment
Hereinafter, a second embodiment of the invention will be described with reference to FIG. 3 . In addition, in the following embodiments including the present embodiment, the same configurations as the first embodiment described with reference to FIGS. 1 and 2 are denoted by the same reference numerals and the description thereof will be omitted.
In the drier 12 B according to the present embodiment, the inclined angles of louvers 14 B are set to be reduced (lie down to the paper) from the center to the end of the sheet width direction, and air stream is formed from the center to the side end of the sheet in the sheet width direction as denoted by arrows on the paper. Accordingly, air ejected from the drier 12 B escapes from the sheet side end outwardly straight. Thus, it is possible to prevent turbulent flow from occurring in the sheet side end and to prevent the sheet side end from floating (curling).
Since air stream is formed from the center to the side end of the sheet width direction, it is possible to reduce the distance of the hot air from the sheet end outward direction after ejecting the hot air onto the recording sheet P. Accordingly, it is possible to rapidly separate air including moisture, which is emitted from the recording sheet P, from the recording sheet P, to suppress air including moisture from being moved to the downstream side; that is, the side of the recording head 10 even when the recording sheet P is transported at a high speed, and to prevent the recording head 10 or the peripheral configuration thereof from bedewing with certainty.
Third Embodiment
Hereinafter, a third embodiment of the invention will be described with reference to FIG. 4 . The hot air drier 12 C shown in FIG. 4 includes an edge regulating plate 22 for pressing the side end of a sheet. The edge regulating plate 22 is slidably provided in the sheet width direction, and an edge regulation position can be adjusted according to the width of the recording sheet P. Accordingly, even when the turbulent flow of hot air is generated in a region deviated from the end of the sheet, it is possible to prevent the sheet side end from floating (curling) by the turbulent flow with certainty. In addition, the edge regulating plate 22 is applicable to the above-described first and second embodiments or the following other embodiments.
Fourth Embodiment
Hereinafter, a fourth embodiment of the invention will be described with reference to FIG. 5 . The hot air drier 12 D shown in FIG. 5 includes a plurality of hot air units 23 and 24 as a blast source. Each of the hot air units individually includes a blast fan 18 and a heater 19 , and can set the temperature of hot air and an ejection speed. Accordingly, it is possible to prevent the sheet side end from floating by setting the flow rate of the hot air from the hot air units 24 disposed at both ends of the sheet width direction to be slightly high.
The hot air unit 23 is fixedly provided at the center of the sheet width direction, and the hot air units 24 disposed at both ends of the sheet width direction are slidably provided in the sheet width direction. That is, since the hot air ejection range from the ejection port 17 a can be adjusted according to the width of the recording sheet P, it is possible to prevent the turbulent flow of the hot air from occurring in a region deviating from the end of the sheet and to prevent the sheet side end from floating (curling) by the turbulent flow with certainty.
In addition, even when all the hot air units are fixedly provided, it is possible to prevent the sheet side end from floating by setting the flow rate of the hot air of the hot air units of both ends to be slightly high.
Fifth Embodiment
Hereinafter, a fifth embodiment of the invention will be described with reference to FIG. 6 . FIG. 6A shows the printer 1 according to the above-described first embodiment and FIG. 6B shows a printer 1 ′ according to the present embodiment in which the transportation unit 2 is replaced with another embodiment (transportation unit 2 ′).
In FIG. 6A , the hot air ejected from the ejection port 17 a of the drier 12 A is prevented from being leaked to the upstream side and the downstream side of the transportation direction by the blade 20 . However, if the hot air is leaked to the downstream side of the transportation direction and thus the turbulent flow is formed between the recording head 10 and the drier 12 A, the front end of the recording sheet P floats as denoted by a reference numeral Ps and collides with the recording head 10 such that the recording surface is contaminated.
Accordingly, in the transportation unit 2 ′ according to the present embodiment, as shown in FIG. 6B , a plurality of suction units 8 A and 8 B is disposed along the transportation direction, and the sheet suction force of the downstream suction unit 8 B is set to be stronger than the sheet suction force of the upstream suction unit 8 A.
The sheet suction of the downstream suction unit 8 B is configured to be immediately performed after passing the drier 12 A. Accordingly, even when the turbulent flow is formed between the recording head 10 and the drier 12 A, it is possible to prevent the front end of the recording sheet P from floating by the turbulent flow and colliding with the recording head 10 and to prevent the recording surface from being polluted. By decreasing the sheet suction just below the drier 12 A, it is possible to suppress the decrease in the temperature of the recording sheet P and to prevent the drying effect of the drier 12 A from being lowered.
The above-described embodiments are portions of the embodiments of the invention, and the range of the invention is not limited thereto. Embodiments obtained by property combining the characteristic configurations of the embodiments may be employed. | Provided is a recording apparatus including: a recording unit for performing recording on a recordable medium; a transportation unit for transporting the recordable medium; and a drier for accelerating the drying of the recordable medium by ejecting gas to the recordable medium, wherein the drier is configured such that the ejection range of the gas in a direction perpendicular to the transportation direction of the recordable medium is changeable. | 1 |
FIELD OF THE INVENTION
This invention is related to an auxiliary tool for cable hauling which is used to link a cable tip end with a hauling means at a laying site of communication cable such as an optical fiber cable or other cable such as an electrical wire.
BACKGROUND OF THE INVENTION
The demand for communication network construction has increased steadily with multimedia development in recent years. Especially, in communication networks such as CATV and intranets, optical fiber cables are generally used because their capacity and communication speed are excellent.
As shown in FIG. 8, a tension member 51 of an optical fiber cable 5 is connected to a connecting tool 7 for cable hauling. Connecting tool 7 is linked with hauling means such as a winch, and then optical fiber cable 5 is hauled at a laying site thereof. When the tension member 51 is connected to the connecting tool 7 , a tip end of the tension member 51 is inserted into a tip end insertion hole 71 , and restraint portion 72 is clamped using specialized equipment, thereby restraining the tip end of the optical fiber cable 5 . The restraint portion 72 has such a small diameter that it has to be clamped by specialized equipment under high pressure. As a result, the tip end of tension member 51 will not disconnect from connecting tool 7 , even if it is hauled with a traction of approximately 800 Kgf.
However, the above-described specialized clamping equipment cannot be used at the laying site of the cable. A cable that is cut at the laying site cannot be connected to the connecting tool. A tip end of the cable, which is exposed by cutting, will be difficult to link to a hauling means with sufficient restraint force.
In the case of delivered cable that has already been connected to a connecting tool by clamping with specialized equipment, such connecting tool may not be suitable for use at certain laying sites because of the diameter of its laying tube. If unable to be used, the connecting tool will have to be cut off from the cable tip end.
Further, this connecting tool is too long to turn in a 90° bend of the laying tube, which is turning up from a horizontal tube to a vertical tube.
The object of the present invention is to solve the above mentioned problems. The invention provides an auxiliary tool for cable hauling capable of constraining a cable tip end which is exposed due to cutting off at a cable laying site, with sufficient restraint force to withstand a hauling force, and can be used even at a laying site where the pipe diameter size is small.
SUMMARY OF THE INVENTION
In the present invention, an auxiliary tool for cable hauling is provided which links a cable tip end with a hauling means to haul said cable for laying comprising: a container containing a cable tip end; a linkage interconnected with said hauling means, said linkage being connected to said container; a restraint means restraining said cable tip end; wherein said restraint means is contained and held in said container in such a manner that said restraint means restrains said cable tip end. Since neither the cable tip end nor the restraint means thereof is exposed, both are out of contact with the inner wall of the laying tube. Furthermore, problems such as hooking or breaking off will not occur. The cable tip end is linked with the hauling means by a linkage tool, providing a reliable and strong linkage.
Further, an auxiliary tool for cable hauling is provided which comprises: a container containing said cable tip end; a linkage interconnected with said hauling means, said linkage being connected to said container; a restraint means restraining said cable tip end; said container being divisible into a tip end container portion and a linking portion, said tip end container portion containing an inserted cable tip end, said linking portion being connected to a linkage. After a cable tip end is restrained by restraint means, it is installed in the container easily.
Furthermore, if a restraint member which is a different body from said container and is freely rotatable is used as the restraint means, it will efficiently prevent twists while cable hauling.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is an exploded perspective illustration which shows the structure of an auxiliary tool for hauling cable of Embodiment 1.
FIG. 2 is side sectional view which illustrates a condition of the cable tip end restrained by an auxiliary tool for hauling cable of Embodiment 1.
FIG. 3 is a graph which compares restraint forces of restraint means of this embodiment and of prior art.
FIG. 4 is a perspective view of another restraint member.
FIG. 5 is a perspective view of the connecting portion of an auxiliary tool for hauling cable of Embodiment 2.
FIG. 6 is an exploded perspective illustration which shows the structure of an auxiliary tool for hauling cable of Embodiment 3.
FIG. 7 is a side section which describes a condition of an auxiliary tool for hauling cable connected to the tip end thereof.
FIG. 8 is a partial cutaway view of connecting toll for hauling cable of a prior art.
DETAILED DESCRIPTION OF THE INVENTION
The present invention provides an auxiliary tool which restrains the tip end of a cable to link with hauling equipment at a laying site of communication line, such as optical fiber cable or an electrical wire, passing through a pulley or laying tube.
The auxiliary tool for hauling comprises a container, a restraint means which is installed in the container, and a linking member which interconnects to hauling equipment. The container utilizes a compact design for smooth hauling in a narrow groove of a pulley or laying tube.
Preferably, a restraint member is used as a restraint means. The restraint member is freely rotatable around the axis along the cable tip end, and therefore, twisting of the cable while hauling thereof is eliminated. In most cases, when a linking portion which is interconnected with hauling equipment contacts the groove wall of a pulley or inner wall of a laying tube, the linking portion rotates. However, rotation of the linking portion does not convey to the restraint member. The restraint member restrains the tip end of the cable and is not stressed because it is freely rotatable as mentioned above. The cable is thereby prevented from separating during hauling.
Various types of restraint members may be used. For example, restraint members may have insertion spaces to insert a cable tip end, such as insertion holes or insertion hollows as described later. To achieve the object of the invention, restraint members of a variety of sizes are selected depending on the type of cable, and a suitable type of container for the selected restraint member is used. Cable can be installed utilizing a narrow existing laying tube having 20 mm diameter or less, up to a big sub-ground tube having a diameter of more than 500 mm.
Further, in addition to only one cable being hauled by one auxiliary tool, a plurality of cables, such as a combination of a communication cable and an electrical wire, are capable of being hauled simultaneously by one auxiliary tool if a proper restraint member is selected. Particularly, although the restraint portion could potentially be easily twisted because of unequal tension forces existing when a plurality of cables are hauled, an auxiliary tool can be used to eliminate this twist. As a result, the effect of the invention is more efficiently achieved.
Embodiment 1
In Embodiment 1, a restraint member restrains a cable tip end as a means of restraining a cable, and the restraint member is put in a container. Thereby, the cable tip end is restrained in the container.
As shown in FIG. 1, an auxiliary tool 1 for hauling cable consists of container 2 , a linkage 3 and a restraint member 4 . The container 2 comprises a tip end container portion 2 a , which cable tip end is inserted and stored therein, and a linking portion 2 b , to which linkage 3 is joined. The linkage 3 is joined with container 2 and links with a hauling means. The restraint member 4 restrains a cable tip end and is installed in container 2 . The tip end container portion 2 a and the linking portion 2 b are secured to each other by threads 21 a and 21 b . The restraint member 4 includes restraint metal fitting 40 and clamping members 42 a and 42 b (Refer FIG. 2 ). The restraint metal fitting 40 is held on the end of thread 21 a when tip. end container portion 2 a and linking portion 2 b are secured to each other and tension is loaded on the cable tip end. The restraint metal fitting 40 is freely rotatable about an axis of the cable tip end.
The restraint metal fitting has six insertion holes 41 . A cable tip end is inserted through the insertion holes 41 and is restrained by clamping of clamping members 42 a and 42 b as described below. Therefore, the restraint metal fitting 40 is installed in the container 2 after restraining the cable tip end, and then the cable tip end is restrained by the auxiliary tool 1 .
The diameter of restraint metal fitting 40 is slightly smaller than the inner diameter of container 2 therearound. Therefore, the restraint metal fitting 40 is freely rotatable about an axis of the cable tip end in the container 2 . Accordingly, even if the cable twists while hauling thereof, the twist will be eliminated by rotation of restraint metal fitting 40 . The cable tip end restrained by the restraint metal fitting is not stressed and is prevented from wrenching off thereof.
An Example of Cable Hauling Using an Auxiliary Tool 1 of Embodiment 1.
In this example, an optical fiber cable is hauled. A tension member is a wick wire located within the optical fiber cable. The wick wire is used as a tension member by the auxiliary tool because tension cannot be applied to the optical fibers directly.
As shown in FIG. 2 ( a ), a tension member 51 is exposed to haul the covered optical fiber cable 5 . The tension member 51 is inserted through an insertion hole 41 and is bent back to be inserted through another insertion hole 41 .
As shown in FIG. 2 ( b ), tension member 51 is bent back,is inserted through another insertion hole 41 , and then is restrained by restraint metal fitting 40 . Since its restraint force is not enough for hauling thereof, it is clamped to be restrained. The tension member, which is turned back, is clamped with the first clamping member 42 a . The tension member is bent back again and is clamped with the second clamping member 42 b and is thereby strongly restrained by the restraint member 4 .
Installing the restraint member 4 that restrains tension member 51 , the tip end container portion 2 a and the linking portion 2 b are secured to each other. The tip end of optical fiber cable 5 is restrained by an auxiliary tool 1 and then it sufficiently withstands hauling.
The restraint forces of the restraint member of this invention, as well as the prior method using a clamping member only, are hereby compared.
A test wire is restrained by a clamping member which is used in the above Embodiment. Another test wire is restrained by restraint member of the Embodiment. These were hauled by a tension tester and the load was measured just before separation failure.
Incidentally, the strength limit of test wire was exceeded and the wire was torn off when it was clamped twice as per the above Embodiment in a tension test. Therefore, only one clamping member is used for a restraint member in comparing the tension tests.
Details of the tension test
1.
Test mode
single (upward)
2.
Speed
10 mm/min
3.
Load cell
500 kgf
4.
F/S Load
500 kgf
As shown in FIG. 3, the maximum load of restraint by the restraint member of this Embodiment was half as much again as the maximum load of restraint by only one clamping member. The time up to separation failure was more than doubled.
One optical fiber cable was hauled in the Embodiment. Since restraint metal fitting 40 of the Embodiment has six insertion holes 41 , it can haul up to three cables. The advantages of hauling a plurality of cables are the following:
(a) Regarding hauling force, three times as much hauling force for one cable is not required when three cables are being hauled. For instance, even if 100 kgf is required to haul one cable, three cables can be hauled with 200 kgf. Thus, the tension in each cable sharply reduces to 66 Kgf when three cables are hauled. Such reduction of load on the cables effectively prevents the cables from tearing off.
(b) When cables are laid on multiple floors or at several positions of one floor, each cable was respectively laid by prior art. However, in the Embodiment, multiple cables are simultaneously and efficiently hauled. Each cable tip end is cut and connected to desired points individual.
Although restraint metal fitting 40 has six insertion holes, the present invention is not restricted by the Embodiment. For example, as shown in FIG. 4, a main insertion hole 41 a and insertion sub-holes 41 b around a main insertion hole 41 a are provided. The cable, which wires are intertwined, is inserted through the main insertion hole 41 a , each wire is untied, and each wire is inserted through insertion sub-holes 41 b . The wires are bound and are restrained by the double clampings.
A variety of restraint metal fittings could be applied if it is installed in a container and restrains a cable tip end by double clampings. The number of cables is also selected depending on the type of restraint metal fitting.
Embodiment 2
In the auxiliary tool for hauling cable of Embodiment 2, restraint means, which restrains the cable tip end, is provided on a linking portion of the container. As shown in FIG. 5, a linking portion 6 of Embodiment 2 is the same shape as the linking portion 2 b of Embodiment 1. A restraint portion 60 is formed as one body on the linking portion 6 to restrain a cable tip end. An insertion hole 61 is bored on the tip of the restraint portion 60 .
Embodiment 3
As shown in FIG. 6, an auxiliary tool for cable hauling of Embodiment 3 uses a restraint metal fitting 40 b as a restraint means. The restraint metal fitting 40 b has insertion hollows 41 c instead of insertion holes of the above Embodiments.
The restraint metal fitting 40 b is preferably utilized to restrain the tip end of a cable possessing too thick a diameter to insert into an insertion hole of the above Embodiments. Alternately, Embodiment 3 is preferably used in an auxiliary tool for hauling a cable having a small diameter because insertion holes are impossible to be bored on the restraint metal fitting.
When a cable tip end is restrained by restraint metal fitting 40 b , as shown in FIG. 6, a tension member 51 is inserted into the insertion hollows 41 c after it is bent back, and then restrained with a clamping member 42 a as per Embodiment 1 above.
Further, this restraint metal fitting 40 b has a large diameter portion 43 b and a small diameter portion 44 b . When a cable tip end is restrained and installed in a container, as shown in FIG. 7, the small diameter portion 44 b is contained in the tip end container portion 2 a , but the large diameter portion 43 b is held on the end of the tip end container portion 2 a . The tip end container portion 2 a and the linking portion 2 b are secured to each other (refer FIG. 2 ), and then the restraint metal fitting 40 b is held in the container 2 so that it is freely rotatable about an axis of the cable tip end.
Therefore, the present invention achieves the following effects:
(1) A cable tip end is easily restrained by using a clamping pliers tool at the laying sight, without specialized equipment.
(2) Since a plurality of cables are capable of being hauled simultaneously, they will be hauled more efficiently and load on the cables will be reduced.
(3) Even in a narrow laying tube, cables can be smoothly hauled because the hauling means of the cable tip end has enough restraint force, and is designed small, which is shorter than the prior art. Particularly, when the cable is turned up from a horizontal tube to a vertical tube, the cable is simply hauled in the corner of tube, without using a switchboard.
(4) Because the restraint metal fitting which restrains the cable is freely rotatable in the container, twisting of the cable is eliminated and breaking off or separation failure by twisting stress is prevented.
Industrial Applicability
An auxiliary tool for cable hauling of this invention is useful to haul communication cables such as an optical fiber cable or other cable such as electrical wires. Particularly, a cable tip end is strongly restrained to link a tip end thereof with a hauling means, and it is contained in a container and is hauled without exposing the cable tip end in the laying tube. | An auxiliary tool for cable hauling capable of restraining a tip end of a cable, which is exposed due to cutting on a cable laying site, with a restraint force enough to withstand a hauling force, and being applied even on a laying site where pipe size is small. A tension member ( 51 ) is exposed and is inserted into and received in a tip end receiving section ( 2 a ) and further is inserted through one of insertion holes ( 41 ) of a restraint member ( 4 ) and held back to be inserted through an other insertion hole ( 41 ). The tension member ( 51 ) thus held back is held on itself to be subjected to clamping with a first clamping member ( 42 b ). The tip end receiving section ( 2 a ) and a connection section ( 2 b ) are screw-engaged with each other in a state in which the restraint member ( 4 ) is received in the tool. | 8 |
CROSS-REFERENCE TO RELATED APPLICATION
[0001] This utility application claims the benefit of co-pending Provisional Application No. 60/444,741, filed Feb. 4, 2003.
FIELD OF THE INVENTION
[0002] This invention relates to reinforcements for concrete structures and, more particularly, to a welded wire reinforcement for modular concrete forms.
BACKGROUND OF THE INVENTION
[0003] Insulated concrete walls constructed with pre-fabricated forms are used to form structural walls both below and above grade. Generally, pre-fabricated foam blocks, which are made with two parallel foam panels held together by form ties, are assembled to form the desired structure. Reinforcing members, such as rebar, are positioned inside the blocks during assembly, and concrete is poured into the foam blocks to complete the walls. These walls provide superior strength and efficiency as opposed to the traditional poured wall construction with above grade wood frame walls. Insulated concrete walls provide all of the features of conventional wood frame construction including doors, windows, and decorative architectural features, such as ledges and further provide additional insulating capability and increased durability and safety.
[0004] The modular concrete forms are simple to position, but the reinforcing members used to provide internal reinforcement can require extra work to prepare and install. Several rebar reinforcements may be required to achieve the desired level of internal strength, often necessitating placement of several vertical rebar reinforcements in the wall. While horizontally oriented rebar are easily positioned into rebar chairs provided on the form ties of the pre-fabricated forms, the vertically oriented rebar reinforcements often must be tied into place. For less ordinary forms, such as those used to create ledges, the reinforcements must be bent or angled, further increasing labor.
BRIEF SUMMARY OF THE INVENTION
[0005] There is, therefore, provided in the practice of the invention a novel welded wire reinforcement for quickly and efficiently reinforcing a modular concrete form wall system. The welded wire reinforcement includes a base bar and several arms extending from the base bar. The welded wire reinforcement is positioned in a rebar chair of a modular concrete form to provide enhanced strength and stability.
[0006] In a preferred embodiment, a welded wire reinforcement includes a base bar and several arms extending downward from the base bar. The arms include end pieces that are positioned in various, selected locations along the arm.
[0007] In another preferred embodiment, the welded wire reinforcement is bent to provide reinforcement to concrete forms used to create ledges. The bent wire reinforcements have a base bar and several arms that are bent to form approximately a 90° angle. The arms include end pieces that are positioned at the end of the arms.
[0008] Accordingly, it is an object of the present invention to provide an improved welded wire reinforcement for use in modular concrete form wall systems.
[0009] It is a further object of the present invention to provide an improved bent wire reinforcement for use in modular concrete form wall systems to enhance the strength of a concrete form that creates a ledge.
BRIEF DESCRIPTION OF THE DRAWINGS
[0010] These and other inventive features, advantages, and objects will appear from the following Detailed Description when considered in connection with the accompanying drawings in which similar reference characters denote similar elements throughout the several views and wherein:
[0011] [0011]FIG. 1 is a front view of a welded wire reinforcement according to the present invention;
[0012] [0012]FIG. 2 is a side view of FIG. 1;
[0013] [0013]FIG. 3 is a front view of several welded wire reinforcements;
[0014] [0014]FIG. 4 is a side view of an alternative embodiment of the present invention;
[0015] [0015]FIG. 5 is a side view of an alternative embodiment of the present invention;
[0016] [0016]FIG. 6 is a side view of a bent wire reinforcement in a modular concrete form;
[0017] [0017]FIG. 7 is a top view the bent wire reinforcement shown in FIG. 6;
[0018] [0018]FIG. 8 is a side view of the bent wire reinforcement shown in FIG. 6.
DETAILED DESCRIPTION
[0019] Referring to the drawings in greater detail, FIG. 1 shows a welded wire reinforcement 20 constructed in accordance with a preferred embodiment of the present invention. The reinforcement 20 includes a substantially rigid base bar 22 and several substantially rigid arms 24 preferably welded to the base bar 22 . Substantially rigid means that the members have sufficient tensile strength to reinforce an intend structure. The reinforcement member is operable to reinforce a concrete wall formed using modular concrete form blocks, including pre-assembled forms and field-assembled forms. While top, bottom, vertical, horizontal, and other orientations are referenced in the specification and claims, it is understood that the structure of the invention could be utilized in other orientations.
[0020] In a preferred embodiment, the base bar 22 , as shown in FIGS. 1 and 2, is a substantially straight and rigid wire having a bar length extending across the top of the welded wire reinforcement 20 in a substantially horizontal orientation. The arms 24 , each having a top end 25 , an arm length, and a free end 27 , extend downward from the base bar 22 , substantially in the same plane as the base bar. The top ends are attached, preferably welded, at or adjacent the top ends. The arms 24 preferably terminate at their free ends with substantially perpendicular end pieces 26 , which can be positioned adjacent the free end. In one embodiment, the end pieces are substantially centered on the arms, so that they extend an equal distance on each side of the arms. The arms preferably each extend away from the base bar at an arm angle, and preferably, the arm angle is substantially ninety degrees, so that the arms are substantially perpendicular to the base bar. The end pieces are preferably substantially parallel to the base bar and thus substantially perpendicular to the arms. The arms 24 are similar in length and shape. The arms are preferably equally spaced along the base bar 22 , so that the arms are positioned between form ties. The base bar 22 extends slightly beyond the position of the left-most 30 and right-most arms 28 . In one embodiment, the base bar 22 , arms 24 , and end pieces 26 are welded together and are all made of substantially rigid wire with similar circumference. In another embodiment, the wire has surface texture.
[0021] The end pieces 26 are aligned in a substantially straight line to form a segmented or discontinuous bottom bar. In one embodiment, the end pieces are offset relative to the arms, so that the end pieces are longer on one side of the arms. In another embodiment, as shown in FIG. 4, the end piece is located on the arm closer to the base bar 22 , with a portion of the arm extending downward from the end piece. In another embodiment, shown in FIG. 5, the arm has multiple end pieces or cross members positioned along the length of the arm. The end pieces along the arm can be evenly spaced or unevenly spaced, depending on the reinforcement needs of the arm, but the end pieces are preferably spaced to align with a set of rebar chairs defined by form ties positioned below the base bar during wall construction. Because some form ties have upper and lower sets of rebar chairs, the end pieces can be spaced for alignment with either or both the upper and lower sets of rebar chairs.
[0022] In a preferred embodiment, the welded wire reinforcement 20 is used with insulated concrete forms 32 , similar to those described in U.S. application Ser. No. 09/691,934, filed on Oct. 10, 2000, which is fully incorporated herein by reference. As shown in FIGS. 2 and 3, the insulated concrete forms 32 are positioned to form concrete walls. The forms 32 include ties 34 , which extend between opposed, substantially parallel, foam panels or walls 35 , shown in FIG. 3. The welded wire reinforcement 20 is hung from the ties 34 between the forms 32 . The base bar is held in rebar chairs 33 , of the ties. In one embodiment, the arms are of a particular length so that the end pieces are aligned with rebar chairs 47 of a lower form tie. This could be the upper set 45 or lower set 47 of rebar chairs. Preferably, the arms are at least long enough so that the end pieces overlap the base bar of a lower reinforcement. In one embodiment, the end pieces would be received in the second, lower set of rebar chairs while the first, upper set of rebar chairs are supporting the base bar of the next lower reinforcement. Thus, at least the free ends of the arms and preferably the lowest discontinuous bar are positioned below the base bar of a lower reinforcement.
[0023] In a method of construction for a structure having more than one of the preferred foam block forms and more than one of the preferred reinforcements, the end pieces can be free between the walls of the form, or the reinforcement can slide left or right, so that the end pieces extend through the aligned rebar chairs of a lower tie. The end pieces have a length that is less than or equal to the approximate distance between the form ties, so that the reinforcement can be inserted from the top of a form with the end pieces and arms passing between the form ties.
[0024] In one embodiment, the welded wire reinforcement 20 is positioned to slightly overlap, in the horizontal orientation, the position of another reinforcement. As the desired number of form block levels, one or more, of the wall are stacked on each other to form layers, the reinforcements are put in place, and the next block layer, again one or more levels, is placed on top. The next reinforcement is then placed into a rebar chair that is just to one side of the previous lower and horizontally adjacent reinforcements. In this fashion, the reinforcements are hanging parallel staggered so they are added to the sequentially high form layers. Preferably the reinforcements are alternated between sets of substantially vertically aligned rebar chairs. Specifically, a first set of rebar chairs support a base bar of a reinforcement and a second set of rebar chairs, which are substantially vertically aligned with the first set, support a discontinuous bottom bar of the same reinforcement member. A next lower reinforcement is supported by substantially vertically aligned sets of rebar chairs, which are horizontally offset from the first and second sets of rebar chairs, and a horizontally adjacent reinforcement is supported by substantially vertically aligned sets of rebar chairs, which are also horizontally offset from the first and second sets of rebar chairs. When the reinforcements are placed in the desired position, concrete is poured into the space between the forms 32 .
[0025] The reinforcement 20 serves to reinforce the concrete wall created using the modular concrete forms 32 . The positions of the reinforcement can be varied based on level of reinforcement necessary for each wall. If more reinforcement is necessary, the reinforcements can be positioned and sized to overlap other reinforcements for greater lengths.
[0026] In another embodiment, referring now to FIGS. 6 and 7, a bent wire reinforcement 52 is disclosed. The bent wire reinforcement 52 is operable to reinforce a concrete wall with a perpendicular/horizontal ledge for supporting exterior finishes, such as bricks or stone, or interior flooring.
[0027] As shown in FIGS. 6 and 7, the bent reinforcement 52 includes a substantially horizontal base 66 with several arms 68 . The horizontal base 66 is shaped like a ladder, with equally spaced rungs 70 . The arms 68 depend at approximately a 90° angle from one edge of the base 66 . The horizontal width of the bent reinforcement 52 is preferably longer than the length of the vertical arms 68 . The arms are preferably continuous and equally spaced along the base and are positioned similar to the rungs 70 , although in an alternate embodiment the arms are not equally spaced. An outer side rail 71 joins the outer ends of the rungs 70 , and an inner side rail 73 joins the arms at 68 and rungs. The two rails 71 , 73 are preferably continuous, substantially straight, parallel to each other, and perpendicular to the arms and rungs, which are preferably integral and formed by bending a straight wire to a ledge angle. In a preferred embodiment, the ledge angle is approximately ninety degrees. In an alternate embodiment, the arms are welded to the rungs. In an alternate embodiment, the bent reinforcement could be formed by welding the arms to the horizontal base. The inner rail 73 is positioned at a midpoint of the arms, so that the base stays in the desired orientation, which is preferably horizontal. The inner rail 73 is thus lower than the outer rail and is preferably held in an innermost rebar chair 74 . Therefore, when positioned, the rungs are approximately horizontal in the form.
[0028] In a preferred embodiment, the reinforcement is galvanized or provided with another coating for corrosion protection. Alternatively, the reinforcement may be made of a material other than metal, including plastic.
[0029] In a preferred embodiment, the welded wire reinforcement 20 is used with insulated concrete ledge form 50 , shown in FIGS. 6 and 7. The ledge form 50 is reinforced by the bent wire reinforcement 52 , and includes a straight concrete form wall 62 , a sloped concrete form wall 54 , and a plurality of form/cross ties 64 . The substantially straight concrete form wall 62 is substantially vertical. The sloped concrete form wall 54 has a slope 58 that extends upward and away from the straight form wall 62 . The sloped form wall forms concrete cavities 72 at regularly spaced intervals that extend away from the plane of the sloped form wall. The cavities can be positioned between the intervals of the reinforcement rungs 70 . The sloped form wall has a longitudinal slot 56 in the top of the form for receiving the outer rail 71 of the reinforcement 52 , as shown in FIG. 6. The slot is discontinuous as it intersects the cavities 72 . The cavities are generally triangular slots open to the gap between the form walls 62 , 54 , and the segments of the slot are open to the cavities.
[0030] The cross ties 64 are positioned between the two form walls 62 , 54 . The ties are positioned between the cavities 72 , as shown in FIG. 7. The ties have rows of equally spaced and similarly positioned rebar chairs 74 along the tie extending between the two form walls 62 and 54 . The straight concrete form wall 62 is positioned opposite the sloped concrete form wall 54 . Several cross ties 64 are positioned between the two form walls 62 and 54 . A bent reinforcement 52 is positioned above the cross ties and the slot 56 formed in the sloped form wall 54 .
[0031] In the construction method, the form walls 62 and 54 , cross ties 64 and bent reinforcement 52 are placed in the desired position, concrete is poured into the space between the form walls. The concrete fills around the cross ties and bent reinforcement, and also fills the slots 56 , and cavities 72 formed by the sloped wall form 54 . The concrete hardens around the rungs, which are in the cavities and the rail which is in the slot, to form a wall with the bent reinforcement as reinforcing rebar. Once the wall and ledge are set, the decorative brick, or other exterior feature, can be applied to the wall and ledge.
[0032] The welded wire reinforcement 20 according to the present invention provides a secure mechanism for internally increasing the strength of an insulated concrete wall created from modular concrete forms.
[0033] Thus, an improved welded wire reinforcement is disclosed which utilizes a novel configuration of arms and end pieces. This invention allows for superior reinforcement of an insulated concrete wall system. While preferred embodiments and particular applications of this invention have been shown and described, it is apparent to those skilled in the art that many other modifications and applications of this invention are possible without departing from the inventive concepts herein. It is, therefore, to be understood that, within the scope of the appended claims, this invention may be practiced otherwise than as specifically described, and the invention is not to be restricted except in the spirit of the appended claims. Though some of the features of the invention may be claimed in dependency, each feature has merit if used independently. | A welded wire reinforcement is used in combination with insulated concrete form blocks having opposed panels joined by form ties. A method of construction forms building structures with insulated concert form blocks. The reinforcement member has a base bar and a plurality of arms extending downwardly from the base bar and is utilized to provide increased internal strength to a modular concrete wall system. The welded wire reinforcement provides vertical and horizontal support without requiring any extra time or material to connect a vertical reinforcement to the concrete forms of the wall system. An alternate embodiment of the reinforcement member includes a horizontal base bar, arms extending downward and perpendicular from the base bar, and a plurality of end pieces attached to the arms to form a discontinuous bottom bar. The base bar and bottom bar are slidably received in rebar chairs defined by the form ties. Another embodiment of the reinforcement member is utilized for reinforcing a modular concrete wall form with a ledge. | 4 |
RELATED APPLICATIONS
This application is a continuation of U.S. patent application Ser. No. 11/754,059, filed May 25, 2007, which is a continuation of U.S. patent application Ser. No. 10/173,813, filed June 19, 2002 (now U.S. Pat. No. 7,239,647), the contents of both of which are incorporated herein by reference.
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to a band control system for a digital subscriber network and a band control method therefore. More particularly, the present invention relates to a band control system implementing flexible control and efficient use of a band between IADs (Integrated Access Devices) and a DSLAM (Digital Subscriber Line Access Multiplexer) situated at subscriber stations and a center, respectively, and a control method therefore.
2. Description of the Background Art
A VoDSL (Voice over Digital Subscriber Line) network using an ATM (Asynchronous Transfer Mode) communication system and a DSL technology provides a transfer path for multimedia communication using voice, data and image. DSL technologies implement high-speed digital transfer over metallic cables, i.e., existing telephone subscriber lines.
A problem with the conventional DSL technologies is that the transfer rate is dependent on the quality of metallic cables and transfer distance and therefore indefinite despite a preselected transfer rate. Consequently, a communication band statistically set beforehand brings about the congestion of ATM cells and thereby causes some users to be blocked. It is therefore necessary to dynamically control band assignment in order to obviate the congestion of ATM cells.
Japanese Patent Laid-Open Publication No. 2000-184061, for example, discloses a technology for dynamically controlling band assignment in a DSL communication system. It has been customary with conventional technologies, including the above technology, to send band control information indicative of the variation of a communication band by using special ATM cells, e.g., RM (Resource Management) cells. this, however, presses the communication band and thereby makes the use of the frequency band uneconomical when such special ATM cells are used to dynamically guarantee the band during communication.
Technologies relating to the present invention are also disclosed in, e.g., Japanese Patent Laid-Open Publication No. 11-331192.
SUMMARY OF THE INVENTION
It is an object of the present invention to provide a band control system for a digital subscriber line network capable of solving the problem stated above and a band control system therefore.
A band control system of the present invention is applicable to a digital subscriber line network in which a first apparatus and a second apparatus situated at a subscriber station and a center, respectively, are interconnected by a metallic cable for interchanging at least a digital data signal with each other. The band control system includes a commanding device included in one of the first and said second apparatuses for monitoring the receipt of ATM (Asynchronous Transfer Mode) cells from the other apparatus and sending, based on the result of monitoring, a band variation command to the other apparatus to thereby cause it to vary a band by using a frequency band not used for signal transfer. A band varying device is included in the other apparatus for receiving the band variation command and varying the band in accordance with the command.
A band control method for the band control system is also disclosed.
BRIEF DESCRIPTION OF THE DRAWINGS
The above and other objects, features and advantages of the present invention will become more apparent from the following detailed description taken with the accompanying drawings in which:
FIG. 1 is a schematic block diagram showing a specific band control system in accordance with the present invention;
FIG. 2 is a flowchart demonstrating the operation of the band control system shown in FIG. 1 ;
FIG. 3 is a schematic block diagram showing specific configuration of a DSLAM included in a first embodiment of the present invention;
FIG. 4 shows a specific frequency characteristic of signals to be interchanged between IADS shown in FIG. 1 and the DSLAM;
FIG. 5 is a schematic block diagram showing a specific configuration of each IAD;
FIG. 6 is a schematic block diagram showing a specific configuration of a DSLAM included in a second embodiment of the present invention;
FIG. 7 is a schematic block diagram showing a specific configuration of an IAD included in the second embodiment;
FIG. 8 is a flowchart demonstrating the operation of the second embodiment;
FIG. 9 is a schematic block diagram showing a third embodiment of the present invention; and
FIG. 10 is a schematic block diagram showing a specific configuration of an ATU-R (Asymmetric digital subscriber line Termination Units-Remote) included in the third embodiment.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
Briefly, in a VoDSL network that allows a plurality of digital voice signals and a plurality of digital data signals to be interchanged via metallic wires, or existing telephone subscriber lines, by use of a DSL technology, the present invention provides a band control system realizing flexible control and efficient use of communication band between IADs and a DSLAM situated at subscriber stations and a center, respectively, and a band control method therefore.
Further, the system and method of the present invention measure the amount of received ATM cells or the ratio of discarded ATM cells VC (Virtual Channel) by VC and then send a band variation command to any one of the IADs by using a frequency band not used for signal transfer in the VoDSL network, e.g., a frequency band lower than 4 kHz inclusive. This dynamically optimizes the frequency band for thereby promoting efficient operation of the VoDSL network.
Referring to FIG. 1 of the drawings, a specific configuration of a band control system in accordance with the present invention. As shown, the band control system includes a public switched telephone network 101 , an IP (Internet Protocol) network 102 , a voice GW (Gate Way) 103 , a BAS (Broadband Access Server) 104 , an ATM network 105 , a DSLAM 106 , IADs 107 , telephones 108 , and personal computers or similar data terminals 109 . A band control method in accordance with the present invention is applied to the DSLAM 106 and IADs 107 . The telephones 108 and data terminals 109 are assigned to voice telephone services and Internet access and other data communication services, respectively.
More specifically, the telephones 108 - 1 through 108 - m (m being a positive integer) and data terminals 109 - 1 through 1 - 9 - n (n being a positive integer) each are accommodated in one of the IADs 107 - 1 through 107 - x (x being a positive integer). The IADs 107 each are connected to the DSLAM 106 by one of metallic cables 111 - 1 through 111 - x. The voice GW 103 is existing network equipment that repeats, when any one of the telephones 108 effects a voice telephone service, all protocols necessary for connecting the ATM network 105 and switched telephone network 101 . Likewise, the BAS 104 is existing network equipment that repeats, when any one of the data terminals 109 effects an Internet access or similar data communication service, all protocols necessary for connecting the ATM network 105 and IP network 102 .
FIG. 2 demonstrates the operation of the band control system in accordance with the present invention. As shown, the DSLAM 106 measures the amount of ATM cells received from each IAD 107 or the ratio of discarded ATM cells VC by VC (step S 1 ). The DSLAM 106 then commands, based on the result of measurement, the IAD 107 to vary the frequency band by using a frequency band not newly occupied by signal transfer in a VoDSL network, e.g., a frequency band lower than 4 kHz inclusive (step S 2 ). In response, the IAD 107 varies the frequency band of a VC newly designated by the DSLAM 106 (step S 3 ).
As stated above, the band control system in accordance with the present invention sends band control information to the IAD 107 not by using conventional special ATM cells, but by using a frequency band not occupied by signal transfer. The system therefore solves the previously stated problem particular to the conventional DSL communication system. It is therefore possible to dynamically maintain an optimal communication band between each IAD 107 and the DSLAM 106 for thereby promoting efficient use of the VoDSL network.
A first embodiment of the present invention also practicable with the configuration shown in FIG. 1 will be described hereinafter. The description on the individual blocks shown in FIG. 1 will not be repeatedly made in order to avoid redundancy. The voice GW 103 has the previously stated function as existing network equipment. More specifically, the voice GW 103 communicates with the IADs 107 with a signaling procedure using, e.g., an LES (Lop emulation Service). Also, the voice GW 103 communicates with the switched telephone network 101 with a signaling procedure using an FR-303 or similar time-division communication system.
The BAS 104 also has the function stated earlier as existing network equipment. More specifically, the BAS 104 communicates with the ATM network 105 with a signaling system using, e.g., a PPPoA (Point to Point Protocol over ATM) system. Also, the BAS 104 interchanges IP packets with the IP network 101 by using an IP signaling system.
A specific configuration of the DSLAM 106 will be described with reference to FIG. 3 . As shown, the DSLAM 106 includes an ATM network interface 201 , an ATM cell multiplexer/demultiplexer 202 , x (x being a positive integer) ATM cell queues 203 ( 203 - 1 through 203 - x ) and x center DSL modems 204 ( 204 - 1 through 204 - x ) as conventional. In the illustrative embodiment, the DSLAM 106 additionally includes x band control information transmitters 205 ( 205 - 1 through 205 - x ) and x signal couplers 206 ( 206 - 1 through 206 - x ).
Each band control information transmitter 205 measures, VC by VC, the amount of ATM cells received from the associated IAD 107 or the ratio of discarded ATM cells. Assume that either the amount of received ATM cells or the ratio of discarded ATM cells exceeds an allowable range implementing preselected communication quality. Then, to command the IAD 107 to vary the communication band assigned to the corresponding VC, the transmitter 205 modulates a band control information signal to a conventional modem signal or similar signal that can be sent in a frequency band lower than 4 kHz inclusive. The modulated signal is fed to the associated signal coupler 206 .
The signal coupler 206 couples a DSL signal received from the center DSL modem 204 and the band control information signal received from the band control information transmitter 205 to thereby produce a signal, which will be described with reference to FIG. 4 later. This signal is sent from the signal coupler 206 to the IAD 107 connected to the DSLAM 106 by the associated metallic cable 111 . In addition, when the signal coupler 206 receives a DSL signal from the IAD 107 , the signal coupler 206 simply transfers the DSL signal to the center DSL modem 203 without any processing.
FIG. 4 shows specific frequency bands assigned to the signals to be interchanged between each IAD 107 and DSLAM 106 . As shown, the signals consist of a DSL signal or main information signal 121 and a band control information signal 122 . A frequency band higher than 4 kHz and a frequency band lower than 4 kHz inclusive are assigned to the DSL signal 121 and band control information signal 122 , respectively, by way of example.
FIG. 5 shows a specific configuration of each IAD 107 . As shown, the IAD 107 includes a terminal DSL modem 302 , an ATM cellularizer/decellularizer 304 , a telephone interface 305 , and a data terminal interface 306 as conventional. In the illustrative embodiment, the IAD 107 additionally includes a signal uncoupler 301 , and a band control information receiver 303 .
The conventional telephone interface 305 allows various kinds of telephone terminals 108 available for voice telephone services to be accommodated in the IAD 107 . For this purpose, the telephone interface 305 functions to terminate POTS (Plain Old Telephone Service) interfaces assigned to traditional analog telephones and S/T point interfaces assigned to ISDN (Integrated Services Digital Network) terminal adapters.
Likewise, the conventional data terminal interface 306 allows various kinds of data terminals 109 available for internet access and other data communication services to be accommodated in the IAD 107 . For this purpose, the data terminal interface 306 functions to terminate a USB (Universal Serial Bus), 10/100 Base-T or similar interface.
The signal uncoupler 301 separates the signals shown in FIG. 4 and received from the DSLAM 106 via the metallic cable 111 into the DSL signal 121 and frequency control information signal 122 that lies in the frequency band lower than 4 kHz inclusive. The DSL signal 121 and band control information signal 122 separated from each other are input to the terminal DSL modem 302 and band control. information receiver 303 , respectively. On the other hand, when a DSL signal is input from the terminal DSL modem 302 to the signal uncoupler 301 , the signal uncoupler 301 simply transfers the DSL signal to the metallic cable 111 without any processing.
The band control information receiver 303 separates the band control information sent from the DSLAM 106 from the band control information signal 122 and analyzes the information. The receiver 303 then causes the ATM cellularizer/decellularizer 304 to vary the communication band assigned to the corresponding VC directed toward the DSLAM 106 .
Specific operations of the illustrative embodiment will be described hereinafter. First, how signals flow when the telephone 108 accommodated in any one of the IADs 107 communicates with the public switched telephone network 101 by using a voice telephone service will be described.
Referring again to FIG. 1 , as for the flow of signals from the telephone network 101 toward the telephone 108 , a digital voice signal based on the time-division communication system is sent from the telephone network 101 to the voice GW 103 and transformed to ATM cells thereby. The cellularized digital voice signal is sent from the voice GW 103 to the DSLAM 106 via the ATM network 105 . In the DSLAM 106 , the ATM cell multiplexer/demultiplexer 202 delivers the cellularized digital voice signal to the center DSL modem 204 via one of the ATM cell queues 203 corresponding to the IAD 107 . The office DSL modem 204 modulates the cellularized digital voice signal to a DSL signal and sends the DSL signal to the IAD 107 connected thereto by the metallic cable 111 .
In the IAD 107 shown in FIG. 5 , the terminal DSL modem 302 demodulates the DSL signal to thereby restore the original ATM cellularized voice signal. Subsequently, the ATM cellularizer/decellularizer 304 decellularizes the cellularized digital signal input from the terminal DSL modem 302 . As a result, the decellularized digital voice signal is input to the telephone interface 305 . The telephone interface 305 transforms the digital voice signal to a voice signal format matching with the telephone 108 and then sends the transformed voice signal to the telephone 108 .
The flow of signals from the telephone 108 toward the telephone network 101 is identical with the flow described above except that the procedure is reversed in direction and will not be described specifically.
As stated above, the illustrative embodiment implements a bidirectional voice telephone service between the telephone 108 accommodated in the IAD 107 and the public switched telephone network 101 .
Next, how signals flow when the data terminal 109 accommodated in any one of the IADs 107 effects a data communication service with the IP network 102 will be described hereinafter. Referring to FIG. 1 , as for the flow of signals from the IP network 102 toward the data terminal 109 , the IP network 102 sends an IP packet or an IP-packeted digital data signal to the BAS 104 . The BAS 104 transforms the received IP packet or the IP-packeted digital data to an ATM cell. The ATM-cellularized IP packet or the IP-packeted digital data signal is sent to the DSLAM 106 via the ATM network 105 . In the DSLAM 107 , the multiplexer/demultiplexer 202 , FIG. 3 , delivers the ATM-cellularized IP packet or the IP-packeted digital signal data to the center DSL modem 204 via the ATM cell queue 203 corresponding to the IAD 107 , which accommodates the data terminal 109 . The center DSL modem 204 modulates the ATM-cellularized IP packet or the IP-packeted digital data signal to a DSL signal and sends the DSL signal to the IAD 107 via the metallic cable 111 .
In the IAD 107 , the terminal DSL modem 302 , FIG. 5 , demodulates the DSL signal to thereby restore the ATM-cellularized IP packet or the IP-packeted digital data signal and feeds it to the ATM cellularizer/decellularizer 304 . The ATM cellularizer/decellularizer 304 decellularizes the ATM-cellulazized IP packet or the IP-packeted digital data signal and inputs the resulting IP packet or the IP-packeted digital data signal to the data terminal interface 306 . The data terminal interface 306 transforms the IP packet or the IP-packeted digital data signal to a format matching with the data terminal 109 and then sends the transformed IP packet or the transformed data signal to the data terminal 109 .
The flow of signals from the data terminal 109 toward the IP network 102 is identical with the flow described above except that the procedure is reversed in direction and will not be described specifically.
As stated above, the illustrative embodiment implements a bidirectional data communication service between the data terminal 109 accommodated in the IAD 107 and the IF network 102 .
Hereinafter will be described a band control procedure to be executed between each IAD 107 and the DSLAM 106 . When a plurality of voice telephone services and a plurality of data communication services, both of which are bidirectional; are effected at the same time, importance should be attached to the communication quality of voice telephone services. This is because voice telephone services allow information to be interchanged between persons and therefore need real-time communication more than data communication services. It is therefore necessary to reduce propagation delays as far as possible. In addition, voice quality falls with an increase in the number of ATM cells discarded due to the failure of retransmission. On the other hand, data communication services should also be effected at high speed as possible for users' convenience.
In light of the above, in the illustrative embodiment, each band control information transmitter 205 , FIG. 3 , measures the amount of ATM cells received from the associated IAD 107 and present on the associated ATM cell queue 203 or the ratio of discarded ATM cells VC by VC (step S 1 , FIG. 2 ). Assume that the amount of ATM cells or the ratio of discarded ATM cells exceeds an allowable range assigned to the communication quality of a voice telephone service, which is determined by the provider of the VoDSL network beforehand. Then, the band control information transmitter 205 modulates the band control information signal 122 , FIG. 4 , to a conventional modem signal or similar signal that can be sent in the frequency band lower than 4 kHz inclusive. The band control information signal 122 is sent to the IAD 107 via the signal coupler 206 in order to command the IAD 107 to vary the frequency band of the VC on which the corresponding data communication service is held (step S 2 , FIG. 2 ).
In the IAD 107 shown in FIG. 5 , the band control information signal 122 is routed through the signal uncoupler 301 to the band control information receiver 303 . The receiver 303 separates the band control information signal 122 and analyzes the communication band designated by the DSLAM 106 . The receiver 303 then controls the ATM cellularizer/decellularizer 304 in order to narrow the communication band assigned to the VC of the corresponding data communication service and directed toward the DSLAM 106 (step S 3 , FIG. 2 ).
On the other hand, assume that the amount of ATM cells or the ratio of discarded ATM cells decreases below the allowable range assigned to the communication quality of the voice telephone service. Then, the DSLAM 106 sends the band control information signal 122 to the IAD 107 in the previously stated manner. Again, the band control information receiver 303 separates the band control information signal 122 and analyzes the communication band designated by the DSLAM 106 . The receiver 303 then controls the ATM cellularizer/decellularizer 304 in order to broaden the communication band assigned to the VC of the corresponding data communication service and directed toward the DSLAM 106 .
A second embodiment of the present invention will be described hereinafter. The second embodiment is essentially similar to the first embodiment except that the DSLAM 106 is also configured to vary the frequency band of the VC designated by the IAD 107 for thereby further promoting efficient operation of the VoDSL network.
As shown in FIG. 6 specifically, the DSLAM 106 includes signal coupler/uncouplers 501 ( 501 - 1 through 501 - x ). Each signal coupler/uncoupler 501 has, in addition to the function of the signal coupler 206 , FIG. 3 , a function of separating the signal received from the IAD 107 into the DSL signal 121 and the signal 122 lying in the frequency bend lower then 4 kHz inclusive and feeding the signal 122 to a band control signal transmitter/receiver 502 .
The band control signal transmitter/receiver 502 has the following function in addition to the function of the band control information transmitter 205 , FIG. 3 . The additional function is to separate the band control information signal sent from the IAD 107 from the signal 122 input from the signal coupler/uncoupler 501 , analyze the signal 122 , control the ATM cell queue 203 in accordance with the result of analysis, and vary the communication band assigned to the corresponding VC and directed toward the IAD 107 .
As shown in FIG. 7 specifically, the IAD 107 includes a signal coupler/uncoupler 601 and a band control signal transmitter/receiver 602 . The signal coupler/uncoupler 601 has, in addition to the function of the signal uncoupler 301 , FIG. 5 , a function of coupling the DSL signal 121 received from the terminal DSL modem 302 and the band control information signal 122 received from the band control information transmitter/receiver 602 and sending the resulting signal to the DSLAM 106 .
The band control information signal transmitter/receiver 602 has the following function in addition to the function of the band control information receiver 303 , FIG. 5 . The additional function is to measure the amount of ATM cells received from the DSLAM 106 and input to the ATM cellularizer/decellularizer 304 or the ratio of discarded ATM cells VC by VC. When the amount of ATM cells or the ratio of discarded ATM cells increases above an allowable range assigned to communication quality, the band control information transmitter/receiver 602 modulates the band control information signal to a conventional modem signal or similar signal that can be sent in the frequency band lower than 4 kHz inclusive. The modulated signal is sent to the signal coupler/uncoupler 601 in order to command the signal coupler/uncoupler 601 to vary the communication band of the corresponding VC.
More specifically, as shown in FIG. 8 , the IAD 107 measures the amount of ATM cells received from the DSLAM 106 or the ratio of discarded ATM cells VC by VC (step S 11 ). The IAD 107 then commands the DSLAM 106 to vary the frequency band by using the band lower than 4 kHz inclusive (step S 12 ). In response, the DSLAM 106 varies the frequency band of the VC designated by the IAD 107 (step S 13 ).
As stated above, in the illustrative embodiment, the IAD 107 can command, based on the amount of ATM cells received from the DSLAM 106 or the ratio of discarded ATM cells, the DSLAM 106 to vary the communication band VC by VC. It follows that the DSLAM 106 can narrow or broaden the band of the VC designated by the IAD 107 accordingly.
A third embodiment of the present invention will be described hereinafter. This embodiment is applicable to a DSL network configured to promote high-speed Internet access and other data communication services by using metallic cables. A DSL network transforms only digital data signals to ATM cells and transfer the ATM cells via metallic cables. FIG. 9 shows a band control system representative of the third embodiment. As shown, the third embodiment includes x ATU-Rs 701 ( 701 - 1 through 701 - x ) in place of the IADs 107 - 1 through 107 - x , FIG. 1 . The x ATU-Rs 701 are connected to the DSLAM 106 by the metallic cables 111 .
FIG. 10 shows a specific configuration of one of the ATU-Rs 701 . As shown, the ATU-R 701 includes the band control information transmitter/receiver 602 and signal coupler/uncoupler 601 in addition to the conventional terminal DSL modem 302 , ATM cellularizer/decellularizer 304 , and data terminal interface 306 . How the illustrative embodiment executes bidirectional control over the communication band between the DSLAM 106 and each ATU-R 701 will be described hereinafter.
When the data terminal 109 accommodated in any one of the ATU-Rs effects a data communication service with the IP network 102 , signals flow in exactly the same manner as when the data terminal 109 accommodated in the IAD 107 effects a data communication service with the IP network 102 .
First, a specific procedure for controlling the communication band directed from the ATU-R 701 toward the DSLAM 106 when a plurality of data communication services are held will be described. In the DSLAM 106 shown in FIG. 6 , each band control information transmitter/receiver 502 measures the amount of ATM cells received from the associated ATU-R 701 and present on the associated ATM cell queue 203 or the ratio of discarded ATM cells VC by VC (step S 1 , FIG. 2 ) . Assume that the amount of ATM cells or the ratio of discarded. ATM cells increases above an allowable range assigned to the communication quality of a voice telephone service, which is determined by the provider of the VoDSL network beforehand. Then, the band control information transmitter/receiver 502 modulates the band control information signal to a conventional modem signal or similar signal that can be sent in the frequency band lower than 4 kHz inclusive. The band control information signal is sent to the ATU-R 701 via the signal coupler/uncoupler 501 in order to command the ATU-R 701 to vary the frequency band of the VC on which the data corresponding data communication service is held (step S 2 , FIG. 2 ).
In the ATU-R 701 shown in FIG. 10 , the band control information signal is routed through the signal coupler/uncoupler 601 to the band control information transmitter/receiver 602 . The transmitter/receiver 602 analyzes the communication band designated by the DSLAM 106 . The transmitter/receiver 602 then controls the ATM cellularizer/decellularizer 304 in order to narrow the communication band assigned to the VC of the corresponding data communication service and for transmission to the DSLAM 106 (step S 3 , FIG. 2 ).
On the other hand, assume that the band control information transmitter/receiver 502 included in the DSLAM 106 , FIG. 6 , determines that the amount of ATM cells or the ratio of discarded ATM cells has decreased below the allowable range assigned to the communication quality of the voice telephone service. Then, the DSLAM 106 sends the band control information signal to the ATU-R 701 in the previously stated manner. Again, the band control information transmitter/receiver 602 separates the band control information signal and analyzes the communication band designated by the DSLAM 106 . The transmitter/receiver 602 then controls the ATM cellularizer/decellularizer 304 in order to broaden the communication band assigned to the VC of the corresponding data communication service and adapted for transmission to the DSLAM 106 .
Next, a specific operation for controlling the communication band directed from the DSLAM 106 toward any one of the ATU-Rs 701 will be described. In the ATU-R 701 shown in FIG. 10 , each band control information transmitter/receiver 602 measures the amount of ATM cells received from the DSLAM 106 and present in the ATM cellularizer/decellularizer 304 or the ratio of discarded ATM cells VC by VC (step S 11 , FIG. 8 ). Assume that the amount of ATM cells or the ratio of discarded ATM cells increases above an allowable range assigned to the communication quality of a voice telephone service, which is determined by the provider of the VoDSL network beforehand. Then, the band control information transmitter/receiver 602 modulates the band control information signal to a conventional modem signal or similar signal that can be sent in the frequency band lower than 4 kHz inclusive. The band control information signal is sent to the DSLAM 106 via the signal coupler/uncoupler 601 in order to command the DSLAM 106 to vary the frequency band of the VC on which the data corresponding data communication service is held (step S 12 , FIG. 8 ).
In the DSLAM 106 , the band control information signal is routed through the signal coupler/uncoupler 501 to the band control information transmitter/receiver 502 . The transmitter/receiver 502 separates the communication band control signal and analyzes the communication band designated by the ATU-R 701 . The transmitter/receiver 502 then controls the ATM cell queue 203 in order to narrow the communication band assigned to the VC of the corresponding data communication service and adapted for transmission to the ATU-R 701 (step S 13 , FIG. 8 ).
On the other hand, assume that the band control information transmitter/receiver 602 included in the ATU-R 701 determines that the amount of ATM cells or the ratio of discarded ATM cells has decreased below the allowable range assigned to the communication quality of the voice telephone service. Then, the transmitter/receiver 602 sends the band control information signal to the DSLAM 106 in the previously stated manner. Again, the band control information transmitter/receiver 502 in the DSLAM 106 separates the band control information signal and analyzes the communication band designated by the ATU-R 701 . The transmitter/receiver 502 then controls the ATM cell queue 203 in order to broaden the communication band assigned to the VC of the corresponding data communication service and adapted for transmission to the ATU-R 701 .
As stated above, the illustrative embodiment provides high-quality data communication services by dynamically optimizing the frequency bands between the DSLAM 106 and the ATU-Rs 701 in opposite directions, thereby promoting efficient operation of the DSL subscriber network.
In summary, it will be seen that the present invention obviates uneconomical use of a communication band by preventing it from being pressed. In addition, the present invention provides high-quality data communication services by dynamically optimizing frequency bands between a DSLAM and IADs for thereby promoting efficient operation of a voDSL network.
Various modifications will become possible for those Skilled in the art after receiving the teachings of the present disclosure without departing from the scope thereof. | A band control system for a digital subscriber line network in which a first apparatus and a second apparatus situated at a subscriber station and a center, respectively, are interconnected by a cable for interchanging at least a digital data signal with each other. The system may cause one of the first apparatus or the second apparatus to monitor receipt of signals from the other of the first apparatus or the second apparatus; send, based on a result of monitoring, a band variation command to the other apparatus for causing the other apparatus to vary a band by using a frequency band not used for signal transfer; cause the other apparatus to receive the band variation command; and vary the band in accordance with the band variation command. | 7 |
This is a continuation of application Ser. No. 327,245, filed Jan. 26, 1973 now abandoned.
DETAILED DESCRIPTION OF THE INVENTION
This invention relates to a new and improved process for the methanation of product gases containing carbon monoxide and hydrogen. More specifically, the invention teaches a methanation process employing a slurry phase fluidized bed system.
In coal and heavy hydrocarbon gasification, the product gases contain significant amounts of carbon monoxide and hydrogen and relatively low amounts of methane. In order to manufacture pipeline gas with 1000 BTU per cubic foot heating value, the carbon monoxide and hydrogen must be converted to methane. Since carbon monoxide is toxic, its content in pipeline gas must be reduced to 0.1% or less. Methanation is the process step used for this conversion.
Methanation for making pipeline gas is not yet a commercial process. To date, process development efforts to convert carbon monoxide to methane have involved fixed bed gas phase systems.
The major problem in gas phase methanation is to control and design the reaction system for the removal of the heat released. This is particularly difficult due to the highly exothermic nature of the carbon monoxide-hydrogen reaction. About 100,000 BTU's are released per pound-mole of carbon monoxide converted. A second problem is to control the reaction temperature within an optimum range. The methanation reaction rate is low below 500° F., while above 850° F. catalyst life is decreased and carbon deposition can occur, deleteriously affecting catalyst life. In addition, at high temperatures, the methanation reaction reverses so that conversion to methane is reduced. A third problem is to minimize pressure drop across the reactors without inordinately increasing catalyst particle size (and decreasing catalyst surface area).
To overcome these problems of the gas phase methanation many design features have been proposed: These include the introduction of cold feed gas between stages and at quench points in the reactor and recycling large quantities of product gas to lower the concentration of carbon monoxide at the reactor inlet. These modifications, however, have not been entirely satisfactory because only a limited amount of heat can be taken up in the feed gas and, where recycle is used, high operating costs are necessary to circulate, cool, reheat and recompress the recycled product gas.
Additional drawbacks to the gas phase process designs are gas distribution, complex reactor systems and the need for a complicated array of heat exchange equipment. In the case of fixed bed designs, large size catalyst particles are required to minimize pressure drop. This results in a high temperature rise across the reactor (on the order of 300° F.) and non-optimum reaction conditions over most of the reactor.
While gas phase fluid bed systems have been proposed and studied to overcome these problems, catalyst attrition is found to be a process difficulty difficult to circumvent.
In accordance with the invention, it has now been discovered that methanation can be performed without the several disadvantages described above by employing an upwardly moving liquid fluid bed of relatively high boiling hydrocarbons.
The liquid hydrocarbon serves to fluidize the active small sized methanation catalyst and as a heat carrier "fly wheel" wherein the heat of hydrogenation of carbon monoxide is taken up by direct contact. The sensible heat and heat of vaporization of the fluidizing oil media, the cold feed gas and recycled liquid provide a heat sink. Isothermal operation of the reaction system is readily achieved by having the catalyst particles in an expanded state and absorbing the exothermic heat with the cool feed gas and cooled liquid recycle streams.
Advantages of the liquid fluidized system are manifold:
1. Reactor design is simplified. Liquids and gases are readily distributed across the reactor cross-sectional area without the necessity for redistribution and quench along the reactor length.
2. Heat control of exothermic hydrogenation reactions is excellent; the reactors are nearly isothermal with a temperature spread of only 5°-10° F. between inlet and outlet.
3. Vapor-liquids can be disengaged without pressure let down.
4. Small size catalyst can be used, thereby achieving higher rates of reaction than with large catalyst particles.
5. Catalyst can be added and withdrawn from the system without the necessity to remove spent catalyst or to "swing" the reaction systems from on-stream operations to regeneration. Regeneration, if needed, is accomplished in external equipment.
6. The isothermal temperature of the system permits optimum conditions favoring the desired reaction kinetics.
7. Catalyst activity can be maintained at a constant "equilibrium" activity level so that it is not necessary to overdesign the reactor size for the poorest catalyst activity level.
In one alternate, a bed of particulate catalyst can be fluidized and retained in the reactor without carry-over of catalyst particles. Alternatively, catalyst and liquids can be carried overhead with the liquid, through the heat exchangers and recycled.
Unlike gas-solid fluidized methanation systems, attrition of methanation catalyst is not a process difficulty because of the relatively low velocities in the liquid fluidized bed. The catalyst is also cushioned by the fluidized oil media.
In contrast to fixed bed gas phase methanation processes, pressure drop across the bed is not a restricting design factor because the large quantities of gas necessary to limit the carbon monoxide concentration in the feed to low levels are not required; since higher inlet concentrations of carbon monoxide are permissible.
The FIGURE is a flow sheet showing the liquid phase methanation process of the invention. In this embodiment the fluidized catalyst is not carried overhead with the liquid.
A purified gasified effluent feed containing 75% hydrogen and 25% carbon monoxide is feed to the methanation process via line 1, passed through the heat exchange 2, thereby increasing its temperature to 1000° F., and thereafter feed via line 3 to the liquid phase methanator 4. The methanator has a diameter of 10 feet and a height of 25 feet. The total pressure therein is 1000 psig, the superficial gas velocity 0.2 feet per second, and the space velocity 800 SCF of gas per hour, SCF of reactor.
The reactor effluent is withdrawn from the liquid phase methanator 4 via line 5 and sent to separator 6. In separator 6 the liquid and vapor effluent is divided, the liquid being pumped out of the bottom of the separator and recycled, after cooling (not shown), back to the bottom of the liquid phase methantor 4 via line 7. The gaseous product is removed from the separator 6 via the line 8 and heat exchanged with the effluent feed in heat exchanger 2. The cool vapor is then passed through cooler 10 via line 9, and then via line 11, to separator 12. In separator 12 the liquid formed upon cooling is separated from the bottom via line 13 and recycled to the separator 6. The remaining vapor is withdrawn overhead via line 14, subject to further cooling in cooler 15 and separated again in separator 16. Additional water is withdrawn and collected via line 17 while the remaining vapor is passed via line 18 to the gas dryer 19. The gas dryer contains silica gel and serves to remove the last traces of moisture from the feed stock. The dried gas is removed via line 20 wherein there is recovered 50 million standard cubic feet of pipeline gas having 92.4% of methane, 1.9% carbon monoxide and 5.7% hydrogen.
The catalyst in the liquid fluidized bed is 59 weight percent nickel oxide and 41% kieselguhr which serves as the catalyst support. The catalyst is in the form of an extrudate having a diameter of 0.032 inches and a length of 0.25 inches. The oil is a desulfurized heavy gas oil, 25° API; having 0.01 weight % sulfur and a boiling range of 650° to 1100° F. The oil velocity in the reactor is 30 gallons per minute per square foot of reactor cross-section.
The aforesaid example, while setting forth a preferred embodiment of the invention, is merely exemplary. The feed composition may be from 1.0 to 25% carbon monoxide and from 3.0 to 75% hydrogen. Preferably, the feed contains from about 5.0 to 20% carbon monoxide and from about 15.0 to 60% hydrogen.
The space velocity may range from 500 to 50,000 SCF/CF reactor-hours. Preferably from 1,000 to 10,000 SCF/CF reactor-hours. The temperature may range from 450° to 950° F., preferably, though, 500° to 800° F.
In addition to the nickel type hydrogenation catalyst shown in the example, iron, cobalt, molybdenum, rhenium and other noble metals on heterogeneous supports may be used. Preferably, nickel and promoted nickel catalysts are selected. Any chemically inert support having a low attrition may be used. Examples of these are kieselguhr, alumina, silica-alumina, zirconia, silicon carbide and carbon. The catalyst is in the form of an extrudate, from 3/8 inch to 100 mesh (150 microns) in a spherical or granular form. This particle size is equivalent to 0.006 to 0.375 inches.
The liquid fluidizing medium must be chemically stable and liquid under the reaction conditions. Preferably it is sulfur-free (especially if the catalyst is poisoned by sulfur). Examples of suitable fluidizing media are mineral oils such as Penndrake code 4417 and Sun 21 (a trademark of Sun Oil Company); paraffinic compounds having a boiling range of from 400° F. to 1000° F.; desulfurized gas oils, silicone oils, and liquid polymers of tetrafloroethylene. The velocity of the liquid fluidizing medium is dependent on the physical characteristice of the extrudate catalyst. For example, if a 3/8 inch catalyst is used, the velocity should be from 60 to 100 gpm/ft 2 . For the finer catalysts, such as the 100 mesh type, from 2 to 10 gallon gpm/ft 2 . is sufficient. As a general rule, the liquid flow should be sufficient to expand the bed by at least 5% as compared to its settled state, preferably not more than 30%.
The advantages of the invention over the fixed bed type process can be readily seen by the following comparative example:
The same feed gas and operating conditions shown in the above example are used, except the fixed bed catalyst is in the form of a tablet 1/4 inch × 1/4 inch, the catalyst loading is 0.385 pounds, and the catalyst space velocity is 130 SCF/Hr pounds catalyst. The analysis of the product gas (on a dry basis) shows only 85.6% methane, 10.8% hydrogen and 3.6% carbon monoxide. This increased level of carbon monoxide is particularly striking and evidences clearly the advantage of the process of the invention. | A gas stream containing carbon monoxide and hydrogen is methanated by pasg the gas stream upwardly through a suspension of a finely divided hydrogenation catalyst in a fluidizing medium. The reaction takes place at a temperature of from 450 to 950° F. | 2 |
CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] Not Applicable
STATEMENT REGARDING FEDERALLY SPONSORED RESEARCH OR DEVELOPMENT
[0002] Not Applicable
BACKGROUND OF THE INVENTION
[0003] 1. Field of the Invention
[0004] The present invention relates generally to portable, freestanding room dividers, more particularly, to such room dividers for use in defining exhibition booths in large meeting halls.
[0005] 2. Description of the Related Art
[0006] Trade shows and exhibitions are commonly held in a multipurpose meeting hall which often has a floor area in excess of 150,000 square feet. Although the hall is used undivided for some events, for trade shows and exhibitions it is subdivided into individual exhibit booths in which different companies display goods and services. The smallest standard exhibition booth is ten feet by ten feet, however exhibitors requiring more space can rent larger areas in ten foot by ten foot increments.
[0007] Regardless of its size, each exhibit booth is separated from the adjacent booths by pipe and drape staging. Specifically, the rear and side walls of the booth are defined by a frame of vertical and horizontal pipes from which drapes are hung to provide some degree of privacy for each exhibitor. The vertical pipes for the rear wall extend upward approximately eight feet from a movable metal plate on the hall floor, while the side wall pipes may extend the same height or be waist high from movable metal plates. The horizontal pipes have hooks at the ends which fit into brackets on the vertical pipes thereby forming the frame of the wall. The top horizontal pipe for each wall extends through a hemmed sleeve along the upper edge of the respective drape which then hangs downward from the pipe. Although the pipe and drape staging defines the exhibit booth area, it provides minimal sound insulation between booths and does not provide a surface on which exhibitors can hang displays.
[0008] The staging system for a single wall comprises many individual pieces: metal floor plates, two or more vertical pipes selected from several sizes, one or more horizontal pipes, and the fabric drape material. All of which must be stored in an organized manner between events. Wheeled carts typically are used to transport the staging materials between the storeroom and the exhibition hall. This erecting and dismantling of conventional pipe and drape staging is a labor intensive, time consuming and thus an expensive process. In addition, the nature of the use often requires that the fabric drape material be cleaned after each use.
[0009] Therefore, there is a need for a more convenient and efficient system for defining exhibition booths of various size increments of the standard ten by ten foot floor area.
[0010] Large rooms of schools and churches can be divided into smaller classrooms by portable freestanding dividers, such as described in U.S. Pat. No. 5,272,848. This room divider has a plurality of hinged wall panels positioned between a pair of end members. The wall panels are supported by casters mounted on feet which project laterally from the bottom of the wall panels. The end members also are supported by casters. The combination of wall panels and end members can be folded into a compact configuration for easy movement and storage. The wall panels of the divider can be open at angles to subdivide areas for a classrooms or other uses.
[0011] Heretofore, such prior room dividers for schools and churches did not meet the needs of exhibition halls for a number of reasons. The previous dividers did not conform to the ten foot by ten foot size of the conventional exhibit booth. Dividers of different heights could not easily be attached to each other to create a sturdy standard booth. The rear and side walls of the booth have to be secured to each other not only to prevent separation during use, but for added stability when exhibitors hang heavy displays on the walls. The side walls have to be immobilized during use to withstand people pushing against the walls. Furthermore conventional room dividers do not have handles for easy gripping in order to move the units and do not have a self contained means to lock adjacent room dividers in a 180° position needed to create the perimeter of an exhibit booth.
SUMMARY OF THE INVENTION
[0012] A portable, freestanding room divider system is provided to break up a large hall into one or more exhibition booths. In its basic form, this system comprises first and second sidewall partitions extending from a rear wall partition.
[0013] The rear wall partition is formed by a plurality of wall panels connected together in a series by hinges at their vertical edges. A first wall panel and a last wall panel in the series both have a section along an outer edge that has two opposing sides with a first connector element on each of those sides. A first plurality of feet project outward from at least some of the plurality of wall panels and have wheels thereon to support the rear wall partition on a floor. A first end support extends transversely outward from each side of the first wall panel and a second end support extends transversely outward from each side of the last wall panel. Both of the first and second end supports have a pair of wheels for engaging the floor.
[0014] The first sidewall partition is connected to the first wall panel and the second sidewall partition is connected to the last wall panel, thereby defining three sides of the exhibition booth. Each of the first and second sidewall partitions includes a plurality of sidewall panels connected together in a series by hinges. A first sidewall panel in the series has second connector element that releasably engages one of the first connector elements on the rear wall partition. A second plurality of feet project outward from at least some of the plurality of sidewall panels with at least one wheel thereon for supporting the respective sidewall partition on the floor.
[0015] In a preferred embodiment, a last sidewall panel in the series has a support stand that in a first position engages the floor to resist movement of the sidewall and in a second position allows the sidewall to move on the floor. Preferably, the first connector element on the rear wall partition comprises a pair of keyholes and the second connector element on the sidewall partition comprises a pair of studs that are releasably captivated in the pair of keyholes to secure the sidewall partition to the rear wall partition.
BRIEF DESCRIPTION OF THE DRAWINGS
[0016] FIG. 1 is an isometric view of a portable, freestanding room divider system assembled to form walls of a standard exhibition booth;
[0017] FIG. 2 is an isometric view of the rear wall partition folded for storing and transporting;
[0018] FIG. 3 is a top view of the embodiment of the folded rear wall partition of FIG. 2 ;
[0019] FIG. 4 is a cut away isometric view illustrating a mechanism to attach a side wall partition to the rear wall partition;
[0020] FIG. 5 is an end view of a side wall partition showing a stand which raises the casters above the floor;
[0021] FIG. 6 is an isometric view of several partitions connected to define a plurality of exhibition booths;
[0022] FIG. 7 illustrates a connector mechanism fastening two abutting rear wall dividers together; and
[0023] FIG. 8 is an isometric view of the novel partitions connected to define another configuration of a plurality of exhibition booths.
DESCRIPTION OF THE PREFERRED EMBODIMENT
[0024] With reference to FIG. 1 , a set of room dividers 10 for an exhibition booth comprises a rear wall partition 12 and two side wall partitions 14 and 15 . To comply with conventional dimensions of an exhibition booth, the rear wall partition 12 is ten feet long and stands eight feet high. The rear wall partition 12 comprises five fabric or vinyl covered wall panels 16 , 17 , 18 19 and 20 of equal width and eight feet high and connected vertical edge to vertical edge in series by hinges 30 (see also FIGS. 2 and 3 ). The hinges allow the partition to be folded into a compact configuration for storing and transporting, as will be described.
[0025] Three of the three wall panels 17 , 18 and 19 have a separate foot 32 extending transversely across their bottom edges so as to project outward from both sides of the respective wall panel. A swivel caster 34 is mounted at each end of the foot 32 . The swivel caster 34 are self leveling in that each comprises a wheel held in a mounting bracket from which a rod extends upward through the foot 32 . A spring around the rod biases the mounting bracket downward with respect to the foot 32 .
[0026] The first and last wall panels 16 and 20 in the series that forms the rear wall partition 12 are wider than the other wall panels because the first and last wall panels include a narrower metal end plate 21 or 22 rigidly attached to the outer vertical edge of the respective wall panel. Alternatively the fabric or vinyl covered portion of the first and last wall panels 16 and 20 themselves may be wider than the intermediate wall panels 17 , 18 and 19 . As will be described, the end plates 21 and 22 have elements of connecting mechanisms which enable the side wall partitions 14 and 15 to be securely fastened to the rear wall partition 12 . An end support 24 or 26 extends transversely to each end plate 21 and 22 , respectively, and has a rectangular frame that is attached to the adjacent end plate 21 or 22 . The details of that attachment are shown in FIG. 2 . The frame of end support 26 passes through the end plate 22 which thereby extends outward from the end support. A similar connection exists between the other end plate 21 and its end support 24 . Two swivel casters 36 are mounted beneath each end support 24 and 26 .
[0027] With reference to FIGS. 2 and 3 , the rear wall partition 12 can be folded at hinges 30 so that the major surfaces of the five wall panels 16 - 20 abut against one another. The folded wall panels 16 - 20 fit between the two end supports 24 and 26 . The rear wall partition 12 is held in the folded state by two fasteners 40 adjacent each end plate 21 and 22 . Each fastener 40 comprises a latch hook 41 that is pivotally attached to the respective end plate 21 or 22 and engaging a latch catch 42 attached to the edge of one of the wall panels 17 or 19 . A handle 45 is provided on the end plates to assist the user in folding and unfolding rear wall partition 12 .
[0028] Referring again to FIG. 1 , the two side wall partitions 14 and 15 have identical construction and consist of five side wall panels 50 with vertical edges abutting one another other in the unfolded state. Each of the wall panels 50 is covered with fabric or vinyl. Hinges connect the adjacent wall panels, allowing them to be unfolded into the illustrated linear arrangement and folded together for storage in the same manner as the rear wall partition 12 . The outermost side wall panels 50 have a side wall end plate 52 or 54 fixedly attached to their exposed vertical edge. Alternatively the first and last wall panels 50 of each partition may be wider than the intermediate wall panels. The side wall end plates 52 and 54 have a transverse foot 56 or 57 secured to its bottom edge and a pair of casters 58 is attached to each end of the foot 56 . Similarly, the middle three side wall panels 50 have a similar foot 60 attached transversely to their lower edges with swivel casters 62 mounted near the ends of the foot.
[0029] The foot 56 , attached to the side wall end plate 52 at the remote end of the side wall 14 or 15 from the rear wall 12 , has a support stand 66 pivotally attached thereto. As depicted in FIG. 5 , the foot 56 has a pair of spaced apart brackets 70 projecting outwardly. The support stand 65 is pivotally connected to the two brackets 70 . Specifically, the support stand 65 has a support bar 67 with a pair of foot pads 69 and a pair of legs 66 welded thereto. Each leg 66 is coupled to one of the brackets 70 by a spring loaded pin 72 that extends through holes in both components. This connection enables the support stand 65 to pivot 90° between a lowered position shown by solid lines in the drawing and a raised position depicted by the dashed lines. The raised position is used during storage and transportation of the sidewall partition 14 or 15 . In the lowered position, the foot pads 69 rest on the floor 68 of the exhibition hall so that the casters 58 are raised off the floor, thereby immobilizing the remote end of the respective sidewall partition 14 and 15 .
[0030] The end plate 54 at the opposite end of each sidewall 14 and 15 is coupled to an end plate 21 or 22 of the rear wall partition 12 . As shown in FIGS. 2 and 4 , the rear wall partition 12 has three upper keyholes 76 on adjacent faces of the end plates and a similar trio of lower keyholes 78 . Note that one of the upper and lower keyholes 76 and 78 is on the back surface of the rear wall end plate 22 in FIG. 4 and thus is hidden from view. The vertical edge of each sidewall end plate 54 has two studs 80 for engaging a pair of upper and lower keyholes 76 and 78 on the adjacent rear wall end plate 21 or 22 . When assembling the partitions to form an exhibition booth, the assembler lifts the sidewall end plate 54 using a recessed flush pull handle 77 , so that the heads of the studs 80 are able to pass through the larger diameter portion of each keyhole 76 and 78 . After the studs have been inserted into the keyholes, the end plate 54 of the sidewall is lowered so that the stud shafts enters the narrower portion of the keyholes in which the stud becomes captivated, thereby securing the sidewall 14 or 15 to the rear wall partition 12 . The sidewall partition can be detached from the rear wall partition by lifting the sidewall partition using a recessed flush pull handle 77 , so that the heads of the studs 80 can pass out of the larger diameter portion of the keyholes thereby enabling sidewall partition to be separated from the rear wall partition.
[0031] As also shown in FIG. 4 , each rear wall end plate 21 and 22 has one upper slot 82 and two lower slots 83 to receive the hooks of horizontal pipes used with standard pipe and drape staging. This enables such staging to be used in combination with the rear wall partition 12 . Near the top of each rear wall end plate 21 and 22 are two alignment tabs 84 and 86 that are attached to the two major surfaces of the end plate 22 of rear wall partition 12 . The guide tabs 84 and 86 project from the side edge of the partition so that an adjacent rear wall partition 12 abutting that edge is received between those tabs to provide lateral support for that junction. The guide tabs 84 and 86 are offset vertically on a given rear wall end plate 21 or 22 to accommodate the two guide tabs 84 and 86 on the edge of the abutting rear wall partition 12 .
[0032] When the present room divider system is used to subdivide a large hall into a plurality of exhibition booths as shown in FIG. 6 , a plurality of unfolded rear wall partitions 12 are placed end to end. With reference to FIG. 7 , the abutting edges of two adjacent rear wall partitions 91 and 92 are locked together by a connector 90 which secures the partitions together. A draw latch assembly 93 is attached by screws to the end plate 21 of each partition, partition 92 in the drawings, and has a hinged wing knob 95 connected by a can mechanism to a sliding hook 94 . A keeper 96 is attached by screws to the other end plate 22 of rear wall partition 91 . Rotating the wing knob 95 , slides the hook 94 behind the keeper 96 . Further rotation of the wing knob 95 draws the hook toward its room divider 92 and against the keeper 96 , thereby securing the two room dividers 91 and 92 together. Connecting the rear wall partitions in this manner adds to the stability of the exhibition booth walls and provides greater privacy between exhibitors than prior pipe and drape staging.
[0033] Referring to the configuration 100 of a plurality of exhibition booths shown in FIG. 6 , a separate sidewall partition 108 , 110 , 114 and 116 is attached to one of the end plates 21 or 22 at the junction between two rear wall partitions 102 , 104 and 106 . These sidewall partitions extend on both sides of these rear wall partitions, thereby forming back to back exhibition booths. An additional pair of sidewall partitions 112 and 118 are attached at the exposed end of the outer most rear wall partition 106 to define the final pair of exhibition booths along the rear walls. If a particular exhibitor desires to have a larger booth, one or more of the interior sidewalls, such as unit 110 , can be eliminated to form a larger width booth.
[0034] FIG. 8 illustrates an alternative configuration 120 for creating a larger exhibition booth by placing two sidewall partitions 128 and 130 and 132 and 134 aligned end to end so that the booth is twenty feet deep. The studs 80 on the end support 129 of one sidewall partition 130 and 134 of each sidewall engage the keyholes in the end section 131 of the other sidewall partition 128 and 132 , respectively to lock the aligned sidewall partitions together. The partition configuration 120 also illustrates how two rear wall partitions 122 and 124 can be placed end to end without an intermediate sidewall partition so that the booth is twenty feet wide.
[0035] As will be appreciated by one skilled in the art, the present room divider system with the unique fastening mechanism can be interlocked in a large variety of configurations to provide exhibition booths that are customized to the needs of a particular exhibitor. Those configurations include sidewall or rear wall partitions positioned in a continuous straight line, partitions interlocked at 90° or 270° orientations, and any curvilinear configurations as allowed by such positioning of the hinged panels
[0036] The foregoing description was primarily directed to preferred embodiments of the invention. Although some attention was given to various alternatives within the scope of the invention, it is anticipated that one skilled in the art will likely realize additional alternatives that are now apparent from disclosure of embodiments of the invention. Accordingly, the scope of the invention should be determined from the following claims and not limited by the above disclosure. | A portable, freestanding room divider system comprises first and second sidewall partitions extending from one or more rear wall partitions to define exhibition booths. Each rear wall and side wall partition has a plurality of wall panels hinged together in a series. The rear wall partition includes first and last wall panels with end panels that have keyholes on opposites sides and an end support with wheels. An end wall panel of each sidewall partition has studs that engage the keyholes to secure the sidewall partition to the rear wall partition. At least some of the wall panels of the rear and sidewall partitions have feet projecting outward therefrom with wheels. A foot on each sidewall has a stand which raises and lowers the wheels with respect to the floor to control movement of the sidewall. | 4 |
CROSS-REFERENCE TO RELATED APPLICATION
[0001] The benefit of the filing date of U.S. Provisional Patent Application No. 61/804,922, filed Mar. 25, 2013, is hereby claimed. The entire disclosure of the aforesaid application is incorporated herein by reference.
REFERENCE TO GOVERNMENT GRANT
[0002] The invention was made with government support under grant no. 1R15DE021016-01 awarded by the National Institutes of Health. The government has certain rights in the invention.
SEQUENCE LISTING
[0003] The instant application contains a Sequence Listing which has been submitted in ASCII format via EFS-Web and is hereby incorporated by reference in its entirety. Said ASCII copy, created on Mar. 21, 2014, is named 035926 — 0479 — 00_WO_SL.txt and is 256,052 bytes in size.
FIELD OF INVENTION
[0004] The invention relates to bacteriophages that infect strains of Enterococcus faecalis , an opportunistic bacterial pathogen that causes human disease, and therapeutic uses thereof.
BACKGROUND OF THE INVENTION
[0005] E. faecalis , and closely related species, such as E. faecium , have emerged as significant human pathogens, being major etiologic agents of infectious endocarditis, nosocomial infections, burn infections, urinary tract infections, meningitis, and surgical wound infections (Lerwis & Zervos, Eur J. Clin Microbiol Infect Dis 9(2): 111-117, 1990; Moellering Jr., Clin. Infect. Dis. 14(6): 1173-1176, 1992; Megran, Clinical Infect. Dis. 15: 63-71, 1992; Emori & Gaynes, Clin. Microbiol. Rev. 6(4): 428-442, 1993; Jett et al., 1994; Edgeworth et al., Crit. Care Med. 28(8): 1421-1428, 1999; Richards et al., Infection Control Hosp. Epidemiol. 21(8): 510-515, 2000; NNIA System, Am J Infect Control, 32: 470-485, 2004; Biedenbach et al., Diagn. Microbiol. Infect. Dis. 50: 59-69 2004; Linden, Semin. Respir. Crit. Care Med. 28: 632-645, 2007). In terms of oral disease, E. faecalis is the most commonly isolated species from infected root canals of teeth that fail to heal following root canal therapy (Sundqvist et al., Oral Surg. Oral Med. Oral Pathol. Oral Radiol. And Endod. 85(1): 86-93, 1998; Peciuliene et al., J. Endod. 26(10): 593-595, 2000; Pinheiro et al., Int. Endod. J. 36: 1-11, 2003; Siqueira Jr. & Rôças, Oral Surg. Oral Med. Oral Pathol. Oral Radiol. Endod. 97: 85-94, 2004; Stuart et al., J. Endod. 32(2): 93-98 2006; Zoletti et al., J Endod. 32(8): 722-726 2006).
[0006] The existing standard treatment for infections, including those due to enterococci, continues to involve the use of antibiotics. In the case of severe enterococcal infections, the regimen typically includes a cell wall active antibiotic, such as a penicillin or cephalosporin plus an aminoglycoside such as streptomycin (Megran, CID 15:63-71, 1992; Noskin, J Lab Clin Med 130:14-20, 1997). As resistance to these drugs became more common, vancomycin replaced these antibiotics as the drug of choice for treating these infections.
[0007] Complicating management of these infections is the development of resistance among many Enterococcal strains against many of the available, previously effective antibiotics, including vancomycin (Harvard et al., Br. Med. J. 1: 688-689, 1959; Murray & Mederski-Samaroj, J. Clin. Invest., 72: 1168-1171, 1983; Uttley et al., Lancet , i: 57-58, 1988; Grayson et al., Antimicrob. Agents Chemother., 35: 2180-2184, 1991; Bonten et al., Lancet Infect. Dis. 1: 314-325, 2001; Tenover & McDonald, Curr. Opin. Infect. Dis. 18: 300-305, 2005). With the appearance of vancomycin resistant enterococci (VREs) that were also resistant to the previously used antibiotics, combinations of vancomycin and quinolone type antibiotics, such as ciprofloxacin, were used, however, quinolone-resistant enterococcal strains also appeared. Although a modest number of new antibiotics, such as linezolid and daptomycin, have been developed to provide treatment alternatives in cases of infection by organisms that are resistant to all previously available antibiotics, there have been numerous reports of resistance by E. faecalis and E. faecium strains to these antibiotics as well (Eliopoulos et al., Antimicrob. Agents Chemother., 45(5): 1088-1092, 1998; Prystowsky et al., Antimicrob. Agents Chemother., 45(7): 2154-2156, 2001; Gonzales et al., Lancet 357(9263): 1179, 2002; Herrero et al., N Eng J Med 346: 867-860, 2002; Johnson et al., Int. J. Antimicrob. Agents 24: 315-319, 2004; Munoz-Price et al., Clin. Infect. Dis., 41: 565-566, 2005; Kanafani et al., Scand. J. Infect. Dis., 39(1): 75-77, 2007; Hidron et al., J Antimicrob. Chemother., 61(6): 1394-1396, 2008; Marshall et al., Microbe, 4(5): 231-238, 2009; Kelesidis et al., Clin. Infect. Dis., 52: 228-234, 2011; Ross et al., J. Chemother., 23(2): 71-76, 2011; Ntokou et al., Antimicrob. Chemother. 67(8): 1819-1823, 2012). Therefore, alternative approaches to manage these infections are desired.
[0008] Bacteriophages are bacterial viruses that infect bacterial cells. During their infectious cycle within a host cell, the bacterial virus produces enzymes that will lead to the lysis of the cell and release of progeny virus particles. Harnessing this capacity of the bacteriophage to lyse and kill the host cell may provide a means of controlling antibiotic resistant bacterial infections. This approach, of using bacteriophages to treat and control bacterial infections has several advantages. Bacteriophages are highly specific in that they are only infectious for bacterial cells, and have no capacity for infecting cells of higher life forms such as mammals. In fact, they are so specific that the host range of any one bacteriophage is typically a single bacterial species, or at most, a few closely related bacterial species. Therefore, the effect of any one bacteriophage is limited to a very narrow portion of a mixed bacterial population. This provides an impact on the pathogenic bacteria while leaving the normal bacterial population unaffected. Both antibiotic sensitive and antibiotic resistant bacterial strains can be vulnerable to bacteriophage infection. In addition, in contrast to conventional antibiotics which decrease in concentration in the body after administration, bacteriophage titer can increase after administration, due to proliferation of the virus in the targeted host cell.
[0009] The therapeutic potential of bacteriophages was tested in 1919 by d'Herelle, who showed that bacteriophage preparations could be used to successfully treat cases of dysentery (described in Chanishvili, Advances in Virus Res. 83: 3-40, 2012). Further work continued, particularly in eastern Europe, on the use of bacteriophages (“phages”) to treat infectious diseases (Barrow, J Chem Technol Biotechnol 76: 677-682, 2001; Duckworth and Gulig Biodrugs, 16(1): 57-62, 2002, Petty et al. TRENDS in Biotechnol., 25(1): 7-15, 2006; Chanishvili, supra). With the advent of antibiotics in the 1940s, this line of research (phage therapy) fell by the wayside in the west since antibiotics were remarkably effective in combating many bacterial infections. However, in eastern Europe, where availability of antibiotics was limited, research into phage therapy continued, particularly in the Soviet Union, Georgia, and Poland. Here, the therapeutic use of phages became an accepted modality for treating a wide variety of bacterial infections.
[0010] Since the 1980s, as antibiotic resistance in pathogenic bacteria began to develop, and become more common in the West, there has been a resurgence in interest in using phages to treat human and animal infections (Summers, Annu. Rev. Microbiol. 55: 437-451, 2001, Alisky et al., J. of Infec. 36: 5-15, 1998, Pirisi, Lancet. 356: 1418, 2000; Ho, Perspectives in Biology and Medicine, 44(1): 1-16, 2001; Merril et al., Naure Revs. Drug Disc. 2: 489-497, 2003; Bradbury, Lancet. 363: 624-625, 2004; Dixon, Lancet Infect Dis. 4: 186, 2004; Schoolnik et al., Nature 22(5): 505-506, 2004; Thiel, Nature 22(1): 31-36, 2004; Skurnik and Strauch, Int. J. Med. Microbiol. 296: 5-14, 2005).
[0011] Several recent studies report successful implementation of phage therapy (using either infectious bacteriophages or phage products) in modifying bacterial infections in animals by Acinetobacter baumanii, Escherichia coli , group A streptococci, Enterococcus faecium, Bacillus anthracis , and Pseudomonas aeruginosa (Soothill, J. Med. Microbiol. 37: 258-261, 1992; Merril et al., Proc. Natl. Acad. Sci. USA. 93: 3188-3192, 1996; Nelson et al., Proc. Nat. Acad. Sci. 98(7): 4107-4112, 2001; Biswas et al., Infect. Immun. 70(1): 204-210, 2002; Schuch et al., Nature 418: 884-889, 2002; Watanabe et al., Antimicrob. Agents Chemother. 51: 446-452, 2007). In this regard, it is significant to note that in a study reported by Smith and Huggins, J Gen Microbiol 128: 307-318 (1982), a single intramuscular (IM) dose of phage was more effective in protecting mice from normally lethal IM or intracerebral injections of Escherichia coli or Salmonella enterica , than multiple IM injections of antibiotics such as tetracycline, ampicillin, chloramphenicol, or trimethoprim plus sulfisoxazole. In addition, in the first controlled trial of phage therapy in humans, it was shown that a cocktail of six Pseudomonas aeruginosa bacteriophages effectively treated antibiotic-resistant chronic otitis (Wright et al, Clin. Otolaryngol. 34: 349-357, 2009).
[0012] In terms of phage therapy to treat E. faecalis infections, there has been relatively little reported. In 2004, Paisano et al., Oral Microbiol Immunol, 19: 327-330 reported that they could reduce the level of infection of a single E. faecalis strain in an infected dental root canal (in vitro), to an undetectable level, using a bacteriophage preparation. However, the bacteriophage used in this study was not characterized in any way (no morphological description, no genomic analysis).
[0013] Isolation of a bacterial virus (phage φEF24C) that could protect mice from otherwise lethal doses of E. faecalis has been reported (Uchiyama et al., FEMS Microbiol Lett. 278: 200-206, 2008; Uchiyama et al., Appl Environ Microbiol. 74(13): 4149-4163, 2008). This bacteriophage was reported to have a broad range of activity against many strains of E. faecalis , and have no untoward effects on the mice. This phage was well characterized and could be described as follows: φEF24C has a contractile tail, giving it the morphology of a Myovirdae type bacteriophage. Its genome consisted of a linear, double stranded DNA, 142,072 by in length, with an estimated 221 ORFs and 5 tRNA genes.
[0014] Other strategies for exploiting bacteriophages for controlling E. faecalis infections involve the use of lytic enzymes produced by the viruses to lyse and kill the bacterial cells. The cell lysis produced by these enzymes is needed by the virus in order to allow the release of progeny viral particles from the infected cells. The strategy for exploiting these bacteriophage-specified lytic enzymes involves the cloning and expression of the genes for these enzymes, followed by the purification of the expressed proteins. One such lytic enzyme, active against strains of E. faecalis (as well as strains of E. faecium , and several Streptococcus species), has reportedly been isolated from E. faecalis bacteriophage φ1 (Yoong et al., J Bacteria 186(145): 4808-4812, 2004). The bacteriophage source of this enzyme, phage φ1, was described as a Myoviridae morphotype; that is, a bacteriophage with a contractile tail. A second report of a bacteriophage lytic enzyme active against strains of E. faecalis came from Son et al., Appl. Microbiol. 108: 1769-1779 (2010). Here, the gene for a putative lytic enzyme specified by E. faecalis bacteriophage EFAP-1 was cloned, and expressed, and the gene product was purified. The purified phage protein was found to have lytic activity against numerous strains of E. faecalis and E. faecium . Bacteriophage EFAP-1, the source of the lytic enzyme described by Son et al., had the non-contractile tail structure of a Siphovirdae morphotype. EFAP-1 had a 21,115 bp genome containing 24 ORFs.
[0015] Several other bacterial viruses that infect strains of E. faecalis have been reported. These include: Bacteriophages φFC1 (Yang et al., J. Bacteriol. 184: 1859-1864, 2002), F4 (Nigutova et al., Folio Microbiol. 53(3): 234-236, 2008), phages 31, 42, 54, and 70 (Mazaheri Nezhad Fard et al., Curr Microbiol. 60: 400-406, 2010), VD13 (Ackermann et al., Can. J. Microbiol., 21: 571-574, 1975), phages 1 and 2 (Rogers and Sarles, J. Bacteriol. 85: 1378-1385, 1963), SAP6 (Lee and Park, J. Virol. 86(17): 9538-9539, 2012), BC-611 (Horiuchi et al., J. Virol. 86(17): 9538-9539, 2012), and phages φFL1A, φFL1B, φFL1C, φFL2A, φFL2B, φFL3A, φFL3B and φFL4A (Yasmin et al., J. Bacteriol. 192(4): 1122-1130, 2010). In addition several unnamed E. faecalis bacteriophages have been reported (Natkin, Arch Oral Biol. 12(5): 669-680, 1967, Timperley et al., J. Pathol. Bacteriol. 9: 631-634, 1966, Follett et al., J. Gen. Virol. 1: 281-284, 1967, Letkiewicz et al., Folio Microbiol. 54: 457-461, 2009, and Bachrach et al., Lett. Appl. Microbiol. 36: 50-53, 2003). However, none of these have been proposed for use in phage therapy.
[0016] φEfl1 is a temperate bacteriophage that was induced from a lysogenic root canal isolate of Enterococcus faecalis (Stevens et al., Oral Microbiol. Immunobiol., 24: 278-284, 2009). φEfl1 prophage is widely disseminated among strains of E. faecalis . It is a member of the Siphoviridae family, with a long (130 nm) non-contractile tail and a small (41 nm diameter) spherical/icosahedral head. The phage produces small, turbid plaques in lawns of E. faecalis JH2-2. The φEfl1 DNA has been sequenced and annotated, disclosing a genome of 42,822 base pairs encoding 65 Open Reading Frames (Stevens et al., FEMS Microbiol. Lett., 317: 9-26, 2011, incorporated herein by reference; GenbankGQ452243.1, incorporated herein by reference).
[0017] The φEfl1 genome is shown in FIG. 10 . The numbered arrows indicate ORFs. The ORF numbering scheme in FIG. 10 corresponds to the numbering system contained in Stevens et al., 2011, supra. ORFs 25-29 are involved in host cell lysis.
[0018] φEfl1 possesses several characteristics making it a favorable candidate virus to be used in phage therapy: There are no toxin-related genes detected in the φEfl1 genome, and it encodes several (4-6) genes encoding proteins with lysis-associated functions (Stevens et al., 2011, supra). However, as a temperate virus that has a very limited host range, and is difficult to propagate, wild-type φEfl1 would not be suitable as a potential therapeutic agent.
[0019] Moreover, since φEfl1 is a temperate bacteriophage, it possesses a module of genes that allows it to integrate its DNA into the host cell chromosome rather than initiating a productive infection and lysing the infected cell. The bacteriophage DNA can remain in this integrated state indefinitely, and the infected cell (a lysogen) will survive and continue to multiply. Furthermore, regulatory elements in the φEfl1 genome whose activation is required for the development of a productive/lytic infection within the cell, are inactivated by a protein (repressor) produced by one of the lysogeny-related genes. Therefore, lysogenic cells producing this repressor are immune to super infection by φEfl1, and would consequently survive exposure to this virus. This further limits the utility of φEfl1 as therapeutic agent
SUMMARY OF THE INVENTION
[0020] Provided is a bacteriophage capable of infecting and lysing an Enterococcus faecalis bacterium, said bacteriophage having a genome comprising:
[0021] (A) the following ORFs with the corresponding Protein ID Numbers from Genbank Accession Number GQ452243, or having the following nucleic acid sequence:
(a) ORF 2, encoding the amino acid sequence of SEQ ID NO: 28, corresponding to Protein ID Number YP 003358792.1; (b) ORF 3, encoding the amino acid sequence of SEQ ID NO: 29, corresponding to Protein ID Number YP 003358793.1; (c) ORF 4, encoding the amino acid sequence of SEQ ID NO: 30, corresponding to Protein ID Number YP 003358794.1; (d) ORF 5, encoding the amino acid sequence of SEQ ID NO: 31, corresponding to Protein ID Number YP 003358795.1; (e) ORF 6, encoding the amino acid sequence of SEQ ID NO: 32, corresponding to Protein ID Number YP 003358796.1; (f) ORF 7, encoding the amino acid sequence of SEQ ID NO: 33, corresponding to Protein ID Number YP 003358797.1; (g) ORF 8, encoding the amino acid sequence of SEQ ID NO: 34, corresponding to Protein ID Number YP 003358798.1; (h) ORF 9, encoding the amino acid sequence of SEQ ID NO: 35, corresponding to Protein ID Number YP 003358799.1; (i) ORF 10, encoding the amino acid sequence of SEQ ID NO: 36, corresponding to Protein ID Number YP 003358800.1; (j) ORF 11, encoding the amino acid sequence of SEQ ID NO: 37, corresponding to Protein ID Number YP 003358801.1; (k) ORF 12, encoding the amino acid sequence of SEQ ID NO: 38, corresponding to Protein ID Number YP 003358802.1; (l) ORF 13, encoding the amino acid sequence of SEQ ID NO: 39, corresponding to Protein ID Number YP 003358803.1; (m) ORF 14, encoding the amino acid sequence of SEQ ID NO: 40, corresponding to Protein ID Number YP 003358804.1; (n) ORF 15, encoding the amino acid sequence of SEQ ID NO: 41, corresponding to Protein ID Number YP 003358805.1; (o) ORF 16, encoding the amino acid sequence of SEQ ID NO: 42, corresponding to Protein ID Number YP 003358806.1; (p) ORF 17, encoding the amino acid sequence of SEQ ID NO: 43, corresponding to Protein ID Number YP 003358807.1; (q) ORF 18, encoding the amino acid sequence of SEQ ID NO: 44, corresponding to Protein ID Number YP 003358808.1; (r) ORF 19, encoding the amino acid sequence of SEQ ID NO: 45, corresponding to Protein ID Number YP 003358809.1; (s) ORF 20, encoding the amino acid sequence of SEQ ID NO: 46, corresponding to Protein ID Number YP 003358810.1; (t) ORF 21, encoding the amino acid sequence of SEQ ID NO: 47, corresponding to Protein ID Number YP 003358811.1; (u) ORF 22, encoding the amino acid sequence of SEQ ID NO: 48, corresponding to Protein ID Number YP 003358812.1; (v) ORF 23, encoding the amino acid sequence of SEQ ID NO: 49, corresponding to Protein ID Number YP 003358813.1; (w) ORF 24, encoding the amino acid sequence of SEQ ID NO: 50, corresponding to Protein ID Number YP 003358814.1; (x) ORF 25, encoding the amino acid sequence of SEQ ID NO: 51, corresponding to Protein ID Number YP 003358815.1; (y) ORF 26, encoding the amino acid sequence of SEQ ID NO: 52, corresponding to Protein ID Number YP 003358816.1; (z) ORF 27, encoding the amino acid sequence of SEQ ID NO: 53, corresponding to Protein ID Number YP 003358817.1; (aa) ORF 28, encoding the amino acid sequence of SEQ ID NO: 54, corresponding to Protein ID Number YP 003358818.1; (bb) ORF 29, encoding the amino acid sequence of SEQ ID NO: 55, corresponding to Protein ID Number YP 003358819.1; (cc) ORF 30, encoding the amino acid sequence of SEQ ID NO: 56, corresponding to Protein ID Number YP 003358820.1; (dd) ORF 37, encoding the amino acid sequence of SEQ ID NO: 63, corresponding to Protein ID Number YP 003358827.1; (ee) ORF 38, encoding the amino acid sequence of SEQ ID NO: 64, corresponding to Protein ID Number YP 003358828.1; (ff) ORF 39, encoding the amino acid sequence of SEQ ID NO: 65, corresponding to Protein ID Number YP 003358829.1; (gg) ORF 40, encoding the amino acid sequence of SEQ ID NO: 66, corresponding to Protein ID Number YP 003358830.1; (hh) ORF 41, encoding the amino acid sequence of SEQ ID NO: 67, corresponding to Protein ID Number YP 003358831.1; (ii) ORF 42, encoding the amino acid sequence of SEQ ID NO: 68, corresponding to Protein ID Number YP 003358832.1; (jj) ORF 43, encoding the amino acid sequence of SEQ ID NO: 69, corresponding to Protein ID Number YP 003358833.1; (kk) ORF 44, encoding the amino acid sequence of SEQ ID NO: 70, corresponding to Protein ID Number YP 003358834.1; (ll) ORF 45, encoding the amino acid sequence of SEQ ID NO: 71, corresponding to Protein ID Number YP 003358835.1; (mm) ORF 46, encoding the amino acid sequence of SEQ ID NO: 72, corresponding to Protein ID Number YP 003358836.1; (nn) ORF 47, encoding the amino acid sequence of SEQ ID NO: 73, corresponding to Protein ID Number YP 003358837.1; (oo) ORF 48, encoding the amino acid sequence of SEQ ID NO: 74, corresponding to Protein ID Number YP 003358838.1; (pp) ORF 49, encoding the amino acid sequence of SEQ ID NO: 75, corresponding to Protein ID Number YP 003358839.1; (qq) ORF 50, encoding the amino acid sequence of SEQ ID NO: 76, corresponding to Protein ID Number YP 003358840.1; (rr) ORF 51, encoding the amino acid sequence of SEQ ID NO: 77, corresponding to Protein ID Number YP 003358841.1; (ss) ORF 52, encoding the amino acid sequence of SEQ ID NO: 78, corresponding to Protein ID Number YP 003358842.1; (tt) ORF 53, encoding the amino acid sequence of SEQ ID NO: 79, corresponding to Protein ID Number YP 003358843.1; (uu) ORF 54, encoding the amino acid sequence of SEQ ID NO: 80, corresponding to Protein ID Number YP 003358844.1; (vv) ORF 55, encoding the amino acid sequence of SEQ ID NO: 81, corresponding to Protein ID Number YP 003358845.1; (ww) ORF 56, encoding the amino acid sequence of SEQ ID NO: 82, corresponding to Protein ID Number YP 003358846.1; (xx) ORF 57, encoding the amino acid sequence of SEQ ID NO: 83, corresponding to Protein ID Number YP 003358847.1; (yy) ORF 58, encoding the amino acid sequence of SEQ ID NO: 84 corresponding to Protein ID Number YP 003358848.1; and (zz) ORF 59, encoding the amino acid sequence of SEQ ID NO: 85, corresponding to Protein ID Number YP 003358849.1; (aaa) ORF 60, encoding the amino acid sequence of SEQ ID NO: 86, corresponding to Protein ID Number YP 003358850.1; (bbb) a portion of ORF 1, having the nucleic acid sequence of SEQ ID NO: 170;
[0077] (B) an inducible or constitutive promoter immediately upstream of ORF 37; and
[0078] (C) the following ORFs from bacteriophage ΦFL1C:
(a) ORF 40 encoding the amino acid sequence of SEQ ID NO: 158; (b) ORF 41 encoding the amino acid sequence of SEQ ID NO: 159; (c) ORF 42 encoding the amino acid sequence of SEQ ID NO: 160; (d) ORF 43 encoding the amino acid sequence of SEQ ID NO: 161; (e) ORF 44 encoding the amino acid sequence of SEQ ID NO: 162.
[0084] In some embodiments, the bacteriophage has a genome comprising:
[0085] (A) the following ORFs having the corresponding Gene ID Numbers from Genbank Accession Number GQ452243, or having the following nucleic acid sequence:
(a) ORF 2, the nucleic acid sequence of SEQ ID NO: 94, corresponding to Gene ID Number 8683900; (b) ORF 3, the nucleic acid sequence of SEQ ID NO: 95, corresponding to Gene ID Number 8683888; (c) ORF 4, the nucleic acid sequence of SEQ ID NO: 96, corresponding to Gene ID Number 8683893; (d) ORF 5, the nucleic acid sequence of SEQ ID NO: 97, corresponding to Gene ID Number 8683933; (e) ORF 6, the nucleic acid sequence of SEQ ID NO: 98, corresponding to Gene ID Number 8683946; (f) ORF 7, the nucleic acid sequence of SEQ ID NO: 99, corresponding to Gene ID Number 8683941; (g) ORF 8, the nucleic acid sequence of SEQ ID NO: 100, corresponding to Gene ID Number 8683932; (h) ORF 9, the nucleic acid sequence of SEQ ID NO: 101, corresponding to Gene ID Number 8683887; (i) ORF 10, the nucleic acid sequence of SEQ ID NO: 102, corresponding to Gene ID Number 8683904; (j) ORF 11, the nucleic acid sequence of SEQ ID NO: 103, corresponding to Gene ID Number 8683926; (k) ORF 12, the nucleic acid sequence of SEQ ID NO: 104, corresponding to Gene ID Number 8683911; (l) ORF 13, the nucleic acid sequence of SEQ ID NO: 105, corresponding to Gene ID Number 8683923; (m) ORF 14, the nucleic acid sequence of SEQ ID NO: 106, corresponding to Gene ID Number 8683914; (n) ORF 15, the nucleic acid sequence of SEQ ID NO: 107, corresponding to Gene ID Number 8683916; (o) ORF 16, the nucleic acid sequence of SEQ ID NO: 108, corresponding to Gene ID Number 8683884; (p) ORF 17, the nucleic acid sequence of SEQ ID NO: 109, corresponding to Gene ID Number 8683912; (q) ORF 18, the nucleic acid sequence of SEQ ID NO: 110, corresponding to Gene ID Number 8683919; (r) ORF 19, the nucleic acid sequence of SEQ ID NO: 111, corresponding to Gene ID Number 8683929; (s) ORF 20, the nucleic acid sequence of SEQ ID NO: 112, corresponding to Gene ID Number 8683927; (t) ORF 21, the nucleic acid sequence of SEQ ID NO: 113, corresponding to Gene ID Number 8683928; (u) ORF 22, the nucleic acid sequence of SEQ ID NO: 114, corresponding to Gene ID Number 8683935; (v) ORF 23, the nucleic acid sequence of SEQ ID NO: 115, corresponding to Gene ID Number 8683908; (w) ORF 24, the nucleic acid sequence of SEQ ID NO: 116, corresponding to Gene ID Number 8683924; (x) ORF 25, the nucleic acid sequence of SEQ ID NO: 117, corresponding to Gene ID Number 8683907; (y) ORF 26, the nucleic acid sequence of SEQ ID NO: 118, corresponding to Gene ID Number 8683925; (z) ORF 27, the nucleic acid sequence of SEQ ID NO: 119, corresponding to Gene ID Number 8683889; (aa) ORF 28, the nucleic acid sequence of SEQ ID NO: 120, corresponding to Gene ID Number 8683944; (bb) ORF 29, the nucleic acid sequence of SEQ ID NO: 121, corresponding to Gene ID Number 8683920; (cc) ORF 30, the nucleic acid sequence of SEQ ID NO: 122, corresponding to Gene ID Number 8683896; (dd) ORF 37, the nucleic acid sequence of SEQ ID NO: 129, corresponding to Gene ID Number 8683921; (ee) ORF 38, the nucleic acid sequence of SEQ ID NO: 130, corresponding to Gene ID Number 8683898; (ff) ORF 39, the nucleic acid sequence of SEQ ID NO: 131, corresponding to Gene ID Number 8683895; (gg) ORF 40, the nucleic acid sequence of SEQ ID NO: 132, corresponding to Gene ID Number 8683940; (hh) ORF 41, the nucleic acid sequence of SEQ ID NO: 133, corresponding to Gene ID Number 8683917; (ii) ORF 42, the nucleic acid sequence of SEQ ID NO: 134, corresponding to Gene ID Number 8683897; (jj) ORF 43 the nucleic acid sequence of SEQ ID NO: 135, corresponding to Gene ID Number 8683894; (kk) ORF 44, the nucleic acid sequence of SEQ ID NO: 136, corresponding to Gene ID Number 8683883; (ll) ORF 45, the nucleic acid sequence of SEQ ID NO: 137, corresponding to Gene ID Number 8683903; (mm) ORF 46, the nucleic acid sequence of SEQ ID NO: 138, corresponding to Gene ID Number 8683943; (nn) ORF 47, the nucleic acid sequence of SEQ ID NO: 139, corresponding to Gene ID Number 8683913; (oo) ORF 48, the nucleic acid sequence of SEQ ID NO: 140, corresponding to Gene ID Number 8683910; (pp) ORF 49, the nucleic acid sequence of SEQ ID NO: 141, corresponding to Gene ID Number 8683937; (qq) ORF 50, the nucleic acid sequence of SEQ ID NO: 142, corresponding to Gene ID Number 8683915; (rr) ORF 51, the nucleic acid sequence of SEQ ID NO: 143, corresponding to Gene ID Number 8683885; (ss) ORF 52, the nucleic acid sequence of SEQ ID NO: 144, corresponding to Gene ID Number 8683890; (tt) ORF 53, the nucleic acid sequence of SEQ ID NO: 145, corresponding to Gene ID Number 8683886; (uu) ORF 54, the nucleic acid sequence of SEQ ID NO: 146, corresponding to Gene ID Number 8683909; (vv) ORF 55, the nucleic acid sequence of SEQ ID NO: 147, corresponding to Gene ID Number 8683902; (ww) ORF 56, the nucleic acid sequence of SEQ ID NO: 148, corresponding to Gene ID Number 8683931; (xx) ORF 57, the nucleic acid sequence of SEQ ID NO: 149, corresponding to Gene ID Number 8683930; (yy) ORF 58, the nucleic acid sequence of SEQ ID NO: 150 corresponding to Gene ID Number 8683899; and (zz) ORF 59, the nucleic acid sequence of SEQ ID NO: 151, corresponding to Gene ID Number 8683936; (aaa) ORF 60, the nucleic acid sequence of SEQ ID NO: 152, corresponding to Gene ID Number 8683942; (bbb) a portion of ORF 1, having the nucleic acid sequence of SEQ ID NO: 170;
[0140] (B) an inducible or constitutive promoter immediately upstream of ORF 37; and
[0141] (C) the following ORFs from bacteriophage ΦFL1C:
(a) ORF 40 having the nucleic acid sequence of SEQ ID NO: 163; (b) ORF 41 having the nucleic acid sequence of SEQ ID NO: 164; (c) ORF 42 having the nucleic acid sequence of SEQ ID NO: 165; (d) ORF 43 having the nucleic acid sequence of SEQ ID NO: 166; (e) ORF 44 having the nucleic acid sequence of SEQ ID NO: 167.
[0147] In some embodiments the bacteriophage has the genome of the bacteriophage ΦEfl1 from Genbank Accession Number GQ452243, corresponding to SEQ ID NO: 92:
[0148] (A) wherein the following ORFs have been deleted:
(a) a portion of ORF 1 having the nucleic acid sequence of SEQ ID NO: 169; (b) ORF 31, encoding the amino acid sequence of SEQ ID NO: 57, corresponding to Protein ID Number YP 003358821.1; (c) ORF 32, encoding the amino acid sequence of SEQ ID NO: 58, corresponding to Protein ID Number YP 003358822.1; (d) ORF 33, encoding the amino acid sequence of SEQ ID NO: 59, corresponding to Protein ID Number YP 003358823.1; (e) ORF 34, encoding the amino acid sequence of SEQ ID NO: 60, corresponding to Protein ID Number YP 003358824.1; (f) ORF 35, encoding the amino acid sequence of SEQ ID NO: 61, corresponding to Protein ID Number YP 003358825.1; (g) ORF 36, encoding the amino acid sequence of SEQ ID NO: 62, corresponding to Protein ID Number YP 003358826.1; (h) ORF 61, encoding the amino acid sequence of SEQ ID NO: 87, corresponding to Protein ID Number YP 003358851.1; (i) ORF 62, encoding the amino acid sequence of SEQ ID NO: 88, corresponding to Protein ID Number YP 003358852.1; (j) ORF 63, encoding the amino acid sequence of SEQ ID NO: 89, corresponding to Protein ID Number YP 003358853.1; (k) ORF 64, encoding the amino acid sequence of SEQ ID NO: 90, corresponding to Protein ID Number YP 003358854.1; (l) ORF 65, encoding the amino acid sequence of SEQ ID NO: 91 corresponding to Protein ID Number YP 003358855.1;
[0161] (B) wherein the P CRO promoter between ORFs 36 and 37 has been replaced with an inducible promoter or a constitutive promoter; and
[0162] (C) comprising the following ORFs from bacteriophage ΦFL1C:
(a) ORF 40 encoding the amino acid sequence of SEQ ID NO: 158; (b) ORF 41 encoding the amino acid sequence of SEQ ID NO: 159; (c) ORF 42 encoding the amino acid sequence of SEQ ID NO: 160; (d) ORF 43 encoding the amino acid sequence of SEQ ID NO: 161; (e) ORF 44 encoding the amino acid sequence of SEQ ID NO: 162.
[0168] In yet further embodiments the bacteriophage has the genome of the ΦEFl1 bacteriophage that is comprised by Enterococcus faecalis NRRL Deposit Number NRRL B-50832, deposited on Mar. 22, 2013:
[0169] (A) wherein the following ORFs have been deleted, which have the following nucleic acid sequence, or the following amino acid sequences, corresponding to the following Protein ID Numbers from Genbank Accession Number GQ452243:
(a) a portion of ORF 1 having the nucleic acid sequence of SEQ ID NO: 169; (b) ORF 31, encoding the amino acid sequence of SEQ ID NO: 57, corresponding to Protein ID Number YP 003358821.1; (c) ORF 32, encoding the amino acid sequence of SEQ ID NO: 58, corresponding to Protein ID Number YP 003358822.1; (d) ORF 33, encoding the amino acid sequence of SEQ ID NO: 59, corresponding to Protein ID Number YP 003358823.1; (e) ORF 34, encoding the amino acid sequence of SEQ ID NO: 60, corresponding to Protein ID Number YP 003358824.1; (f) ORF 35, encoding the amino acid sequence of SEQ ID NO: 61, corresponding to Protein ID Number YP 003358825.1; (g) ORF 36, encoding the amino acid sequence of SEQ ID NO: 62, corresponding to Protein ID Number YP 003358826.1; (h) ORF 61, encoding the amino acid sequence of SEQ ID NO: 87, corresponding to Protein ID Number YP 003358851.1; (i) ORF 62, encoding the amino acid sequence of SEQ ID NO: 88, corresponding to Protein ID Number YP 003358852.1; (j) ORF 63, encoding the amino acid sequence of SEQ ID NO: 89, corresponding to Protein ID Number YP 003358853.1; (k) ORF 64, encoding the amino acid sequence of SEQ ID NO: 90, corresponding to Protein ID Number YP 003358854.1; (l) ORF 65, encoding the amino acid sequence of SEQ ID NO: 91, corresponding to Protein ID Number YP 003358855.1;
[0182] (B) wherein the P CRO promoter between ORFs 36 and 37 has been replaced with an inducible promoter or a constitutive promoter; and
[0183] (C) comprising the following ORFs from bacteriophage ΦFL1C:
(a) ORF 40 encoding the amino acid sequence of SEQ ID NO: 158; (b) ORF 41 encoding the amino acid sequence of SEQ ID NO: 159; (c) ORF 42 encoding the amino acid sequence of SEQ ID NO: 160; (d) ORF 43 encoding the amino acid sequence of SEQ ID NO: 161; (e) ORF 44 encoding the amino acid sequence of SEQ ID NO: 162.
[0189] In some embodiments of the previous embodiment, for the following ORFs from bacteriophage ΦFL1C:
(a) ORF 40 has the nucleic acid sequence of SEQ ID NO: 163; (b) ORF 41 has the nucleic acid sequence of SEQ ID NO: 164; (c) ORF 42 has the nucleic acid sequence of SEQ ID NO: 165; (d) ORF 43 has the nucleic acid sequence of SEQ ID NO: 166; (e) ORF 44 has the nucleic acid sequence of SEQ ID NO: 167.
[0195] In further embodiments the bacteriophage comprises the genome of the bacteriophage ΦEfl1 from Genbank Accession Number GQ452243 corresponding to SEQ ID NO: 92:
[0000] (A) wherein nucleotides 39671-42813 and nucleotides 1-336 have been deleted and replaced by nucleotides 14600-17836 from bacteriophage ΦFL1C; and
(B) wherein the P CRO promoter between ORFs 36 and 37 of the genome of bacteriophage ΦEfl1 have been replaced with an inducible promoter or a constitutive promoter.
In further embodiments the bacteriophage is φEfl1 (vir) PnisA and is comprised by Enterococcus faecalis NRRL Deposit Number NRRL B-50833.
[0196] In further embodiments, the bacteriophage is a variant of the bacteriophage φEfl1(vir) PnisA comprised by Enterococcus faecalis NRRL Deposit Number NRRL B-50833, wherein the nisin promoter present in said deposited bacteriophage is replaced by a constitutive promoter, and wherein the erythromycin resistance gene present in said deposited bacteriophage is deleted.
[0197] In some embodiments the promoter is a constitutive promoter. In further embodiments the constitutive promoter is the Tu promoter having the nucleic acid sequence of SEQ ID NO: 168.
[0198] In some embodiments the inducible promoter is the nisin promoter.
[0199] Also provided is a bacteria comprising the bacteriophage of any one of the preceding bacteriophage embodiments. In some bacteria embodiments, the bacteria is a strain of Enterococcus faecalis.
[0200] Provided is a composition for prevention and treatment of Enterococcus faecalis or Enterococcus faecium infection comprising the bacteriophage of any one of the preceding embodiments, provided that the inducible promoter is not a promoter that utilizes a toxic inducer (e.g., the promoter is not the nisin promoter); and a pharmaceutically acceptable carrier.
[0201] Also provided is a method for prevention or treatment of Enterococcus faecalis or Enterococcus faecium infection comprising administering to a subject in need of such treatment or prevention the composition of the preceding embodiment. In some embodiments the composition is administered orally, optically, subcutaneously, peritoneally, intravenously, topically, intradentally or parenterally. In further embodiments the composition is administered to a root canal. In yet further embodiments the infection is resistant to at least one antibiotic. In yet further embodiments the infection is in an immunocompromised patient.
[0202] As envisioned in the present invention with respect to the disclosed compositions of matter and methods, in one aspect the embodiments of the invention comprise the components and/or steps disclosed herein. In another aspect, the embodiments of the invention consist essentially of the components and/or steps disclosed herein. In yet another aspect, the embodiments of the invention consist of the components and/or steps disclosed herein.
Abbreviations
[0203] AGE means agarose gel electrophoresis.
[0204] ORF means open reading frame.
DESCRIPTION OF THE FIGURES
[0205] FIG. 1 is a schematic representation of the construction of plasmid pΔ31-36PnisA, the vector used to delete ORFs 31-36, and replace P cro with P nisA in the φEfl1(Δ61-1, φFL1C40-44) prophage. The sequence comprising the two component nisin sensor system (nisR/nisK) is marked “A”. The fragment representing the nisin promoter (P nisA ) is marked “B”. The segment representing an erythromycin resistance marker (erm) is marked “C”. Fragments immediately upstream (pre31) and downstream (post 36) of the φEfl1 genomic region targeted for allelic exchange are marked “D”.
[0206] FIGS. 2A-2F show the results of a plaque assay of φEfl1 wild type (WT), spontaneous recombinant [(φEfl1(φ61-1, φFL1C40-44)], and virulent mutant [φEfl1(vir) PnisA ]: ( 2 A) WT after incubation for 1 day, ( 2 B) WT after incubation for 2 days, ( 2 C) spontaneous recombinant after incubation for 1 day, ( 2 D) spontaneous recombinant after incubation for 4 days, ( 2 E) virulent mutant after incubation for 1 day, ( 2 F) virulent mutant after incubation for 4 days.
[0207] FIGS. 3A-3B show the results of an agarose gel electrophoresis analysis of ethidium bromide-stained NdeI restriction fragments of φEfl1 and φEfl1(φ61-1, φFL1C 40-44) DNA. ( 3 A) Lanes 1 and 2: DNA molecular length standards (values on left are DNA lengths in kilobase pairs); 3: intact (undigested) φEFl1 DNA; 4: NdeI-digested φEfl1 DNA. ( 3 B) Lane 1: DNA molecular length standards (values on left are DNA lengths in kilobase pairs); 2: NdeI-digested φEfl1(φ61-1, φFL1C 40-44) DNA. Note that fragment 6, seen in gel containing Nde1 fragments of φEfl1 DNA, is missing in the gel containing the NdeI-digested φEfl1(φ61-1, φFL1C
[0208] FIG. 4 shows a Nde1 restriction site analysis of the φEfl1 DNA. The φEfl1 DNA is 42,822 in length and is oriented as described in Stevens et al., 2011. supra), with the genes arranged with ORF 1 at the extreme left end and ORF 65 at the extreme right end. Nde1 restriction sites (bp coordinates) are indicated the boxes. The Nde1 restriction fragments, as visualized in agarose gel electrophoresis analysis AGE, are labeled 1-12. The first Nde1 site is located 1.036 kbp from the left terminus of the DNA (coordinate 1036), and the Nde1 site is located 1.754 kbp from the right terminus of the DNA (coordinate 41,068). The combined length of these two fragments (2,7980 kbp) is equal to the size estimated from Nde1 fragment 6 observed in AGE analysis.
[0209] FIG. 5 presents an overview of the regions of φEfl1 (top) and φFL1C (bottom) that recombined to yield recombinant φEfl1(Δ61-1, φFL1C 40-44) (middle). Non-bolded line portions indicate φEfl1 sequences, bolded lines indicate φFL1C sequences.
[0210] FIG. 6 shows the PCR detection of φFL1C genes in E. faecalis JH2-2. Template DNA, lanes: 1-3: φEFl1(Δ61-1, φFL1C40-44); 4-6: E. faecalis JH2-2; 7-9: φEFl1 wildtype. Primers, lanes: 1, 4, 7: φFL1C gp40 internal primers (FL1A35F/FL1A35R); 2, 5, 8: φFL1C gp44 internal primers (FL1A37F/FL1A38R); 3, 6, 9: φEFl1 ORF44 internal primers (EF44F/EF44R); M: DNA marker.
[0211] FIG. 7 shows a one-step growth curve for phage φEfl1 (wild type), φEfl1(461-1, φFL1C40-44) (spontaneous recombinant), and φEfl1(vir)P nisA (virulent variant). Log phase broth cultures of E. faecalis JH2-2 were infected with a phage stock. After adsorption for 30 minutes, the cells were collected by centrifugation, washed, and incubated at 37° C. At various time points aliquots of the suspension were centrifuged to remove the cells, and the supernatants were plaque assayed for phage titer (pfu/ml) using JH2-2 indicator cells. (-- φEfl1 titer (pfu/ml); -▪- φEfl1(Δ61-1, φFL1C40-44) titer (pfu/ml); -▴- φEfl1 (vir)P nisA titer (pfu/ml).
[0212] FIG. 8 represents a φEFl1 (wild type) and φEFl1(vir) PnisA sequence comparison. The virulent mutant, φEFl1(vir) PnisA , genes ORF30-ORF36 as well as the cro promoter were allelically exchanged for the Nisin promoter cassette, and OR61-ORF1 were allelically exchanged with gp40-gp44 of φFL1C.
[0213] FIG. 9 shows a PCR analysis of the φEfl1(vir) PnisA genome demonstrating absence of φEfl1 ORFs 31 and 36, and the presence of nisR, P nisA , φFL1C ORFs gp40 and gp44. PCR products were separated by electrophoresis in 2% agarose gels and detected by ethidium bromide staining. Numbers to the left of the gel indicate DNA fragment size (kbp). Template DNA for PCR reactions: φEfl1(vir) PnisA (vir/lanes 1-4 and 7-8); φEFl1 (wt/lanes 5-6 and 9-10). Primers used in the PCR reactions (see FIG. 8 for primer binding sites): Primer set EF31UUF/RK5R spanning ORF 29 to nisR (lane 1), primers PNISaF/37DDR spanning P nisA to ORF 38 (lane 2); primers EF31MF/EF31MR within ORF 31 (lanes 3 and 5); primers EF36MF/EF36MR within ORF 36 (lanes 4 and 6); primers FL1A35F/FL1A35R within φFL1C ORF gp40 (lanes 7 and 9), primers FL1A37F/FL1A38R within φFL1C ORF gp44 (lanes 8 and 10). Lane M: molecular weight markers (BenchTop 1 kb ladder, Promega).
[0214] FIG. 10 shows the φEFl1 genome. The numbered arrows indicate ORFs. The ORF numbering scheme in FIG. 10 corresponds to the numbering system contained in Stevens et al., 2011, supra. ORFs 25-29 are involved in host cell lysis.
[0215] FIGS. 11A-11E show a nucleotide sequence alignment of phages φEfl1, φFL1C, and spontaneous recombinant phage [φEfl1(Δ61-1, φFL1C 40-44)] in the region of recombination (φEfl1 ORFs 60/61-1 and φFL1C ORFs 39/40-44). Non-bolded text indicates φEfl1 sequences, boldface text indicates φFL1C sequences. Spontaneous recombinant is abbreviated as Sp. Genomic coordinates are indicated to right of each row of sequence. Sites of sequence identity between φEFl1 and φEfl1(Δ61-1, φFL1C 40-44) are indicated by *****. The figures show φEfl1 sequence from 39307 to 41213 (SEQ ID NO: 171) (within ORF60) and from 1 through 451 (SEQ ID NO:172) (within ORF1), and φFL1C sequence from 14237 to 16206 (SEQ ID NO: 173) (within ORF39) and from 1672 to 17451 (SEQ ID NO: 174) (within ORF44). The segment of the φEfl1 sequence that has been replaced by the φFL1C sequence to form the φEfl1(Δ61-1, φFL1C 40-44) recombinant is indicated as enclosed by the hashed brackets. The figures shows the nucleotide sequence of the spontaneous recombinant phage [φEfl1(Δ61-1, φFL1C 40-44)] from 1772 to 3740 (SEQ ID NO: 175) and from 4527 to 5006 (SEQ ID NO: 176). NdeI restriction site in φEfl1 sequence is indicated.
DETAILED DESCRIPTION OF THE INVENTION
[0216] According to the present invention, engineered Enterococcus faecalis bacteriophages are provided that are virulent, highly lytic, incapable of lysogeny, insensitive to repressor, and capable of an extended host infectivity range. These characteristics make the recombinant phages useful as therapeutic agents in treatment and prevention of Enterococcus faecalis infections.
[0217] A recombinant bacteriophage, designated φEfl1 (vir) PnisA , has been derived from φEfl1. A lysogenic Enterococcus faecalis strain harboring phage φEfl1(vir) PnisA was deposited in the Agricultural Research Service Culture Collection (NRRL), National Center for Agricultural Utilization Research Agricultural Research Service, USDA, 1815 North University Street Peoria, Ill. 61604-3999 on Mar. 22, 2013 under accession number NRRL-50833. The wild type phage φEfl1 was deposited in the same depository on Mar. 22, 2013 under accession number NRRL-50832.
[0218] φEfl1 is a temperate bacteriophage that was induced from a lysogenic root canal isolate of Enterococcus faecalis (Stevens et al., Oral Microbiol. Immunol., 24: 278-284, 2009). Passage of φEfl1 in E. faecalis JH2-2 has yielded the recombinant variant, φEfl1(Δ61-1, φFL1C40-44), which provides elevated phage titers in broth cultures compared to the φEfl1 wild type. The recombinant bacteriophage also produces much larger, clearer zones of lysis in lawns of E. faecalis cells, than does the wild type φEfl1. Genetic analysis of the cloned virus producing the large plaques revealed that the variant was a recombinant between φEfl1 and a defective φFL1C-like prophage located in the E. faecalis JH2-2 chromosome. The recombinant possessed 5 ORFs of the defective φFL1C-like prophage in place of 6 ORFs of the φEfl1 genome. Deletion of ORFs 31-36 and replacement of the putative cro promoter from the recombinant phage genome with an exogenous regulatory element (inducible promoter) resulted in no loss of virus infectivity. Deletion of all lysogeny-related genes has resulted in a recombinant no longer having the capacity to form lysogens.
[0219] It was found that ORFs 31-36 are completely dispensable for lytic cycle function, since deletion of these genes did not prevent productive infection by the virus. Infection of lawns of host cells by the mutant virus lacking these genes produced clear plaques. Furthermore, surviving (presumptive lysogenic) cells from the plaques produced by the mutant virus lacking ORFs 31-36 could not be recovered. This confirms that deleting these genes from the viral genome, results in an φEfl1 mutant that is incapable of lysogeny.
[0220] Regulatory elements in the φEfl1 genome whose activation is required for the development of a productive/lytic infection within the cell, are inactivated by a protein (repressor) produced by ORF 36, one of the lysogeny-related genes. Lysogenic cells producing this repressor are thus immune to super infection by φEfl1, and would consequently survive exposure to this virus.
[0221] Accordingly, a stem-loop structure surrounded by P L and P R promoter sequences in the φEfl1 genome lying between a putative cI repressor gene and a putative cro gene was replaced with an exogenous regulatory element that is not susceptible to inactivation by the repressor. This P CRO region lies between ORFs 36 and 37. Specifically, the native promoter sequence was replaced with a nisin-inducible promoter, generating a virus that was capable of productively infecting E. faecalis (φEfl1) lysogens, in the presence of the φEfl1 cI repressor protein. Accordingly, replacement of the φEfl1 wild type regulatory element with an exogenous regulatory element that is not susceptible to inactivation by the repressor, as provided herein, allows the variant bacteriophage to productively infect and lyse lysogenic cells that harbor a previously integrated φEfl1 genome.
[0222] Surprisingly, spontaneous recombinational replacement of 5 genes (ORFs 61-65) of the DNA replication/modification module and 1 gene (ORF 1/terminase A) of the packaging module by 5 genes (ORFs 40-44) of E. faecalis phage φFL1C also had an effect on the virulence properties of the virus. While this genetic recombination had no effect upon host range, it did markedly alter the lytic properties observed during infection of either broth cultures or soft agar overlay lawns of susceptible host cells. Broth cultures rapidly and more thoroughly cleared, after infection by the recombinant phage φEfl1(Δ61-1, φFL1C40-44), as compared to infection by the wild type φEfl1 virus. Similarly, plaques produced by the recombinant phage φEfl1(Δ61-1, φFL1C40-44) appeared as large, extensively spreading lytic zones with a clearer center, compared to those formed by the wild type φEfl1 virus. Without wishing to be bound by any theory, the replacement (φFL1C) genes may contribute to a more robust, more productive lytic infection by increasing the efficiency of either phage DNA synthesis or packaging, or both. The results of one step growth experiments for wild type φEfl1 and recombinant φEfl1(Δ61-1, 95FL1C40-44) phages appear to bear out this hypothesis in that recombination of φEfl1 with the φFL1C genes results in a greatly (>100 fold) enhanced production of progeny virus.
[0223] The recombination that occurred resulted in the deletion of a portion of ORF 1 of φEfl1 corresponding to the nucleic acid sequence of SEQ ID NO: 169. The portion of ORF 1 of φEfl1 corresponding to the nucleic acid sequence of SEQ ID NO: 170 was retained in the spontaneous recombinant phage φEfl1 (Δ61-1, 95FL1C40-44). The region upstream of the recombined ORF 1 sequence is an intergenic sequence between ORFs 65 and ORF 1.
[0224] In addition, the source of the φFL1C genes (i.e., the E. faecalis JH2-2 chromosome) was unexpected, since previous studies reported that this E. faecalis strain was susceptible to φFL1C infection, and in fact, could form φFL1C lysogens following φFL1C infection, suggesting that this strain did not initially harbor a φFL1C prophage (Yasmin et al., J. Bacteria 192(4):1122-1130, 2010). PCR analysis failed to reveal other regions of the φFL1C genome that could be detected in JH2-2, suggesting that the φFL1C sequence that was detected was part of a defective (incomplete) prophage, or was the only φFL1C-like portion of a complete prophage.
[0225] A genetic construct incorporating all the afore-mentioned φEfl1 genomic modifications has resulted in the generation of a variant, designated φEfl1(vir) PnisA , that is incapable of lysogeny and insensitive to repressor, rendering it virulent and highly lytic, with a notably extended host-range in comparison with the wild type virus φEfl1. Compared to the wild type φEfl1, the recombinant virus produces a more robust infection of E. faecalis cells and a greater degree of lysis of the host E. faecalis cells.
[0226] The φEfl1(vir) PnisA virus has been constructed, in part, by replacing the repressor-sensitive cro promoter of the wild type φEfl1 virus with the repressor-insensitive, nisin-inducible promoter system to drive phage lytic infection functions. This replacement has proved to be a very effective and useful strategy in making genetic modifications in the virus, and allows the φEfl1(vir) PnisA virus to function as a useful intermediate in the preparation of derivative virus containing the desirable features discussed above. It may be appreciated, however, that to provide a therapeutic phage for managing Enterococcal infections would require replacement of the nisin-inducible promoter system of φEfl1(vir) PnisA with an alternative inducible promoter responsive to a non-toxic inducer, or with a constitutive promoter.
[0227] One such promoter is the following constitutive promoter Tu derived from an E. faecalis strain:
[0000]
(SEQ ID NO: 168)
TCTAGATITTTCCTTGAGAATAAAAGGTTTGTTTTTAGAACTATCCTTT
TTTCAAGATTTCGTGTAAAATAGCTTATGATGATCAGACGATTTTTAGT
AACGTCTATCACATATAAAACAAACAATAAAATTTATATTTTTAGGAGG
AACATTCAAA
[0228] φEfl1(vir) PnisA was engineered to include the property of antibiotic (erythromycin) resistance in order to assist in the selection of transformant lysogen clones containing prophages with the desired genotype. The skilled artisan would recognize that this feature would be omitted from a therapeutic phage, without prejudice to the desirable characteristics discussed above.
[0229] The bacteriophages of the present invention have been exemplified by preparation of φEfl1 (vir) PnisA Further variants may be prepared by utilizing φEfl1 as a template and carrying out the following genetic modifications as described in detail in the Example: (i) deletion of lysogeny ORFs 31-36; (i) replacement of the repressor-sensitive cro promoter of the wild type φEfl1 virus with a repressor-insensitive inducible promoter system or constitutive promoter system to drive phage lytic infection functions; (iii) replacement of 5 genes (ORFs 61-65) of the wild type DNA replication/modification module and 1 gene (ORF 1/terminase A) of the wild type packaging module by five genes (ORFs 40-44) of E. faecalis phage 95FL1C. Utilization of the nisin-inducible promoter system as described in the Example, and provision for erythromycin resistance results in the φEfl1(vir) PnisA phage, may be omitted.
[0230] Alternatively, variants of phage φEfl1 (vir) PnisA may be prepared by utilizing φEfl1(vir) PnisA phage as a starting material, and optionally removing the erythromycin resistance gene and optionally substituting the nisin-inducible promoter system of φEfl1(vir) PnisA with either an inducible promoter system that does not rely on a toxic inducer, or with a constitutive promoter system, e.g., the constitutive Tu promoter of SEQ ID NO: 168.
Indications
[0231] The bacteriophages used in the methods and compositions of the present invention may be used to prevent and treat Enterococcus faecalis and Enterococcus faecium infections. Non-limiting sites of infection include, for example, the urinary tract, bloodstream, abdomen, biliary tract, burn wounds, indwelling catheters, infected root canals and the heart (e.g. endocardium).
[0232] The bacteriophages used in the methods and compositions of the present invention may be used to prevent and treat antibiotic-resistant Enterococcus faecalis and Enterococcus faecium infections, as well as infections that may be antibiotic-sensitive, to augment the antibiotic treatment regimen. The bacteriophages may also be used to treat immunocompromised patients and patients suffering from opportunistic hospital infections. Especially advantageous indications for the present invention may be as a treatment for root canal infections, infectious endocarditis, nosocomial infections, burn infections, urinary tract infections, meningitis and surgical wound infections.
Administration
[0233] The bacteriophages used in the methods and compositions of the present invention may be administered by any route, including orally, optically, subcutaneously, peritoneally, intravenously, topically, intradentally or parenterally. Also contemplated within the scope of the invention is the instillation of bacteriophage in the body of the patient in a controlled formulation, with systemic or local release of the drug to occur at a later time. For example, the bacteriophage may be localized in a depot for controlled release to the circulation, or for release to a local site of Enterococcus infection.
[0234] The bacteriophage may be placed on or imbedded within a wound dressing, e.g., a surgical wound dressing, to treat or prevent Enterococcus infection of the wound. The bacteriophage may be applied to the wound in this fashion alone or in combination with other antibacterial agents that do not interfere with antibacterial action of the bacteriophage. For example, the bacteriophage may be contained in a composition impregnated in a wound dressing, e.g. a cotton wool dressing, for topical administration to a wound site.
[0235] The specific dose of bacteriophage to obtain therapeutic benefit for treatment of an Enterococcus infection will, of course, be determined by the particular circumstances of the individual patient including, the size, weight, age and sex of the patient, the stage of the disease, the aggressiveness of the disease, and the route of administration of the bacteriophage.
[0236] The daily dose of the bacteriophage may be given in a single dose, or may be divided, for example into two, three, or four doses, equal or unequal, but preferably equal, that comprise the daily dose. When given intravenously, such doses may be given as a bolus dose injected over, for example, about 1 to about 4 hours.
[0237] The bacteriophages used in the methods of the present invention may be administered in the form of a pharmaceutical composition, in combination with a pharmaceutically acceptable carrier. The active ingredient in such formulations may comprise from 0.1 to 99.99 weight percent. By “pharmaceutically acceptable carrier” is meant any carrier, diluent or excipient which is compatible with the other ingredients of the formulation and not deleterious to the recipient.
[0238] The bacteriophage is preferably administered with a pharmaceutically acceptable carrier selected on the basis of the selected route of administration and standard pharmaceutical practice. The active agent may be formulated into dosage forms according to standard practices in the field of pharmaceutical preparations. See Alphonso Gennaro, ed., Remington's Pharmaceutical Sciences, 18th Ed., (1990) Mack Publishing Co., Easton, Pa. Suitable dosage forms may comprise, for example, tablets, capsules, solutions, parenteral solutions, troches, suppositories, or suspensions.
[0239] The compositions of the present invention can include pharmaceutically acceptable carriers such as lactose, dextrose, sucrose, sorbitol, mannitol, starch, acacia rubber, calcium phosphate, alginate, gelatin, calcium silicate, micro-crystalline cellulose, polyvinyl pyrrolidone, cellulose, water, syrup, methyl cellulose, methylhydroxybenzoate, propylhydroxybenzoate, talc, magnesium stearate and mineral oil, but not always limited thereto. The composition of the present invention can additionally include lubricants, wetting agents, sweetening agents, flavors, emulsifiers, suspensions and preservatives.
[0240] The composition of the present invention contains bacteriophage as an active ingredient. The bacteriophage may be included at the concentration of 1×10 1 pfu/ml-1×10 15 pfu/ml or 1×10 1 pfu/g-1×10 15 pfu/g, and more preferably at the concentration of 1×10 4 pfu/ml-1×10 9 pfu/ml or 1×10 4 pfu/g-1×10 9 pfu/g. Other concentrations may be envisioned by the skilled artisan.
[0241] For parenteral administration, the bacteriophage may be mixed with a suitable carrier or diluent such as water, an oil (particularly a vegetable oil), ethanol, saline solution, aqueous dextrose (glucose) and related sugar solutions, glycerol, or a glycol such as propylene glycol or polyethylene glycol. Solutions for parenteral administration preferably contain a water soluble salt of the active agent. Stabilizing agents, antioxidant agents and preservatives may also be added. Suitable antioxidant agents include sulfite, ascorbic acid, citric acid and its salts, and sodium EDTA. Preservatives may be included, but must be selected so as not to inactivate or otherwise impact the bacteriophage. The composition for parenteral administration may take the form of an aqueous or nonaqueous solution, dispersion, suspension or emulsion.
[0242] For oral administration, the bacteriophage may be combined with one or more solid inactive ingredients for the preparation of tablets, capsules, pills, powders, granules or other suitable oral dosage forms. For example, the bacteriophage may be combined with at least one excipient such as fillers, binders, humectants, disintegrating agents, solution retarders, absorption accelerators, wetting agents absorbents or lubricating agents. According to one tablet embodiment, the bacteriophage may be combined with carboxymethylcellulose calcium, magnesium stearate, mannitol and starch, and then formed into tablets by conventional tableting methods.
[0243] The pharmaceutical composition is preferably in unit dosage form. In such form the preparation is divided into unit doses containing appropriate quantities of the active component. The unit dosage form can be a packaged preparation, the package containing discrete quantities of preparation, such as packeted tablets, capsules, and powders in vials or ampoules. Also, the unit dosage form can be a capsule, tablet, cachet, or lozenge itself, or it can be the appropriate number of any of these in packaged form.
[0244] The pharmaceutical compositions of the present invention may be used for the prevention and treatment of Enterococcus faecalis and Enterococcus faecium infections.
[0245] The practice of the invention is illustrated by the following non-limiting example.
Example
A. Materials and Methods
[0246] 1. Bacterial Strains and Growth Conditions
[0247] TUSoD11 is a lysogenic E. faecalis strain, harboring a φEfl1 prophage, which was previously isolated from an infected root canal (Stevens et al., Oral Microbiol. Immunol., 24:278-284 (2009). Following curing, the non-lysogenic variant of this strain was designated E. faecalis TUSoD11 (ΔφEfl1).
[0248] JH2-2 is a Fus r , Rif r mutant of a clinical E. faecalis isolate (Jacob & Hobbs, J. Bacteriol. 117(2):360-372, 1974) that was generously provided to us by Dr. Nathan Shankar. In the course of this study, it was found that this strain harbored a φFL1C-type prophage element (Yasmin et al., J. Bacteriol. 192(4):1122-1130, 2010), indicating that this strain was a lysogen with a defective prophage. Other E. faecalis strains used in this study are listed in Table 1.
[0249] All strains were grown in brain heart infusion (BHI) broth (or on brain heart infusion agar, with appropriate antibiotics). Escherichia coli one shot mach-T1® (Invitrogen) was used in cloning plasmids as describe below. The cells were grown in LB medium supplemented with the appropriate antibiotics. Additional bacterial species used as negative controls in PCR experiments are also listed in Table 1.
[0000]
TABLE 1
Bacterial strains
E . faecalis strain
Characteristics
Source
TUSoD11
Lysogenic root canal isolate harboring
1
φEfll prophage
JH2-2
Rif r , Fus r , clinical isolate harboring
2, 3
defective φFL1C prophage
OG1RF
Rif r , Fus r
3,4
MMH594
Gen r
3
OG1SSp
Str r , Spc r
5
ER3/2s, ER5/1
root canal isolates
6, 7
E1, E2, E3, E4, E5, E6, E7, E8, E10, E11
oral isolates
6, 8
GS1, GS2, GS3, GS4, GS5, GS6, GS7, GS8,
root canal isolates
9
GS9, GS10, GS12, GS13, GS14, GS15, GS16,
GS17, GS18, GS19, GS21, GS22, GS23, GS24,
GS25, GS26, GS27, GS28, GS29, GS30, GS31,
GS32, GS33
GS34
tongue
6, 7
OS25
oral isolate
6, 10
AA-OR3, AA-OR4, AA-OR26, AA-OR34
oral isolates
6, 11
AA-T4, AA-T26
tongue
6, 11
V583
Van r , clinical isolate
6, 12
OS16
oral isolate
6, 10
TUSoD1, TUSoD2, TUSoD3
Lysogenic root canal isolate
1
TUSoD9, TUSoD10, TUSoD12
root canal isolates
1
TUSoD15, TUSoD17, TUSoD18
Non-Enterococcal spp:
Streptococcus mutans 10449
grown in BHI broth
ATCC
Streptococcus sanguis 43055
grown in BHI broth
ATCC
Fingoldia ( Peptostreptococcus )
grown in chopped meat broth
ATCC
magna ( magnus )
Clostridium perfringens 13124
grown in modified PY broth
ATCC
Actinomyces israelii 10049
grown in BHI broth
ATCC
Eubacterium lentum 43033
grown in chopped meat broth
ATCC
1 Stevens et al., Oral Microbiol . Immunol ., 24: 278-284 (2009);
2 Jacobs and Hobbs, J . Bacteriol . 117(2): 360-372 (1974);
3 Dr. Nathan Shankar;
4 Dunny et al, Plasmid , 2: 454-465 (1979);
5 Dunny, Plasmid , 2: 454-465 (1979);
6 Dr. Christine Sedgley;
7 Johnson et al., J . Endod 32: 946-950 (2006);
8 Sedgley et al., Oral Microbiol Immunol . 19: 95-102(2004);
9 Sedgely et al., Oral Microbiol Immunol 20: 10-19 (2005a);
10 Sedgley et al., Archs oral Biol . 50(8): 575-583 (2005);
11 Sedgley et al., J . Endod 32(2): 104-111 (2006);
12 Sahm et al., Antimicrob Agents Chemother 33: 1588-1591 (1989).
[0250] 2. Construction of Recombinant Plasmids
[0251] The allelic exchange plasmid pΔ31-36 P nisA was prepared as follows.
[0252] The Nisin promoter (P nisA ) cassette containing an erythromycin selection marker (erm) was PCR-amplified using the AccuPrime DNA Taq Polymerase High Fidelity kit (Invitrogen) with primer set PNISaF/PNISR (see Table 2 for primer specifications) from plasmid pMSP3535 (Bryan et al. Plasmid, 44:183-190, 2000), a kind gift from Dr. B. Buttaro. PCRs were performed in 30 μl reaction mixtures containing 2 μl template DNA, 2 μl (20 pmol) forward primer, 2 μl (20 pmol) reverse primer, 21.5 μl dH 2 0, 2 μl buffer (provided by manufacturer), and 0.5 μl AccuPrime DNA Taq Polymerase. The PCR program used was: 95° C. for 2 min, followed by 35 cycles of (i) 95° C. for 45 sec, (ii) 55° C. for 45 sec, and (iii) 72° C. for 2 min. This was followed by an additional 5 min extension at 72° C. Following PCR, the amplicons were detected by agarose gel electrophoresis and ethidium bromide staining.
[0253] The allelic exchange plasmid pΔ31-36 P nisA was then constructed as follows, as shown in FIG. 1 . The amplicons generated by the above procedure were cloned into pCR8/GW/TOPO vector (Life Technologies) to create pErm-PnisA. The two-component Nisin sensor system (nisR/nisK) that controls the activation of P nisA by Nisin, was also amplified from pMSP3535 by PCR, using primer set RKnpF/RKaxR, and cloned into pCR8/GW/TOPO to create pRK. The P nisA fragment plus the erythromycin selection marker was digested from pErm-PnisA with AatII and SphI, and inserted into pRK to create pRK-Erm-PnisA. A fragment (pre31) of 1088 bp from nucleotide coordinates 24585 to 25672 of φEfl1 (upstream of ORF31, the first gene of the putative lysogeny module) and a fragment (post36) of 1090 bp from 28588 to 29577 of φEfl1 (immediately upstream of the putative cro gene, ORF37) were PCR-amplified using primer sets EF31UF/EF31UR and EF37DF/EF37DR, respectively, and cloned into pCR8/GW/TOPO to create pPre31 and pPost36. The post36 fragment was cut out from the pPost 36 with BamHI and SphI and inserted into pRK-Erm-PnisA, to create pPost36-RK-PnisA. The pPre31 was first digested with EcoRI and blunt-ended with the Klenow fragment of DNA polymerase I (Promega), then digested with PstI. Following this, the digested pre31 fragment was cloned into pPost36-RK-PnisA to create the allelic exchange plasmid pΔ31-36 P nisA .
[0254] 3. Isolation of Spontaneous Phage φEfl1/φFL1C-Like Recombinant [φEfl1(φ61-1, φFL1C40-44)] and the Creation of a Lysogen Harboring the Recombinant Prophage.
[0255] A log phase BHI broth culture of E. faecalis JH2-2 was inoculated with phage φEfl1. After incubation at 37° C. for 1 hr, the culture was centrifuged (17,000×g for 3 min) and the supernatant was filtered (0.45 μm) before being plaque-assayed. After overnight incubation at 37° C., the plates were examined, and several large, extensively-spreading plaques were noticed among a background of small, turbid plaques. These large plaques were picked, and the virus in these large plaques was cloned by successive plaque purifications. The genomic DNA from the cloned virus was sequenced by Sanger di-deoxy sequencing reactions as described previously (Stevens et al., FEMS Microbiol. Lett., 317: 9-26, 2011).
[0256] To create a lysogen harboring a φEfl1(Δ61-1, φFL1C40-44) prophage, JH2-2 cells from surviving colonies in the center of the large plaques produced by this virus were cloned and screened for the presence of the recombinant phage genome. This was done by PCR using primers (EF60F/FL1A35R) that recognized φEfl1 ORF 60 at the 5′ end and φFL1C ORF 40 at the 3′ end (see Table 2 for primer specifications). The lysogen harboring this recombinant prophage was designated E. faecalis JH2-2[φEfl1(Δ61-1, φFL1C40-44)]. In addition, virus spontaneously released from this lysogen was detected by plaque assay, and also confirmed to be recombinant by PCR analysis.
[0000]
TABLE 2
Primers
Primer
Sequence (5′→3′)
Use
EF31UF
GATAGTTCTTGTTTCGACAAATCAC
Amplify upstream
(SEQ ID NO: 1)
of φEf11 Orf31
EF31UR
CTGTCGACGTTCCTGCAGAGCTCTAAATAAATATGG
Amplify upstream
CAAGTA (SEQ ID NO: 2)
of φEf11 Orf31
EF37DF
CTGGATCCATGTGCTATGATTACTCAAAATTAGCAG
Amplify downstream of
(SEQ ID NO: 3)
φEf11 Orf36
EF37DR
CTGCATGCCCTTTACCAGTAATTTTCGGCGT
Amplify downstream of
(SEQ ID NO: 4)
φEf11 Orf36
RKnpF
CTCCATGGTCTCTCCTGCAGATAGAATTCTCATGTTT
Amplify nisR and nisK
GACAGCTTATCA (SEQ ID NO: 5)
RKaxR
CTGCATGCTCTCTCGACGTCGCCAGTTAATAGTTTGC
Amplify nisR and nisK
CGAA (SEQ ID NO: 6)
PNISaF
CTGACGTCACAAAAGCGACTCATAGAATTATTTCCTC
Amplify Erm-P nisA
C (SEQ ID NO: 7)
PNISR
GCTTATCGAAATTAATACGACTCACTATAGG
Amplify Erm- PnisA
(SEQ ID NO: 8)
EF31UUF
AAGAGCACCTCAAATTCCAGT (SEQ ID NO: 9)
Detection of φEf11
ΔOrf31-36 (upstream)
RK5R
TGATAAGCTGTCAAACATGAGAATTCT
Detection of φEf11
(SEQ ID NO: 10)
ΔOrf31-36 (upstream)
37DDR
TGTGATTTGCATGTAGACATCTCCT
Detection of φEf11
(SEQ ID NO: 11)
ΔOr131-36 (downstream)
PNIS3F
TTGTAAAACAGGAGACTCTGCATG
Detection of φEf11
(SEQ ID NO: 12)
ΔOrf31-36 (downstream)
EF31MF
AAGTTGTTTCCGTGTCAACGTGGC
Detection of φEf11 Orf31
(SEQ ID NO: 13)
deletion
EF31MR
GTGTCCATCATGGTCGTTTAGCAG
Detection of φEf11 Orf31
(SEQ ID NO: 14)
deletion
EF36MF
TTATCAGGGTCTGGTGAATGCG
Detection of φEf11 Orf36
(SEQ ID NO: 15)
deletion
EF36MR
GCAACTTATGAGTGAGCGCAA
Detection of φEf11 Orf36
(SEQ ID NO: 16)
deletion
φEF11F
GAGAGTGGAAGTGGA TTCAATG (SEQ ID NO: 17)
Detection of φEf11 Orf43
φEf11R
GCACTTTCATCTAAACTCTCG (SEQ ID NO: 18)
Detection of φEf11 Orf43
EF44F
ACCAAGATTTGACGCAGAAGTTGCC (SEQ ID NO: 19)
Detection of φEf11 Orf44
EF44R
TGGCCATCGTCGTCTTTATCTGCT (SEQ ID NO: 20)
Detection of φEf11 Orf44
EF60F
AGACGTTTGGACCGAATAGCTGGT (SEQ ID NO: 21)
Detection of φEf11 Orf60
EF60R
TGCGGTAAGCTTCTGCGAATTCAA (SEQ ID NO: 22)
Detection of φEf11 Orf60
Fl1A35F
GGGAACTAGCAGTTGAAGAATCGC (SEQ ID NO: 23)
Detection of φFL1C gp40
Fl1A35R
TTCCTTTGTACTATCTTGATCTCCA (SEQ ID NO: 24)
Detection of φFL1C gp40
Fl1A37F
GAGCGTTTAGATAAGTCGGATTGG (SEQ ID NO: 25)
Detection of φFL1C gp44
Fl1A38R
CCAAGTTTCTTTAGCCTGGTCACG (SEQ ID NO: 26)
Detection of φFL1C gp44
[0257] 4. Deletion of the Lysogeny Module and Replacement of Cro Promoter with P nisA by Allelic Exchange
[0258] Cells of E. faecalis lysogen JH2-2[φEfl1(Δ61-1, 4FL1C40-44)] were made competent using the procedures described by Shepard & Gilmore, Methods Mol Biol. 47:217-226 (1995). Briefly, the cells were grown in SGM17 medium (37.25 g/L M17, 0.5M sucrose and 8% glycine) for 48 hours at 37° C. The cells were then harvested by centrifugation, washed twice with EB buffer (0.5M sucrose and 10% glycerol), and finally resuspended in EB buffer. Plasmid pΔ31-36 P nisA was linearized with XhoI and then electroporated into the competent JH2-2 lysogens using the BioRad MicroPulser System. Following electroporation, 1 ml of SGM17MC medium (SGM17 plus 10 mM MgCl 2 and 10 mM CaCl 2 ) was added to the electroporation cuvette, which was then incubated for 2 hours. Transformants were selected on BHI agar containing erythromycin (30 μg/ml). Presumptive transformant colonies were screened for deletion of the lysogeny module genes (φEfl1 ORFs 31-36) and replacement of P cro by P nisA by PCR using primers EF31UUF/RK5R, PNIS3F/37DDR, EF31MF/EF31MR and EF36MF/EF36MR. In addition, control of lytic functions in the prophage by the P nisA was demonstrated by measuring phage induction in the presence or absence of Nisin (40 ng/ml). The phage recovered from the induced lysogens lacking ORFs 31-36 and P cro , but containing the P nisA promoter, was designated φEfl1 (vir) PnisA .
[0259] 5. Screening for the Presence of φEFl1 Prophages in E. faecalis Strains
[0260] Primers specific to φEfl1 were designed from φEfl1 ORF 43 (GenBank accession number GQ452243.1, Gene ID number 8683894). This sequence (ORF 43) of the φEfl1 genome was chosen since searches of all available data bases failed to disclose any homologous sequences to this gene. The forward (φEfl1F) and reverse (φEfl1R) primers for amplification of a 165 bp amplicon of this gene are specified in Table 2, above. Template DNA was prepared as follows: 10 ml broth cultures of each strain to be screened were pelleted by centrifugation, washed in 4 ml of wash solution [20 mM Tris-HCl (pH 8.5), 0.85% NaCl], resuspended in 2 ml of lysis buffer [1% Triton X-100, 20 mM Tris-HCl (pH 8.5), 2 mM EDTA], and heated to 95°-100° C. for 10 min. The suspension was then centrifuged and the supernatants were collected and frozen away at −80° C. until being used in PCR assays (Goncharoff et al., 1993, Oral Microbiol Immunol 8:105-110). Extracts from E. faecalis TUSoD11 (lysogenic for φEfl1) were used as positive controls, and extracts from E. faecalis JH2-2 (non-lysogenic for φEfl1) and numerous unrelated species (see Table 1) were used as negative controls. Reaction mixtures (Σ=40 μl) for PCR contained 5 μl of template DNA, 5 μl (50 pmol) of forward primer, 5 μl (50 pmol) of reverse primer, 5 μl dH 2 O, and 20 μl 2× Go Taq green PCR master mix (Promega). The PCR program used was 97° C. for 1 min, followed by 26 cycles of (i) 97° C. for 1 min, (ii) 50° C. for 45 sec, and (iii) 72° C. for 1 min. This was followed by an additional 4 min at 72° C. Following PCR, amplification products were detected by agarose (2%) gel electrophoresis and ethidium bromide staining.
[0261] 6. Preparation of Cured E. faecalis TUSoD11
[0262] Cells of E. faecalis TUSoD11 were made competent for electroporation as described above. After electroporation with the allelic exchange vector pΔ31-36 PnisA, erythromycin-resistant colonies were screened for homologous recombination-mediated deletion of the lysogeny module genes (ORFs 31-36) in the genome of E. faecalis TUSoD11. Strains exhibiting deletion of ORFs 31-36 were further tested by PCR for the presence of φEfl1 genes outside of the lysogeny module. In addition to clones containing φEfl1 genes other than ORFs 31-36, a few rare clones were identified that lacked any of the φEfl1 genes. Such clones could not be induced, but could now be infected by phage φEfl1. These cured clones were designated E. faecalis TUSoD11(4 φEfl1).
[0263] 7. Testing Adsorption of φEfl1 and φEfl1(Δ61-1, 4FL1C40-44) to Lysogenic and Non-Lysogenic E. faecalis Strains
[0264] E. faecalis strains JH2-2, TUSoD11 and the cured strain, TUSoD11 (ΔφEfl1) were grown in BHI medium to log phase. 100 μl of φEfl1 or φEfl1(Δ61-1, φFL1C40-44) preparations were added to 1 ml E. faecalis strains. After incubation at 37° C. for 10 minutes the mixtures were centrifuged at 17,000 g for 3 minutes, the supernatants were filtered through 0.45 μm filters, and filtrates containing any unabsorbed phage, were plaque-assayed, using JH2-2 indicator cells, to determine residual phage titers.
[0265] 8. One Step Growth Curve
[0266] The cells of a log phase BHI broth culture (2 ml) of E. faecalis JH2-2 were collected by centrifugation, resuspended in 1 ml of BHI broth, and inoculated with 100 μl of a stock culture of either phage φEfl1, φEfl1(Δ61-1, φFL1C40-44) or φEfl1(vir) PnisA . After incubation for 30 minutes to allow phage adsorption, the cells were recovered by centrifugation, washed 3 times in BHI broth, and finally resuspended in 10 ml of BHI broth. Aliquots (500 μl) of the suspension were made, and each was incubated at 37° C. At various time points, an aliquot was centrifuged to remove the cells, and the supernatant was plaque-assayed, using fresh JH2-2 indicator cells, for phage titer.
[0267] 9. Host range determination for φEfl1, φEfl1(Δ61-1, φFL1C40-44), and φEfl1(Vir) PnisA .
[0268] Plaque assays and spot tests were conducted with wild type phage φEfl1 and recombinant phages φEfl1(Δ61-1, φFL1C40-44) and φEfl1(vir) PnisA using a panel of 66 E. faecalis strains as indicators. The E. faecalis panel included both lysogenic and non-lysogenic strains. Lytic infection by each phage was detected by plaque assay with each E. faecalis indicator strain.
B. Results and Discussion
[0269] 1. Isolation of Spontaneous φEfl1/φFL1C Recombinant
[0270] Repeated propagation and plaque assay of phage φEfl1 on host strain E. faecalis JH2-2, revealed that variants of the wild type virus were being generated. Whereas wild type φEfl1 produced small, turbid plaques in lawns of JH2-2 ( FIG. 2A ), approximately 0.02% of the plaques appeared as large, extensively spreading, somewhat clearer zones of lysis. Interestingly, incubation of plaque assays of clones obtained by plaque purification of the virus producing these larger plaques resulted in continued expansion of the plaques to the extent that virtually the entire JH2-2 lawn was lysed ( FIGS. 2C-2D ). In contrast, wild type plaques typically disappeared after extended incubation, presumably due to growth of surviving lysogens within the plaques ( FIG. 2B ).
[0271] AGE analysis of the NdeI restriction fragments of the DNA from the virus producing these large plaques revealed that it was missing one of the fragments (fragment 6, 2.79 kbp) that was present in the NdeI DNA digestion of the original φEfl1 isolate ( FIG. 3B ). In addition, it was also noticed that another one of the NdeI fragments (fragment 2, approx. 9.4 kbp) from the DNA of the virus producing the large plaques, had increased in size (compared to the NdeI fragment 2 from the original φEfl1 DNA) ( FIG. 3A ) by an amount approximately equal to the size of the missing NdeI fragment 6 ( FIG. 3B ).
[0272] FIG. 4 shows the NdeI restriction site analysis of the φEfl1 DNA. The φEfl1 DNA is 42,822 in length and is oriented as described in Stevens et al., FEMS Microbiol. Lett., 317: 9-26 (2011), with the genes arranged with ORF 1 at the extreme left end and ORF 65 at the extreme right end. NdeI restriction sites (bp coordinates) are indicated the boxes. The NdeI restriction fragments, as visualized in agarose gel electrophoresis analysis AGE, are labeled 1-12.
[0273] Inspection of the φEfl1 NdeI restriction map ( FIG. 4 ) and the φEfl1 NdeI restriction digest summary (Table 3), revealed that NdeI fragment 6 was composed of the two extreme ends of the genome (fragment coordinates 0-1,036 plus 41,068-42,822), and that in a circularly permuted genome, this fragment is immediately adjacent to NdeI fragment 2 (coordinates 33,692-41,068) ( FIG. 4 ).
[0000]
TABLE 3
NdeI restriction digest summary for φEf11 genome
Fragment Number
(as seen in gel)
Fragment Length
Fragment Coordinates
1
12,126
9,349-21,475
2
7,376
33,692-41,068
3
5,029
26,948-31,977
4
4,660
22,288-26,948
5
4,247
3,065-7,312
6
2,790
0-1,036 + 41,068-42,822
7
2,037
7,312-9,349
8
1,818
1,248-3,065
9
1,715
31,977-33,682
10
547
21,741-22,288
11
266
21,475-21,741
12
212
1,036-1,248
[0274] FIGS. 5 and 11 A- 11 E show the nucleotide sequence alignment of phages φEfl1, φFL1C, and spontaneous recombinant phage [φEfl1(Δ61-1, φFL1C 40-44)] in the region of recombination (φEfl1 ORFs 60/61-1 and φFL1C ORFs 39/40-44). FIG. 5 presents an overview of the regions of φEfl1 and φFL1C that recombined to yield recombinant φEfl1(Δ61-1, φFL1C 40-44). FIGS. 11A-11E show φEfl1 sequence from 39307 (within ORF60) through 451 (within ORF1), and φFL1C sequence from 14236 (within ORF39) to 17451 (within ORF44). Non-bolded text indicates φEfl1 sequences, boldface text indicates φFL1C sequences. Spontaneous recombinant is abbreviated as Sp. Genomic coordinates are indicated to right of each row of sequence. Sites of sequence identity between φEfl1 and φEfl1(Δ61-1, φFL1C 40-44) are indicated by *****.
[0275] Sequencing this region of the genome thus disclosed that ORFs 60 through 65 and 1 of φEfl1 (coordinates 39671-42822 and 1-336), were replaced by ORFs 40 through 44 (coordinates 14600-17336) of E. faecalis phage φFL1C ( FIGS. 5 and 11 ). NdeI restriction site at coordinate 41,068 which divides NdeI fragment 2 from NdeI fragment 6 in the φEfl1 DNA is absent in the φFL1C DNA and consequently in the DNA of the recombinant virus ( FIGS. 11A-11E ). No other modifications of the genome were detected. Consequently, this φEfl1/φFL1C recombinant was designated phage φEfl1(Δ61-1, φFL1C40-44).
[0276] Since the JH2-2 genome was the only possible source of the φFL1C genes, E. faecalis JH2-2 was screened for the φFL1C prophage. φFL1C (ORFs 40-44)-specific primers (Table 2) were used in PCR with JH2-2 extracts, prepared as described previously. As seen in FIG. 6 , φFL1C-specific amplicons were generated from the JH2-2 templates and the φFL1C-specific primers, confirming the presence of (at least a portion of) a φFL1C prophage in the JH2-2 chromosome. PCR, using JH2-2 template DNA and primers specific for regions of the φFL1C genome other than ORFs 40-44, failed to produce any amplicons (data not shown).
[0277] 2. Deletion of the Lysogeny Module and Replacement of Cro Promoter in φEfl1(Δ61-1, φFL1C40-44) by Allelic Exchange
[0278] A one-step growth curve was generated as follows for phage φEfl1 (wild type), φEfl1(Δ61-1, φFL1C40-44) (spontaneous recombinant), and φEfl1(vir)P nisA (virulent variant). Log phase broth cultures of E. faecalis JH2-2 were infected with a phage stock. After adsorption for 30 minutes, the cells were collected by centrifugation, washed, and incubated at 37° C. At various time points aliquots of the suspension were centrifuged to remove the cells, and the supernatants were plaque assayed for phage titer using JH2-2 indicator cells. The results are shown in FIG. 7 (-- φEfl1 titer (pfu/ml); -▪- φEfl1 (Δ61-1, φFL1C40-44) titer; -▴- φEfl1 (vir)P nisA titer. The φEfl1(Δ61-1, φFL1C40-44) recombinant exhibited enhanced lytic activity (compared to wild type virus) as judged by the extensively enlarged plaques it forms in lawns of host cells ( FIG. 2C ), and the elevated titers it achieved in productive infection ( FIG. 7 ). These variants of phage φEfl1 could be subject to repression due to superinfection immunity, and be limited in lytic infection due to the possibility of entering into lysogeny, rather than generating a productive infection. Accordingly, all lysogeny-related genes were deleted and regulatory genetic elements were rendered insensitive to repressor control, as follows.
[0279] Clones of JH2-2[φEfl1(Δ61-1, φFL1C40-44)] transformed with plasmid pΔ31-36 PnisA, were selected on erythromycin-containing media. PCR analysis and sequencing of these erythromycin-resistant JH2-2[φEfl1(Δ31-36, ΔP CRO , P nisA , erm, nisR/K, Δ61-1, φFL1C40-44)] clones demonstrated that they lacked φEfl1 ORFs 31-36, and the φEfl1 cro promoter, but contained the nisin promoter (P nisA ) and nisR/nisK ( FIG. 8 and FIG. 9 ). In the analysis, PCR products were separated by electrophoresis in 2% agarose gels and detected by ethidium bromide staining. Numbers in FIG. 9 to the left of the gel indicate DNA fragment size (kbp). Template DNA for PCR reactions: φEfl1(vir) PnisA (vir/lanes 1-4 and 7-8); φEfl1 (wt/lanes 5-6 and 9-10). For the primers used in the PCR reactions, see FIG. 8 for primer binding sites: Primer set EF31UUF/RK5R spanning ORF 29 to nisR (lane 1), primers PNISaF/37DDR spanning P nisA to ORF 38 (lane 2); primers EF31MF/EF31MR within ORF 31 (lanes 3 and 5); primers EF36MF/EF36MR within ORF 36 (lanes 4 and 6); primers FL1A35F/FL1A35R within φFL1C ORF gp40 (lanes 7 and 9), primers FL1A37F/FL1A38R within φFL1C ORF gp44 (lanes 8 and 10). In FIG. 9 , lane M shows molecular weight markers (BenchTop 1 kb ladder, Promega).
[0280] Exposure of a population of this lysogenic clone, harboring a mutant prophage containing the nisin promoter (P nisA ) in place of the wild type cro promoter/operator (P CRO ), to nisin (40 ng/ml) resulted in the induction of phage, yielding a titer of 6.82×10 7 pfu/ml (±0.31×10 7 ). In the absence of nisin, a similar population of these lysogens spontaneously released phage, producing a titer of 5.57×10 5 pfu/ml (±0.31×10 5 ). In contrast, phage induction from lysogens [JH2-2{φEfl1(Δ61-1, φFL1C40-44)}] containing a prophage with the wild type cro promoter/operator did not appear to be affected by the presence of nisin: In the presence of nisin (40 ng/ml), these cells produced a phage titer of 3.36×10 5 pfu/ml (±0.25×10 5 ), whereas the same cells produced a titer of 3.31×10 5 pfu/ml (±0.38×10 5 ) in the absence of nisin. These data indicate that productive infection was now under control of the nisin-sensitive promoter (P nisA ), albeit somewhat leaky.
[0281] The virus obtained, phage [φEfl1(Δ31-36, ΔP CRO , P nisA , erm, nisR/KΔ61-1, φFL1C40-44)], by Nisin induction of the JH2-2[φEfl1(Δ31-36, ΔP CRO , P nisA , erm, nisR/KΔ61-1, φFL1C40-44)] lysogens produced large, clear plaques ( FIG. 2E-2F ), and was designated φEfl1 (vir) PnisA . As will be shown below, this derivative of temperate phage φEfl1 had all the characteristics of a virulent virus.
[0282] 3. Isolation of Cured E. faecalis TUSoD11
[0283] After electroporation of E. faecalis TUSoD11 with the gene exchange vector pΔ31-36 PnisA, erythromycin-resistant colonies were screened by PCR for deletion of ORF31-ORF36. Unexpectedly, a few colonies were found with deletions of not only the intended ORF31-ORF36 lysogeny module, but also all other phage genes outside this region. These clones may have been generated by the homologous recombination between the gene exchange vector and a permutated and terminally redundant prophage DNA that may have positioned the ORF30 and ORF37 regions at either end of the φEfl1 prophage within the host E. faecalis TUSoD11 chromosome. These E. faecalis clones, lacking any detectable φEfl1 genes, were designated TUSoD11(φEfl1), and were further tested for phage induction. No phage could be induced from these cells.
[0284] 4. Restoration of Adsorption of φEfl1 and φEfl1(Δ61-1, φFL1C40-44) by a Cured E. faecalis Strain
[0285] Phage suspensions were incubated with each of the E. faecalis strains indicated in Table 4 for 10 minutes, whereupon the cultures were centrifuged and filtered to remove the cells along with all adsorbed phage. The cell-free filtrates were then assayed for residual phage titer. The values shown in Table 4 represent the mean of triplicate assays ±standard deviation.
[0000]
TABLE 4
Phage adsorption by lysogenic and non-lysogenic E . faecalis strains.
Phage titer
Residual phage titer after adsorption with:
before
Lysogen
Non-lysogen
Non-lysogen
Phage
adsorption
TUSoD11
JH2-2
Cured TUSoD11
φEf11
1.2 × 10 5
1.17 × 10 5 ±
3.2 × 10 2 ±
2.74 × 10 2 ±
0.16 × 10 5
0.25 × 10 2
0.16 × 10 2
φEf11(Δ61-1, ΦFL1C40-44)
5.58 × 10 7
5.23 × 10 7 ± 0.2
4.79 × 10 2 ±
3.82 × 10 2 ±
3 × 10 7
0.23 × 10 2
0.17 × 10 2
[0286] As shown in Table 4, neither φEfl1 nor φEfl1(Δ61-1, φFL1C40-44) could produce a viable infection on the lysogenic TUSoD11 strain due to superinfection immunity. It was interesting that incubation of either φEfl1 or φEfl1 (Δ61-1, φFL1C40-44) with a cell suspension of lysogenic E. faecalis strain TUSoD11 failed to result in phage adsorption to the cells. In contrast, cell suspensions of either strain JH2-2 (non-lysogenic with respect to φEfl1) or TUSoD11(φEfl1), a cured E. faecalis strain, effectively adsorbed both virus strains.
[0287] 5. Host Range of φEfl1(Vir) PnisA
[0288] Plaque assays and spot tests were conducted with wild type phage φEfl1 and recombinant phages φEfl1(Δ61-1, φFL1C40-44) and φEfl1 (vir) PnisA using a panel of 66 E. faecalis strains as indicators. The E. faecalis panel included both lysogenic and non-lysogenic strains. Lytic infection by each phage was detected by plaque assay with each E. faecalis indicator strain. The results are shown in Table 5. It can be seen that whereas wild type φEfl1 productively infected only 4 (6%) of the 67 E. faecalis strains tested, productive infection occurred in 33 (49%) of these strains inoculated with phage φEfl1(vir) PnisA . The panel of E. faecalis strains was also screened by PCR for the presence of a prophage, using φEfl1-specific primers. Among the strains tested, 14 were found to be φEfl1 lysogens (data not shown). Of these 14 φEfl1 lysogens, none were susceptible to wild type φEfl1, however, 4 of these lysogenic strains (strains GS2, GS8, GS22 and GS25) could be productively infected by φEfl1(vir) PnisA . Furthermore, the presence of the φEfl1 repressor gene (cI/ORF-36) was confirmed in these φEfl1(vir) PnisA -susceptible lysogenic strains by PCR (data not shown).
[0000]
TABLE 5
Host range of E. faecalis phages
Phage
φEf11 (Δ61-1,
φEf11(Δ31-36,
φFL1C39-44
ΔP cro , P nisA , Δ611,
E. faecalis
φEf11
(spontaneous
φFL1C39-44)
strain
(wild type)
recombinant)
(virulent mutant)
OG1RF
−
−
−
ER3/2s
−
−
−
ER5/1
−
−
+
E1
+
+
+*
E2 #
−
−
−
E3 #
−
−
−
E4 #
−
−
−
E5 #
−
−
−
E6
−
−
−
E7 #
−
−
−
E8
−
−
+
E10
−
−
+
E11
−
−
+
GS1
−
−
−
GS2 #
−
−
+
GS3
−
−
+
GS4
−
−
−
GS5
−
−
−
GS6
−
−
+
GS7
−
−
+
GS8 #
−
−
+
GS9 #
−
−
−
GS10
−
−
−
GS12
−
−
−
GS13
−
−
+
GS14
−
−
+*
GS15
−
−
+
GS16
−
−
+
GS17
−
−
−
GS18
−
−
−
GS19
−
−
+
GS21
−
−
−
GS22 #
−
−
+
GS23#
−
−
−
GS24
−
−
+
GS25 #
−
−
+
GS26
−
−
+
GS27
−
−
+
GS28
−
−
−
GS29 #
−
−
−
GS30
−
−
+*
GS31
−
−
−
GS32
−
−
−
GS33 #
−
−
−
GS34
−
−
−
OS25
−
−
+
AA-OR3
−
−
+
AA-OR4
−
−
+
AA-OR26
−
−
+*
AA-OR34 #
−
−
−
AA-T4
−
−
+
AA-26
−
−
+*
V583
−
−
+
OS16
−
−
+
TUSoD1
+*
+*
+
TUSoD2
−
−
−
TUSoD3
−
−
−
TUSoD9
−
−
+
TUSoD10
−
−
−
TUSoD12
−
−
−
TUSoD15
−
−
−
TUSoD17
−
−
−
TUSoD18
+*
−
−
MMH594
−
−
−
OG1SSP
−
−
+
DG16
−
−
−
JH2-2
+
+
+
Cumulative
6.0%
4.5%
49.3%
+ = Sensitive to phage (plaque assay)
+* = Sensitive to phage (spot test)
− = Not sensitive to phage
# = Lysogenic E. faecalis strain containing Ef11 prophage
[0289] The disclosures of each and every patent, patent application, and publication cited herein are hereby incorporated herein by reference in their entirety. One skilled in the art will readily appreciate that the present invention is well adapted to carry out the objects and obtain the ends and advantages mentioned, as well as those inherent therein. While the invention has been disclosed with reference to specific embodiments, it is apparent that other embodiments and variations of this invention may be devised by others skilled in the art without departing from the true spirit and scope used in the practice of the invention. The appended claims are intended to be construed to include all such embodiments and equivalent variations. | Bacteriophages are provided that infect strains of Enterococcus faecalis , an opportunistic bacterial pathogen that causes human disease. Also provided are methods of treating Enterococcus faecalis by therapeutic administration of such bacteriophages. | 2 |
RELATED APPLICATIONS
This application is a continuation-in-part of U.S. patent application Ser. No. 07/785,862 filed on Oct. 28, 1991 (now abandoned), which was a continuation of U.S. patent application Ser. No. 07/501,617 filed Mar. 26, 1990 (now abandoned).
FIELD OF THE INVENTION
The present invention relates generally to communication systems and, more specifically, to a mobile telephone capable of both speech and data communication in a digital mobile telephone system.
BACKGROUND OF THE INVENTION
Mobile telephone use has evolved into a critical communication link for information flow. Originally, mobile telephones were capable of transmitting and receiving only speech signals. The proliferation of data transmission, such as facsimile and computer information, made it necessary for mobile telephones to be capable of both speech and data communication. This additional capability has been achieved primarily through the use of digital telephone network that are capable of converting analog speech signals to digital signals and combining them with the digital data signals. Examples of such digital telephone networks are the Pan-European digital mobile system Groupe Special Mobile (GSM) and a proposed U.S. system. The mobile digital telephone systems typically employ a type of time division multiplexing or "burst" communication where each burst contains several bits of digital information arranged according to a frame format defined in the standard for the system. Frames of information are divided into time slots, with each time slot being one or to more bits. The information conveyed in the time slots can be speech, data, or control signals.
The control signals determine whether a speech-only call or a speech and data call will be established between the mobile telephone and the mobile telephone system. In a speech-only call, the mobile telephone need only extract the appropriate time slot information designated as speech information according to the frame format. In a speech and data call, the mobile telephone must extract the appropriate signals from the speech time slots as well as from the data time slots. The received speech or speech and data information must then be stored in memory for processing by the mobile telephone. It is thus seen that a speech-only mobile telephone requires less memory than a speech and data telephone. A mobile telephone's memory is costly and consumes considerable power, thus, there is a need for mobile telephone circuit arrangements that provide speech or speech and data capabilities while at the same time reducing cost, power consumption, and complexity.
Because not all mobile telephone users require data capabilities, one possible solution to the above mentioned disadvantages is to offer two types of mobile telephones, a speech-only version and a speech and data version. In so doing, the speech-only version is not burdened with the added complexity, cost, and power consumption needed to provide data capabilities. The purchaser of a voice only mobile telephone who later desires to add data capabilities must discard his speech-only telephone and purchase a speech and data version, thereby wasting his initial capital investment.
SUMMARY OF THE INVENTION
The present invention eliminates these drawbacks.
The invention relates to a modular mobile telephone having two separate modules: a speech-only module, and a data-only adaptor module. A speech-only mobile telephone is achieved with the use of the speech-only module, which comprises a fully functional mobile telephone capable of transmitting and receiving signals to and from the mobile telephone system. A speech and data mobile telephone is achieved via the addition of a data module to the speech module. The data adaptor module provides all the added circuitry required for processing data signals. The radio telephone can be designed so that the data module can be purchased separately and added on to the speech-only telephone. The data module may be capable of processing both data signals received from the mobile telephone system and signals received directly from a data terminal.
In one embodiment, the adaptor has digital data encoding and multiplexing circuits as well as decoding and demultiplexing circuits. It also contains the additional memory necessary for digital operation. This memory may be substituted or used in combination with the speech-only memory. Further memory may be provided for connecting the data adaptor module directly to a data terminal.
BRIEF DESCRIPTION OF THE DRAWING
The invention is described below referring to FIG. 1. FIG. 1 is a block diagram of a mobile telephone according to the present invention. The figure illustrates the principal functional blocks. A person skilled in the art can realize the functional blocks with logic circuitry in a variety of ways without undue experimentation.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
The functional blocks of a mobile telephone include a transmitter/receiver (6) which receives "bursts" of information transmitted from the mobile telephone system, and transmits information from the mobile telephone to the mobile telephone system. Additionally, the transmitter modulates and demodulates the transmitted and received signals, respectively, according to the relevant modulation requirements for the mobile telephone standard being implemented. For example, if the standard being implemented were the Groupe Special Mobile (GSM) standard of the Pan-European digital mobile telephone system, the modulating technique employed would be Minimal Shift Keying (MSK). Other mobile telephone standards, such as that for the U.S. digital system, may also be used.
Further, in the transmit direction,the functional blocks of a mobile telephone include a speech encoder (1), a channel encoder (2), and a multiplexer (3). The speech encoder (1) converts input analog speech signals into digital bits and compresses the digital bits in order to remove redundant information and reduce the amount of information that is required to be transmitted. The speech encoder may be, for example, a pulse excited linear predictive coder with a long-term prediction. The channel encoder (2) generates error correction patterns that are added to the compressed digital bit stream output from the speech encoder (1). The multiplexer (3) arranges the compressed digital bits and the error correcting bits into appropriate time slot information, which is then transmitted by the transmitter/receiver (6) to the mobile telephone system in the appropriate speech time slots according to the frame structure defined in the relevant digital mobile telephone communication standard.
In the receive direction, the functional blocks of a mobile telephone include a demultiplexer/channel decoder (4) and a speech decoder (5). The demultiplexer/channel decoder (4) extracts the appropriate speech time slot information from the received information from the mobile telephone network, as well as stripping away the error correction bits and performing any necessary error correction. The speech decoder (5) expands the received compressed speech data and converts it into analog form for further audio processing.
The architecture of the mobile telephone is implemented with a microprocessor based central processing unit (CPU) (11) and a random access memory (RAM) (12). The CPU (11) controls the other functional blocks and stores information in the RAM (12). The size of the RAM (12) is determined mainly by the frame format and data structure of the particular digital mobile telephone standard being implemented. Additionally, a small amount of memory is required for the control and operation of the various functional blocks.
For example, if the standard being implemented were GSM, the RAM (12) would be sized based on the particular parameters of the GSM standard. In the GSM standard, each time slot contains 114 bits. For a speech-only call, there are 8 time slots of speech information and 4 time slots of control signal. Thus, each frame is (8+4)*114=1,368 bits. In addition, the mobile telephone must be capable of storing 4 frames of received information. Therefore, the required memory for the receive function is 1,368*4=5,472 bits. In the transmit direction, the transmitter need only be capable of storing 1 frame of information or 1,368 bits. Thus, the total memory required for the transmit/receive portion of a speech-only mobile telephone is (5,472+1,368)=6,840 bits. These figures will vary for other mobile telephone system standards.
In the case of a speech and data call, the time slots are still 114 bits. However, there are 8 time slots of speech information, 4 time slots of control signal, and 15 time slots of data information per frame. Since the receiver portion must be capable of storing 4 received frames, the required receive memory will be (8+4+15)*114*4=12,312 bits. In the transmit direction, the transmitter only needs to store 1 frame of information which is (8+4+15)*114=3,078 bits. Thus, the total memory required for the transmit/receive portion of a speech and data mobile telephone is (12,312+3,078)=15,390 bits.
The modular approach of the present invention results in a circuit arrangement for a speech-only mobile telephone that requires significantly less memory than a speech and data version. For example, under the GSM standard, a speech-only module requires less than half the memory of a speech and data module (6,840 versus 15,390).
In order to facilitate the use of a modular design, the speech-only module is provided with an interface (20), to which a data adaptor or auxiliary terminal (30) can be connected. This interface (20) may be a fast bus interface. The data adaptor (30) comprises substantially similar functional blocks to those found in the speech-only module. Specifically, the data adaptor (30) contains a channel encoder (2') and a multiplexer (3') similar to channel encoder (2) and multiplexer (3). Also, the data adaptor (30) contains a demultiplexer/channel decoder (4') similar to demultiplexer/channel decoder (4).
The data adaptor (30) communicates with the CPU (11 ) via the interface (20). In the GSM system, for example, the control signal received by the CPU indicates whether the received signal contains voice only or voice and data. The CPU (11 ) in accordance with the protocol being implemented will disassemble received frames and route speech information to the demultiplexer/channel decoder (4) and data information to the demultiplexer/channel decoder (4') in the data adaptor. Likewise, in assembling a frame to be transmitted the CPU (11) will route speech information from the multiplexer (3) and data information from multiplexer (3') to the transmitter portion of the transmitter/receiver (6). The data adaptor may also be directly connected to a data terminal (40) via a data terminal interface (50) to receive data-only signals from a data source.
The additional RAM (32) in the data adaptor (30) will be used by the CPU (11) either as either an additional RAM (12) or a replacement for RAM (12). For example, in the case of the GSM standard, RAM (12) may be about 7,000 bits for a speech-only configuration. In the case of speech and data, RAM (32) may be used as a replacement for RAM (12), in which case it would be about 16,000 bits in order to satisfy the memory requirements for a speech and data mobile telephone. Alternatively, it may be about 4,000 bits and used in combination with RAM (12).
The mobile telephone can be arranged so that the data adaptor can be added onto a speech-only phone. That is, a user can purchase a speech-only phone and later purchase the data adaptor, which will plug into an interface constructed in the speech-only mobile phone.
While the present invention has been particularly shown and described with reference to preferred embodiments thereof, it is understood by those skilled in the art that various changes in the form and details may be made therein without departing from the spirit and scope of the invention. | A mobile phone with a basic unit provided with a memory necessary for the processing of speech signals only, whereby the processing of the possible data signals is carried out in an auxiliary unit connected to the interface, the auxiliary unit comprising the memory required for the processing of the data signals. | 7 |
BACKGROUND OF THE INVENTION
Many analogues of LRH have been recently produced and tested as agents for ovulation induction. Modification of the amino acid sequence of LRH has been most advantageous to date with removal of the Gly 10 group and production of the Pro-NHC 2 H 5 terminus, providing a compound reportedly three to five times as active as LRH itself. Fujino et al., Biochem. Biophys. Res. Commun. 49 863 (1972). D-Ala 6 -LRH was subsequently shown to be more potent than LRH, by Monahan et al., Biochemistry 12 4616 (1973). Various other D-amino acids have been inserted in 6-position of LRH and des-Gly 10 -Pro-NHC 2 H 5 -LRH to produce products with improved ovulation inducing properties. U.S. 3,913,412 and Vilchez-Martinez et al., Biochem. Biophys. Res. Commun. 59 1226 (1974). The potency of D-Ala 6 , des-Gly 10 -LRH ethylamide was reported by Coy et al., Biochem. Biophys. Res. Commun. 57 335 (1974) to be about twice that of D-Ala 6 -LRH in stimulating LH secretion. Ling et al., Biochem. Biophys. Res. Commun. 63 801 (1975 ) report the synthesis and biological activity of D-Ala 6 , (Nα-Me)Leu 7 -LRH in stimulating the secretion of LH, which was found to possess 560% of LRH's potency, placing it in the same potency range as D-Ala 6 -LRH.
DESCRIPTION OF THE INVENTION
In accordance with this invention there is provided a group of novel nonapeptides of the formula:
L-p-Glu-L-His-L-Trp-L-Ser-L-Tyr-X-Y-L-Arg-L-Pro-NHC.sub.2 H.sub.5
in which
X is D-Trp or D-2-(1,4-cyclohexadienyl)Gly
and
Y is L-(N-methyl)Leu or L-(N-methyl)Tle
or a non-toxic acid addition salt thereof. Of these compounds, [D-Trp 6 ,(N-methyl)Leu 7 , des-Gly-NH 2 10 , Pro-ethylamide]LRH is the preferred species from its activity standpoint. These compounds induce ovulation in animals and are claudogenic-interceptive agents useful in preventing or terminating pregnancy in mammals. In the use aspect of this invention, the compounds act as claudogenic-interceptive agents when administered post-coitally to a female mammal after ovulation, in that they disrupt the normal physiological processes necessary for implantation and/or maintenance of a fertile ovum.
The intermediates employed in the production of the nonapeptides of this invention form an additional aspect of the invention. The intermediates are the fully protected polypeptideresin and the fully protected polypeptide ethylamides of the formula:
p-Glu-His(R)-Trp-Ser(R.sup.1)-Tyr(R.sup.2)-X-Y-Arg(R.sup.3)-Pro-Z
in which
Z represents the --OCH 2 [polystyrene resin support] or --NHC 2 H 5 ,
X and Y are defined, supra:
R is a protecting group for the imino nitrogen of the histidyl moiety and R 3 is a protecting group for the the guanyl function of the arginyl moiety selected from tosyl, acetyl, benzoyl, tert-butyl, trityl, benzyl, benzyloxycarbonyl and adamantyloxycarbonyl. The tosyl group is preferred as the protecting group for both R and R 3 . However, the guanyl group of the arginyl moiety may be protected via the N 107 or N.sup.ω1 nitrogen atoms by the nitro or tosyl protecting groups and via the N.sup.δ nitrogen atom or either of the N.sup.ω or N.sup.ω1 nitrogen atoms by benzyloxycarbonyl, adamantyloxycarbonyl or trityl group;
and
R 1 and R 2 are protecting groups for the hydroxyl groups of serine and tyrosine. The hydroxyl protecting groups conventionally employed for this purpose are acetyl, tosyl, benzoyl, tert-butyl, trityl, benzyl, benzyloxycarbonyl, 2,6-dichlorobenzyl, and the like, the benzyl and 2,6-dichlorobenzyl groups being preferred for this purpose.
The nonapeptides of this invention are prepared by solid phase methodology, following techniques generally known in the art for building an amino acid sequence from an initial resin supported amino acid. Merrifield, J.A.C.S. 85, 2149 (1963) generally illustrates the technique involved.
The resin support employed may be any suitable resin conventionally employed in the art for the solid phase preparation of polypeptides, preferably polystyrene which has been crosslinked with from 0.5 to about 3-percent divinyl benzene, which has been chloromethylated to provide sites for ester formation with the initially introduced protected amino acid. The amino protected proline is coupled to the chloromethylated resin according to the procedure of Gisin, Helv. Chim. Acta., 56, 1476 (1973). Following the coupling of the amino protected proline to the resin support, the amino protecting group is removed by standard methods employing trifluoroacetic acid in methylene chloride, trifluoroacetic acid alone or HCl in dioxane. The deprotection is carried out at a temperature between about 0° C. and room temperature. After removal of the amino protecting group the remaining α-amino protected and, if necessary, side chain protected amino acids are coupled, seriatim, in the desired order to obtain the product. Alternatively, multiple amino acid group may be coupled by the solution method prior to coupling with the resin supported amino acid sequence. The selection of an appropriate coupling reagent is within the skill of the art. A particularly suitable coupling reagent is N,N'-diisopropyl carbodiimide. Another applicable coupling agent is N,N'-dicyclohexylcarbodiimide.
Each protected amino acid or amino acid sequence is intorduced into the solid phase reactor in a two to six fold excess and the coupling is carried out in a medium of dimethylformamide: methylene chloride or in either dimethylformamide or methylene choride alone. In cases where incomplete coupling occurs the coupling procedure is repeated before removal of the α-amino protecting group, prior to introduction of the next amino acid to the solid phase reactor. The success of the coupling reaction at each stage of the synthesis is monitored by the ninhydrin reaction as described by E. Kaiser et al., Analyt. Biochem, 34, 595 (1970).
The necessary α-amino protecting group employed for each amino acid introduced into the polypeptide is preferably tert-butyloxycarbonyl, although any such protecting group may be employed as long as it is not removed under coupling conditions and is readily removed selectively in relation to the other protecting groups present in the molecule under conditions which otherwise do not effect the formed molecule. Additional examples of such α-amino protecting groups from which selection may be made, after consideration of the rest of the polypeptide molecule, are trityl, phthalyl, tosyl, allyloxycarbonyl, cyclopentyloxycarbonyl, tert-amyloxycarbonyl, benzyloxycarbonyl, o or p-nitrobenzyloxycarbonyl and the like.
The criterion for selecting protecting groups for R-R 3 are (a) the protecting group must be stable to the reagent and under the reaction conditions selected for removing the α-amino protecting group at each step of the synthesis, (b) the protecting group must retain its protecting properties (i.e. not be split off under coupling conditions), and (c) the protecting group must be readily removable upon conclusion of the polypeptide synthesis, under conditions that do not otherwise effect the polypeptide structure.
The fully protected, resin supported nonapeptides present the amino acid sequence:
p-Glu-His(R)-Trp-Ser(R.sup.1)-Tyr(R.sup.2)-X-Y-Arg(R.sup.3)-Pro-O-CH.sub.2 -[polystyrene resin support]
in which the group -O-CH 2 -[polystyrene resin support] represents the ester moiety of one of the many functional groups present in the polystyrene resin.
The fully protected nonapeptides are removed from their resin support by treatment with ethylamine at room temperature followed by removal of any excess ethylamine to yield the intermediate.
p-Gly-His(R)-Trp-Ser(R.sup.1)-Tyr(R.sup.2)-X-Y-Arg(R.sup.3)-Pro-NHC.sub.2 H.sub.5
the fully protected intermediate described in the preceding paragraph is deprotected with liquid hydrogen fluoride in the presence of anisole to yield the nonapeptide claudogenic-interceptive agents of this invention.
The acid addition salts of the nonapeptides of this invention are produced by known techniques from either inorganic or organic acids known to afford pharmaceutically acceptable non-toxic addition products, such as hydrochloric, hydrobromic, sulfuric, phosphoric, maleic, acetic, citric, benzoic, succinic, malic, ascorbic acid, and the like.
The claudogenic-interceptive agents of this invention, when administered to a female mammal, post-coitally pursuant to a daily regimen of at least about 3 micrograms per day per kilogram host body weight for a period of at least three days, completely prevent pregnancy.
Although applicants do not wish to be bound by any specific theory of activity, they propose and believe, based upon studies conducted with a variety of animal models, that the nonapeptides of this invention exert a claudogenic/interceptive action via stimulation of the hypophysical-ovarian steroid axis.
In any event, regardless of the physiological pathway to the end result, the nonapeptides of this invention effectively prevent pregnancy in female mammals upon administration after coitus.
Hence the nonapeptides of this invention are useful as "morning-after" contraceptives to prevent or terminate pregnancy in the female mammal. Within this context, the nonapeptides may be used as anti-littering agents for control of rodent populations without use of redenticides and their possible undesirable effect on other animals in the environment.
Pregnancy was avoided in the animal models by daily administration of the nonapeptide of this invention during the day 1 to day 7 period after coitus as well as upon daily administration over the day 7 to day 12 period, post coitus. Thus both a claudogenic (pre-implantation) as well as an interceptive (post-implantation) type of interference with pregnancy was established.
The procedure followed in evaluating the anti-gravidity properties of the nonapeptides of this invention was as follows: Mature, female, Sprague-Dawley rats (350 + 30 grams body weight) maintained on a 14:10 light:dark schedule were caged with fertile male rats on the evening of proestrus. The presence of vaginal sperm the next morning was considered day 1 of pregnancy. The nonapeptide ethylamine produced in the following examples, representative of the entire group of compounds of this invention, was administered subcutaneously in a corn oil vehicle on days 1-7, or 7-12 of pregnancy at a rate of as low as 1 μg/rat/day. One-half the daily dose was administered at 9 A.M. and at 3 P.M. each day. The recipients of day 1-7 treatment were autopsied on day 14. The recipients of day 7-12 treatment were autopsied on day 18 of pregnancy. The effectiveness of the ethylamide and its effective dose was established by the absence of uterine implantation sites and fetuses. The presence of at least one normal fetus was considered to be the criterion for pregnancy. The claudogenic/interceptive activity of the nonapeptides of this invention was thereby established at a daily dose as low as about 3 micrograms per kilogram host body weight, the treatment being 100 percent effective at a dose of 1 microgram per rat per day in a five rat sample for the day 1-7 period and 10 micrograms for the day 7-12 period.
For the purpose of defining the post coital stages of pregnancy in the rat as an experimental model, the following schedule is provided in definition of post-coital contraceptive activity which, for the purpose of this disclosure, is intended to embrace both pre-(claudogenic) and post-(interceptive) implantation contraceptive activity; day 1 -- vaginal sperm; days 1-3 -- ova transport in oviducts, fertilization; days 3-5 -- blastocyst free in uterine lumen; days 5-7 -- implantation into uterine wall; days > 7 -- post implantation.
Based upon the findings of activity in the prevention of development of pregnancy in the rat model and the fact that present evidence indicates that the hormonal situation relating to the reproductive cycle up to and including ovulation, is basically the same in all female vertebrates, e.g. the human reproductive cycle is physiologically analogous with that of the rat, the activity of the nonapeptides of this invention effectively interferes with the development of the blastocyst pre- and post- implantation in the uterus in all mammals, including the human.
Thus, in accordance with the use aspect of this invention there is provided a method for preventing pregnancy in a mammal which comprises administering:
L-pyroglutamyl-L-histidyl-L-tryptophyl-L-seryl-L-tyrosyl-D-tryptophyl-L-(N-methyl)leucyl-L-arginyl-L-prolylethylamide
or
L-pyroglutamyl-L-histidyl-L-tryptophyl-L-seryl-L-tyrosyl-D-2-(1,4-cyclohexadienyl)glucyl-L-(n-methyl)leucyl-L-arginyl-L-prolylethylamide or the (n-methyl)isoleucyl.sup.7 analogue of either compound,
to said mammal, post coitally, in a daily regimen containing at least about 3 micrograms per kilogram host body weight for a period sufficient to terminate said pregnancy. In operation, the anti-gravidity compounds of this invention interfere with the mechanism of gestation, whether that interference is by an early post-coital, pre-implantation contraceptive or by a postimplantation interceptive mechanism. Hence, the effective sequence of daily administration in the human is from day 1 of ovulation-fertilization to about day 6 to produce a claudogenic response, or from day 6 to about day 14 post ovulation -- fertilization to effect an interceptive response in the gestational period. The human dose, based upon the posology of the experimental model, is approximately 1.5 milligrams per day for a 50 kilogram female. For practical purposes, the applicable subcutaneous human dose is about 50 μg/kg/day or 2.5 mg/50 kg female for a claudogenic effect and about 500 μg/kg/day or 25 mg/50 kg female/day for an interceptive effect.
The nonapeptides of this invention may be administered in any convenient form, orally or parenterally, with or without conventional pharmaceutical adjuvants well known to the art. In addition, conventional adducts of the nonapeptides may be employed to prolong their effectiveness, such as the protamine zinc or aluminum adducts which are parpared by conventional techniques.
The ovulation-induction properties of the nonapeptides of this invention was determined with the preferred compound, [D-Trp 6 ,(N-methyl)Leu 7 ,des-Gly-NH 2 10 ,Pro-ethylamide]LRH as follows: Proestrous female Sprague-Dawley rats were injected intraperitoneally with a hypnotic dose of Nembutal® (50 mg/kg) at 1:30 PM. Between 1:40 and 1:50 PM the rats received the test material via the jugular vein. The following morning the animals were sacraficed and the fallopian tubes examined for ova under a dissecting microscope. The results of this test demonstrated ovulation inducing activity in 100 percent of the rats at a dose of 0.1 mg per rat, in comparison with LRH which requires about 3 mg per rat to obtain 100 percent ovulation and [D-Ala 6 ,des-Gly-NH 2 10 , Proethylamide]LRH which requires about 1 mg per rat for the same response. Thus, in its ovulation induction, the preferred compound of this invention is about ten times as active as its closest structural analogues.
The following examples illustrate the preparation of
p-Glu-His-Trp-Ser-Trp-D-Trp-(N-methyl)Leu-Arg-Pro-NHC.sub.2 H.sub.5
which is the preferred claudogenic-interceptive agent of this invention. It is to be understood, that the other nonapeptides disclosed herein are prepared in the same manner by merely substituting the indicated specific amino acid into the preparatory sequence at the proper position. Thus, the examples are illustrative rather than limiting in nature.
EXAMPLE 1
Preparation of tert-butyloxycarbonylproline resin (method of Gisin, Helv. Chim. Acta, 56, 1476[1973])
Tert-Butyloxycarbonylproline (18.56 g., 86.3 m moles) in an ethanol (112 ml.) -- water (48 ml.) mixture was treated with concentrated aqueous cesium hydrogen carbonate solution until the pH of the solution reached 7. The reaction mixture was stripped and dried by repeated stripping using ethanol, ethanol-benzene, benzene (three times). The residue was dried over phosphorous pentoxide, in vacuo at room temperature overnight.
The total product in dimethylformamide (880 ml.) was stirred overnight at 50° C, under nitrogen, with 80 g. of Bio-Beads S.X. 1 Resin (chloromethylated capacity 0.89 meq./g.). The filtered resin was washed thoroughly with dimethylformamide (twice), dimethylformamide-10% water (twice), dimethylformamide (twice), methanol (twice), chloroform (thrice) and dried over P 2 O 5 . Amino acid analysis indicated a substitution on the resin of 0.56 meq./g.
EXAMPLE 2
L-Pyroglutamyl-N im -tosyl-L-histidyl-L-tryptophyl-O-benzyl-L-seryl-O-(2,6-dichlorobenzyl)-L-tyrosyl-D-tryptophyl-N-methyl-L-leucyl-N g -tosyl-L-arginyl-L-prolyl acyl resin ester ##STR1##
The tert-butyloxycarbonylprolin resin (4.725 g) from Example 1 was placed in a Beckman 990 peptide synthesizer and treated as follows:
1. Wash with methanol.
2. Wash with methylenechloride.
3. Wash with methanol (two times).
4. Wash with methylenechoride (two times)
5. Prewash with 1:1 trifluoroacetic acid-methyl chloride (v/v) containing 0.5% dithioerythritol.
6. Deprotection with the solvent from step 5 (two times for 15 minutes each).
7. Wash with methylenechloride.
8. Wash with dimethylformamide.
9. Wash with 12.5% triethylamine in dimethylformamide (v/v) for 10 minutes (two times).
10. Wash with dimethylformamide.
11. Wash with methylene chloride (two times)
12. Wash with methanol (two times).
13. Wash with methylene chloride (three times).
14. The peptide resin is then gently stirred with 9 moles of the desired tert-butyloxycarbonyl amino acid in ca. 30 ml. of a 1:1 dimethylformamide-methylene chloride (v/v) solvents.
15. 1M diisopropylcarbodiimide (DIC) in methylene chloride (10 m moles) is added in two portions over 30 minutes.
16. The reaction mixture is stirred for 7 hours.
A contact time of 1.5 minutes is allowed for each step unless otherwise stated.
The above steps are repeated until all of the desired amino acids are added.
The following amino acid residues were then introduced consecutively: t-Boc-N g -tosyl-L-arginine (9 m mole), t-Boc-N-methyl-L-Leucine (9 m moles), t-Boc-D-tryptophan (9 m moles), then without deblocking a second portion of t-Boc-D-tryptophan (9 m moles) was allowed to react. Then resuming the normal sequence t-Boc-2,6-dichloro-benzyl-L-tyrosine (9 m moles), t-Boc-O-benzyl-L-serine (9 m moles), t-Boc-L-tryptophan (9 m moles), t-Boc-im-tosyl-L-histidine (9 m moles), and L-2-pyrrolidone-5-carboxylic acid (9 m moles) were added. The washed peptide resin was dried in vacuo and weighed 8.422 g.
EXAMPLE 3
L-pyroglutamyl-N im -tosyl-L-histidyl-L-tryptophyl-O-benzyl-L-seryl-O-(2,6-dichlorobenzyl)-L-tyrosyl-D-tryptophyl-N-methyl-L-leucyl-N g -tosyl-L-arginyl-prolinethylamide
Protected peptide-resin (8.422 g) from Example 2 and ethylamine (120 ml.) were stirred overnight in a glass pressure bottle. Ethylamine was removed under reduced pressure and the residue washed with methanol, dimethylformamide (four times), methanol and methylene chloride. The combined filtrates were evaporated in vacuo below 35° C. to give the title compound (3.277 g).
EXAMPLE 4
L-pyroglutamyl-L-histidyl-L-tryptophyl-L-seryl-L-tyrosyl-D-tryptophyl-N-methyl-L-leucyl-L-arginyl-L-prolinethylamide
The product of Example 3 was treated in vacuo with anhydrous liquid hydrogen fluoride (120 ml.) and anisole (35 ml.) for 50 minutes at 0° C. Hydrogen fluoride was removed under reduced pressure and the residue distributed between diethyl ether and 10% aqueous acetic acid. Lyophyllization of the acid layer afforded the crude title product (2.404 g.).
EXAMPLE 5
Purification and characterization of L-pyroglutamyl-L-histidyl-L-tryptophyl-L-seryl-L-tyrosyl-D-tryptophyl-N-methyl-L-leucyl-L-arginyl-L-prolin-ethylamide
The crude peptide (2.404 g.) in a minimum volume of 0.2N acetic acid was applied to a column of Bio Gel P-2 previously equilibrated with 0.2N acetic acid and then eluted with the same solvent. Fractions of 9 ml. each were collected. Peptide material was located by Ehrlich spot test and UV analysis. One major fraction was obtained, 34 50 (2.234 g.). A second Bio Gel P-2 column afforded 1.928 g. of desired material. This material was rechromatographed on a partition column of Sephadex G-25 fine (2.5 × 100 cm.) prepared by equilibration with lower phase and then upper phase of the BAW system (n-butanol:acetic acid:water, 4:1:5). Elution with upper phase afforded fractions A 36-48 (820 mg.), B 49-64 (633 mg.). Fraction A was rechromatographed using the same system which afforded 295 mg. of the desired peptide.
The Rf value of the peptide (30 μg load) in the thin layer system (silica, plates-Brinkman) n-butanol:acetic acid: water (4:1:5, upper phase). Rf 0.21 n-butanol:acetic acid:ethyl acetate:water (1:1:1:1). Rf 0.57.
The optical rotation measured on a Carl Zeiss LEP A-2 photoelectric precision polarimeter, [a] D 26 = -80.91° (c=0.98, 1% acetic acid).
Hydrolysis of the peptide in methanesulfonic acid (0.2 ml/1 mg. peptide) for 20 hours at 110° C. in a closed evacuated system revealed all of the required amino acids to be present. | Compounds of the formula:
L-p-Glu-L-His-L-Trp-L-Ser-L-Tyr-X-Y-L-Arg-L-Pro-NHC.sub.2 H.sub.5
in which X is D-Trp or D-2-(1,4-cyclohexadienyl)Gly Y is L-(N-methyl)-Leu or L-(N-methyl)-ILe or a non-toxic acid addition salt thereof, are potent ovulation inducers and claudogenic-interceptive agents useful in preventing or terminating pregnancy in mammals. | 0 |
CROSS-REFERENCE TO THE RELATED APPLICATIONS
The present application is related to the application Ser. No. 901,776 filed on Aug. 29, 1986, now U.S. Pat. No. 4,709,775, and assigned to the same assignee of the present application.
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to a vehicle driving torque transmitting system, and more particularly to a system for transmitting a driving torque from a power plant to a vehicle wheel. More specifically, the present invention pertains to means for controlling the torque transmitted to the wheels in such driving torque transmitting system.
2. Description of the Prior Art
In a conventional torque transmitting system, it has been known to provide a slip clutch in a torque transmitting path to control the torque to be transmitted. In one type, there is interposed in the torque transmitting path a wet clutch which includes an input friction member and an output friction member which are forced into engagement under a fluid pressure. The capacity of the wet clutch of transmitting torque is dependent on the value of the fluid pressure so that the torque to be transmitted can be controlled by changing the fluid pressure forcing the friction members into engagement.
In another type, a viscous coupling is interposed in the torque transmitting path. The viscous coupling includes input and output friction plates which are located adjacent to each other with a viscous fluid interposed therebetween. One example of the torque transmitting system using such viscous coupling is shown in the U.S. Pat. No. 3,760,992. In the viscous coupling disclosed by the U.S. patent, the friction plates are formed with openings which determines the torque transmitting capacity. By changing the diameter of the openings, it is possible to obtain viscous couplings of different torque transmitting capacity.
It should be noted that in the conventional torque transmitting system there is always a certain extent of slip between the input and output friction members so that there is a possibility of temperature increase due to generation of heat under the slip movement. There will be no serious problem as long as the temperature increase is within an allowable limit, however, if there is an excessive slip, the temperature increase will be such that the friction plates are damaged under the heat.
SUMMARY OF THE INVENTION
It is therefore an object of the present invention to provide a driving torque transmitting system having transmitting torque control means which can control the torque transmitting capacity without having a danger of overheating.
Another object of the present invention is to provide a torque trnasmitting system in which the torque transmittal is controlled in accordance with the heat generated in the system.
According to the present invention, the above and other objects can be accomplished by a driving torque transmitting system including torque transmitting means disposed in a torque transmitting path from a power plant to a vehicle wheel, said torque transmitting means having friction members which are adapted to be brought into engagement with each other under a biasing force which determines a torque transmitting capacity of the torque transmitting means, control means operable in accordance with a predetermined control characteristics to adjust the biasing force within a control range so that a slip rate between the friction members is changed in accordance with the control characteristics, detecting means for detecting a condition of heat generation in the torque transmitting means, judging means for judging as to whether the condition of heat generation is in a predetermined heat generating range and producing an output representing that the condition of heat generation is in the predetermined heat generating range, biasing force adjusting means responsive to the output of the judging means for controlling the control means so that the biasing force is fixed to a value which is out of said control range and in which the heat generation is suppressed.
According to one aspect of the present invention, the fixed value of the biasing force is such that the torque transmittal is interrupted. In another aspect, the fixed value of the biasing force is such that the friction members are locked so that they rotate without slippage as a unit. Means may be provided to provide a first and second predetermined heat generating ranges so that the judging means makes a judgement as to whether the condition of heat generation is in either of the heat generating ranges.
The detecting means may detect the condition of heat generation in terms of the difference between the input and output speeds and the amount of the torque being transmitted. The torque transmitting system in accordance with the present invention can be advantageously applied to a four wheel drive motor vehicle. In that case, the torque transmitting system may be provided in the rear wheel drive system of the vehicle.
The above and other objects and features of the present invention will become apparent from the following descriptions of a preferred embodiment taking reference to the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a diagrammatical plan view of a vehicle power transmitting system to which the present invention can be applied;
FIG. 2 is a diagrammatical illustration showing one embodiment of the present invention;
FIG. 3 is a diagram showing the relationship between the input and output speed difference and the torque being transmitted; and,
FIG. 4 is a program flow chart showing the control in accordance with the embodiment of the present invention.
DESCRIPTION OF THE PREFERRED EMBODIMENT
Referring to the drawings, particularly to FIG. 1, there is shown a four wheel drive vehicle drive system to which the present invention can be applied. The system includes a power plant 10 which may be an internal combustion engine or a transmission gear mechanism which transmit the engine output power. The power plant 10 has an output shaft 12 which carries a driving gear 13a of a transfer gear mechanism 13. The gear 13a is in meshing engagement with a driven gear 13b of the transfer gear mechanism 13. The driven gear 13b is provided on a front propeller shaft 14 which is connected through a final gear unit 17 such as a front differential gear unit with front wheels 18.
The output shaft 12 of the power plant 10 is further connected through a torque transmitting mechanism such as a hydraulic variable clutch 15 with a rear propeller shaft 16. The rear propeller shaft 16 is connected through a final gear unit such as a rear differential gear unit 19 with rear wheels 20. It will therefore be understood that a first torque transmitting path is provided by the power plant 10, the output shaft 12, the transfer gear mechanism 13, the front propeller shaft 14, the front differential gear unit 17 and the front wheels 18. A second torque transmitting path is provided by the power plant 10, the output shaft 12, the variable clutch 15, the rear propeller shaft 16, the rear differential gear unit 19 and the rear wheels 20.
The variable clutch 15 is of a type in that the torque transmitting capacity can be adjusted by controlling the hydraulic pressure applied to the clutch 15. Referring to FIG. 2, it will be noted that the variable clutch 15 includes a casing 15a which is formed integrally with the output shaft 12 of the power plant 10 and defines a clutch chamber 15b in the casing 15a. The casing 15a is provided with a plurality of friction plates 15c projecting into the clutch chamber 15b. The rear propeller shaft 16 carries a plurality of fiction plates 15d which are interlaced with the friction plates 15c on the casing 15a. The friction plates 15c are carried on the casing 15a for axial movements and a piston 15e is provided in the casing 15a for forcing the friction plates 15c on the casing 15a into friction engagement with the friction plates 15d on the rear propeller shaft 16.
Behind the piston 15e, there is defined a hydraulic chamber 15f which is connected through a control valve 23 with a hydraulic pump 22. The hydraulic pump 22 draws hydraulic liquid from a hydraulic oil reservoir 21 and supplies the hydraulic oil under pressure to the control valve 23. The control valve 23 functions to adjust the hydraulic pressure applied to the hydraulic chamber 15f in the variable clutch 15. It will be understood that the slip rate between the friction plates 15c and 15d can be adjusted by changing the hydraulic pressure applied to the hydraulic chamber 15f.
In order to control the valve 23 so that the hydraulic pressure to the chamber 15f is appropriately controlled, there is provided a control unit 24. The control unit 24 is connected with a vehicle speed detector 25, a vehicle steering angle detector 26, a speed difference detector 27 and an engine accelerator pedal position detector 28 to receive signals therefrom. The vehicle speed detector 25 functions to detect the vehicle speed for example in terms of the rotating speed of the output shaft 12 of the power plant 10 and produces a vehicle speed signal Sv representing the vehicle speed. The steering angle detector 26 detects the vehicle steering angle and produces a steering angle signal Sa. The speed difference detector 27 functions to detect the speed difference between the shafts 12 and 16 and produce a speed difference signal Sdn. The engine accelerator pedal position detector 28 detects that the engine accelerator pedal is in the minimum output position and produces an accelerator off signal Soff. The speed difference detector 27 may be substituted by a rear propeller shaft speed detector which detects the rotating speed of the rear propeller shaft 16. The speed difference maythen be calculated in the control unit 24 from the speed signal Sv and the rear propeller shaft speed signal.
The control unit 24 has a map which determines values of control current i depending on the vehicle speed, the vehicle steering angle and the speed difference between the shafts 12 and 16. The control unit 24 functions to calculate the control current i based on the input signals Sv, Sdn and Sa and applies the control current i to the control valve 23.
The control valve 23 is of a type that produces a hydraulic pressure which is proportional to the control current i. Thus, the hydraulic pressure applied to the hydraulic chamber 15f is controlled by the control current i. The clutch 15 is of a type in which the torque transmitting capacity is proportionally determined by the hydraulic pressure applied to the hydraulic chamber 15f. In the four wheel drive vehicle system as shown in FIG. 1, the torque transmitting capacity of the clutch 15 determines the torque split ratio between the front propeller shaft 14 and the rear propeller shaft 16 and the torque in the output shaft 12 of the power unit 10 is transmitted to the rear propeller shaft 16 in an amount corresponding to the transmitting capacity of the clutch 15.
In the embodiment which is being described, the control current i is determined in accordance with the speed difference between the shafts 12 and 16 so that the relationship between the torque T transmitted through the clutch 15 and the speed difference dn becomes as shown by a solid line T=f(dn) in FIG. 3. According to the features of the present invention, the torque transmittal through the clutch 15 is controlled in accordance with the condition of heat generation in the clutch 15. In the embodiment, assumption is made that the quantity of heat generated in the clutch 15 is proportional to the product of the speed difference and the torque transmitted through the clutch 15. In other words, the quantity of heat generation P can be represented by the formula P=K(dn)(T). In FIG. 3, the safety limit of heat generation is shown by a line P 1 and the region (I) which is below the line P 1 shows the safety zone. The allowable limit of heat generation is shown by a line P 2 . The region (II) which is between the lines P 1 and P 2 represents the region wherein the operation can be continued in a limited time. The region (III) which is above the line P 2 represents the dangerous zone.
In operation, the control current i is provided in accordance with the input signals Sv, Sdn and Sa as described previously, and the control valve 23 is controlled by the control current i. Thus, the hydraulic pressure to the clutch 15 is controlled and the torque transmitted through the clutch 15 is regulated so that the relationship between the torque and speed difference is changed as shown by the line T=f(dn). When the operating condition goes into the region (II) as shown by the point A, count is made of a time t wherein the operation in the region (II) is continued. When the time t exceeds a predetermined value t 1 , the control current i is increased so that the pressure to the clutch 15 is correspondingly increased to have the clutch 15 is directly connected. As the result, the shaft 12 is directly connected with the shaft 16. Although the torque transmitted through the clutch is increased as shown by a line Tr1 in FIG. 3, the operating condition is shifted back to the safety zone (I) and the operation is continued at the point B. It should be noted that the pressure to the clutch 15 may be relieved when the time t exceeds the predetermined value t 1 so that the clutch 15 is disengaged and torque transmittal is interrupted as shown by a line Tr3. The operating condition in this instance is shown by the point E. When the operating condition goes to a point C where the line T=f(dn) crosses the line P2. Then, the hydraulic pressure to the clutch 15 is relieved and the torque transmittal through the clutch 15 is interrupted as shown by a line Tr2. The operating condition in this instance is shown by a point D. Alternatively, the clutch 15 may be directly connected to shaft the operating condition to the point B as shown by a line Tr4.
In the control as shown in FIG. 3, the torque transmitted through the clutch 15 can be determined in relation to the speed difference in accordance with the curve T=f(dn). Therefore, it is possible to represent the condition of heat generation in terms of the speed difference dn or the slip ratio of the clutch 15. In FIG. 3, the speed difference dn 1 shows the upper limit of the safety zone (I) whereas the speed difference dn 2 shows the upper limit of the region (II) or the allowable limit of heat generation.
Referring now to FIG. 4, there is shown a flow diagram of the operation of the control unit 24 which may be constituted by a microprocessor. When the control unit 24 is initialized, the input signals Sv, Sa, Sdn and Soff are read in the step ST1 and a judgement is made in the step ST2 as to whether the accelerator off signal Soff is produced. When there is no signal Soff, it is judged that the accelerator pedal is actuated and the engine is producing an output to drive the wheels 18 and 20 and the step ST3 is carried out. In the step ST3, the position of the flag 2 is read. When it is judged that the flag 2 is not in the "1" position, a judgement is made in the step ST4 as to whether the actual speed difference dn is not smaller than the speed difference dn 2 . If the result of the judgement is that the actual speed difference dn is smaller than the speed difference dn 2 , the position of the flag 1 is read in the step ST5. If it is judged that the flag 1 is not in the position "1", the control current i is determined in the step ST7 so that the relationship between the speed difference dn and the torque T transmitted through the clutch 15 is established in accordance with the function T=f(dn) as shown in FIG. 3. For example, the control current i is determined to a value so that the torque Tr5 is transmitted through the clutch 15 to establish the speed difference dn 3 .
When it is judged in the step ST6 that the actual speed difference dn is greater than the value dn 1 , the count in the timer t is read in the step ST8. If the timer count is not greater than the value t 1 , the value one is added to the timer count in the step ST9 and the step ST7 is then carried out. If the timer count is greater than the value t 1 , the flag 1 is set to the position "1" in the step ST10 and the control current i is increased in the step ST11 so that the direct connection is established in the clutch 15. When it is judged in the step ST5 that the flag 1 is in the position "1", the step ST11 is carried out to establish the direct connection in the clutch 15. By directly connecting the clutch 15, it is possible to avoid overheating while maintaining the four wheel drive. When the clutch 15 is directly connected, the heat generation increases temporarily as shown by the line Tr1 in FIG. 3, however, overheating can be avoided in this operating range.
When it is judged in the step ST4 that the actual speed difference dn is greater than the value dn 2 , the flag 2 is set to the position "1" in the step ST12 and the control current i is decreased in the step ST13 to thereby release the clutch 15. When it is judged that the flag 2 is already in the position "1" in the step ST3, the step ST13 is carried out to release the clutch 15. By immediately releasing the clutch 15, it is possible to decrease the heat generation as shown by the line Tr2 in FIG. 3 without any temporary increase in the heat generation.
If the judgement in the step ST2 is such that there is produced the signal Soff, it is judged that the engine throttle valve is in the minimum opening position so that no driving effort is given from the engine to the wheels 18 and 20. Then, the procedure goes from the step ST2 to the step ST14 wherein the flags 1 and 2 are set to the positions "0". Thereafer, the timer is set to "0" in the step ST15 and the step ST7 is then carried out.
It will be understood that, by the control procedure as described with reference to FIG. 4, it is possible to determine the torque transmitted through the clutch 15 so that the slip rate in the clutch 15 is changed as shown in FIG. 3 as long as the speed difference is smaller than the value dn 1 . When the speed difference is between the values dn 1 and dn 2 , the time of operation in this operating region is counted and the time count exceeds the value t 1 the clutch 15 is directly connected to avoid overheating of the clutch 15. If the speed difference dn exceeds the value dn 2 , the clutch 15 is immediately disengaged.
The invention has thus been shown and described with reference to a specific embodiment, however, it should be noted that the invention is in no way limited to the details of the arrangements described but changes and modifications may be made without departing from the scope of the appended claims. | A vehicle driving system including a hydraulic clutch having a plurality of friction members which are adapted to be forced into engagement with each other by a hydraulic pressure applied to a piston in the clutch. A control unit is provided to detect a condition of heat generation in the hydraulic clutch and relieving the hydraulic pressure to the clutch or increasing the hydraulic pressure to the hydraulic clutch when the condition of heat generation is out of an allowable limit. | 5 |
CLAIM OF PRIORITY
[0001] The present application claims the benefit of priority to U.S. Provisional Application No. 61/713,911 filed on Oct. 15, 2012, which is incorporated herein in its entirety by reference.
FIELD OF THE INVENTION
[0002] The present invention relates to drivelines for vehicles and more particularly to a fastening assembly for a drive pinion.
BACKGROUND OF THE INVENTION
[0003] Conventionally, drive pinions used with axle assemblies have been drivingly engaged with other components of a drivetrain of a vehicle using a companion flange. The companion flange is a hollow annular body which has a substantially “L” shaped cross-section. The companion flange typically provides a location for securing a portion of a universal joint thereto; however, other components of a drivetrain may be coupled thereto. An outermost portion of the companion flange usually includes a plurality of apertures formed therein, which receive threaded fasteners to secure a component to the companion flange.
[0004] The companion flange, however, has limitations that restrict its use in certain applications. A design of the companion flange can become excessive in size as a torque requirement of a drivetrain increases. Ease of manufacturability of the companion flange can be decreased in certain applications. Further, assembly of the drivetrain including the companion flange may be time consuming. Consequently, selecting the companion flange as a drivetrain component may become costly and problematic.
[0005] It would be advantageous to develop a fastening assembly for a drive pinion that is compact, able to handle increased torque loads, and is easy to manufacture.
SUMMARY OF THE INVENTION
[0006] Presently provided by the invention, a fastening assembly for a drive pinion that is compact, able to handle increased torque loads, and is easy to manufacture, has surprisingly been discovered.
[0007] In one embodiment, the present invention is directed to a drive pinion fastening assembly. The drive pinion fastening assembly comprises a drive pinion, a pinion sleeve, an external sleeve, and a pinion fastener. The pinion sleeve is disposed on and engaged with the drive pinion. The external spline is formed on one of the drive pinion and the pinion sleeve for engaging a power transmission component. The pinion fastener is disposed on and engaged with the drive pinion. The pinion fastener militates against axial movement of the pinion sleeve with respect to the drive pinion.
[0008] In another embodiment, the present invention is directed to a drive pinion fastening assembly. The drive pinion fastening assembly comprises a drive pinion, a pinion sleeve, an external spline, and a pinion fastener. The drive pinion includes a locking spline portion. The pinion sleeve is disposed on and engaged with the drive pinion. The external spline is formed on the drive pinion for engaging a power transmission component. The pinion fastener is disposed on and engaged with the locking spline portion of the drive pinion through an interference fit. The pinion fastener militates against axial movement of the pinion sleeve with respect to the drive pinion.
[0009] In yet another embodiment, the present invention is directed to a drive pinion fastening assembly. The drive pinion fastening assembly comprises a drive pinion, a pinion sleeve, an external spline, and a pinion fastener. The drive pinion includes a splined portion. The pinion sleeve includes an inner splined portion for engaging the splined portion of the drive pinion. The pinion sleeve is disposed on and engaged with the drive pinion. The external spline is formed on the pinion sleeve and engages a power transmission component. The pinion fastener includes a thread formed on an inner surface thereof. The pinion fastener is disposed on and threadingly engaged with the drive pinion. The pinion fastener militates against axial movement of the pinion sleeve with respect to the drive pinion.
[0010] Various aspects of this invention will become apparent to those skilled in the art from the following detailed description of the preferred embodiment, when read in light of the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
[0011] The above, as well as other advantages of the present invention will become readily apparent to those skilled in the art from the following detailed description when considered in the light of the accompanying drawings in which:
[0012] FIG. 1 is a perspective view of a pinion sleeve and a pinion fastener of a pinion fastening assembly according to an embodiment of the present invention;
[0013] FIG. 2 is a cross sectional view of a pinion fastening assembly according to an embodiment including the pinion sleeve and the pinion fastener illustrated in FIG. 1 ;
[0014] FIG. 3 is a perspective view of a pinion sleeve of a pinion fastening assembly according to another embodiment of the present invention; and
[0015] FIG. 4 is a cross sectional view of a pinion fastening assembly according to an embodiment including the pinion sleeve and the pinion fastener illustrated in FIG. 3 .
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0016] It is to be understood that the invention may assume various alternative orientations and step sequences, except where expressly specified to the contrary. It is also to be understood that the specific devices and processes illustrated in the attached drawings, and described in the following specification are simply exemplary embodiments of the inventive concepts defined herein. Hence, specific dimensions, directions or other physical characteristics relating to the embodiments disclosed are not to be considered as limiting, unless expressly stated otherwise.
[0017] FIGS. 1 and 2 illustrate a drive pinion fastening assembly 100 according to an embodiment of the present invention. The drive pinion fastening assembly 100 includes a drive pinion 102 , a pinion sleeve 104 , and a pinion fastener 106 . The pinion sleeve 104 is disposed on the drive pinion 102 and is threadingly engaged with the drive pinion 102 . The pinion fastener 106 is disposed in the pinion sleeve 104 and is in engagement with the pinion sleeve 104 and the drive pinion 102 .
[0018] FIG. 2 illustrates the drive pinion 102 . The drive pinion 102 is an elongate member rotatably disposed in a housing 108 . It is understood that the drive pinion 102 and the housing 108 may be used with a front axle drive assembly (not shown) or a rear axle drive assembly (not shown). The drive pinion 102 is formed by machining and heat treating a metal such as steel. A pair of bearings 110 is disposed between the drive pinion 102 and the housing 108 , to facilitate rotation of the drive pinion 102 therein. The drive pinion 102 includes a threaded portion 112 , a locking spline portion 114 , and an engagement spline portion 116 .
[0019] The threaded portion 112 of the drive pinion 102 is formed on an outer surface of the drive pinion 102 adjacent the locking spline portion 114 , intermediate a first end 118 and a second end 120 of the drive pinion 102 . When the pinion sleeve 104 is disposed on the drive pinion 102 , the pinion sleeve 104 may be threadingly engaged with the threaded portion 112 .
[0020] The locking spline portion 114 of the drive pinion 102 is formed on an outer surface of the drive pinion 102 between the threaded portion 112 and the engagement spline portion 116 . The locking spline portion 114 engages the pinion fastener 106 when the pinion fastener 106 is disposed thereon. The locking spline portion 114 comprises a plurality of splines in an annular arrangement; however, it is understood that the locking spline portion 114 may comprise other features for engaging the pinion fastener 106 . A diameter of the locking spline portion 114 is less than a diameter of the threaded portion 112 .
[0021] The engagement spline portion 116 of the drive pinion 102 is formed adjacent an end thereof. When the drive pinion 102 is disposed in the housing 108 , the end including the engagement spline portion 116 extends therefrom. The engagement spline portion 116 comprises a plurality of splines formed on the outer surface of the drive pinion 102 in an annular arrangement. A diameter of the engagement spline portion 116 is less than a diameter of the threaded portion 112 and the locking spline portion 114 ; however, it is understood that the diameter of the engagement spline portion 116 may be substantially equal to the diameter of the locking spline portion 114 . The engagement spline portion 116 engages a power transmission component (not shown), such as a universal joint.
[0022] The pinion sleeve 104 is a hollow annular body having a first end 122 and a second end 124 . As shown in FIGS. 1 and 2 , the second end 124 has a diameter greater than a diameter of the first end 122 ; however, it is understood that the first end 122 and the second end 124 of the pinion sleeve 104 may have other sizes and shapes. At least a portion of an inner surface 126 of the pinion sleeve 104 has a thread 128 formed thereon corresponding to the threaded portion 112 of the drive pinion 102 . A fastening recess 130 is formed in the second end 124 of the pinion sleeve 104 .
[0023] When the drive pinion fastening assembly 100 is assembled, the first end 122 of the pinion sleeve 104 abuts one of the bearings 110 and applies a force thereto to secure the drive pinion 102 within the housing 108 .
[0024] The second end 124 of the pinion sleeve 104 extends radially outwardly from a remaining portion of the pinion sleeve 104 . As shown in FIG. 1 , the second end 124 is shaped to facilitate engagement with a fastening tool (not shown); however, it is understood that the second end 124 may be shaped in any manner that facilitates rotation of the pinion sleeve 104 . The fastening recess 130 is hexagonal in shape and substantially corresponds to a shape of the pinion fastener 106 ; however, it is understood that other shapes may be used.
[0025] The pinion fastener 106 is a member formed from a metal. The pinion fastener 106 may be formed by stamping a sheet metal, coining a workpiece, or any other suitable process. The pinion fastener 106 is disposed in the fastening recess 130 , about the drive pinion 102 , and is in driving engagement with the drive pinion 102 when the drive pinion fastening assembly 100 is assembled. The pinion fastener 106 has an inner peripheral edge 132 and an outer peripheral edge 134 . The inner peripheral edge 132 defines a circular perforation through the pinion fastener 106 and has a diameter greater than the diameter of the engagement spline portion 116 and less than the diameter of the locking spline portion 114 . The outer peripheral edge 134 is substantially hexagonal in shape and substantially corresponds to a shape of the fastening recess 130 ; however, it is understood other shapes may be used.
[0026] In use, the drive pinion fastening assembly 100 facilitates securing the drive pinion 102 within the housing 108 in a manner that isolates the pinion sleeve 104 and the pinion fastener 106 from torque applied to drive pinion 102 . Torque is applied directly to the drive pinion 102 through the engagement spline portion 116 , and thus the pinion sleeve 104 and the pinion fastener 106 are isolated from torque applied to drive pinion 102 .
[0027] When the drive pinion fastening assembly 100 is assembled, the drive pinion 102 is disposed through the pair of bearings 110 and the first end 118 of the drive pinion 102 including the engagement spline portion 116 extends from a perforation 136 formed in the housing 108 . Next, the pinion sleeve 104 is disposed on the drive pinion 102 and the thread 128 is engaged with the threaded portion 112 . The pinion sleeve 104 is rotated until the first end 122 contacts one of the bearings 110 and a predetermined level of torque or rotation angle is applied thereto, which secures the drive pinion 102 and the bearings 110 . Next, the pinion fastener 106 is disposed in the fastening recess 130 , with the inner peripheral edge 132 disposed against, but not engaged with, the locking spline portion 114 .
[0028] To secure the pinion fastener 106 to the locking spline portion 114 , a press (not shown) or other tool is disposed against the pinion fastener 106 and a force is applied thereto in a direction of the pinion sleeve 104 . The inner peripheral edge 132 deforms as a result of the force being applied by the press, and the pinion fastener 106 becomes engaged with both the locking spline portion 114 and the pinion sleeve 104 . The pinion fastener 106 is engaged with the locking spline portion 114 through an interference fit and the pinion fastener 106 is engaged with the pinion sleeve 104 because the outer peripheral edge 134 is disposed within the fastening recess 130 . Such an arrangement militates against rotation of the pinion sleeve 104 and therefore prevents the pinion sleeve 104 from becoming unfastened as the pinion sleeve 104 is in driving engagement with the pinion fastener 106 .
[0029] FIGS. 3 and 4 illustrate a drive pinion fastening assembly 200 according to another embodiment of the present invention. The drive pinion fastening assembly 200 includes a drive pinion 202 , a pinion sleeve 204 , and a pinion fastener 206 . The pinion sleeve 204 is disposed on the drive pinion 202 and is spliningly engaged with the drive pinion 202 . The pinion fastener 206 is disposed in the pinion sleeve 204 and is threadingly engaged with the drive pinion 202 .
[0030] FIG. 4 illustrates the drive pinion 202 . The drive pinion 202 is an elongate member rotatably disposed in a housing 208 . It is understood that the drive pinion 202 and the housing 208 may be used with a front axle drive assembly (not shown) or a rear axle drive assembly (not shown). The drive pinion 202 is formed by machining and heat treating a metal such as steel. A pair of bearings 210 is disposed between the drive pinion 202 and the housing 208 , to facilitate rotation of the drive pinion 202 therein. The drive pinion 202 includes a splined portion 212 and a threaded portion 214 formed thereon.
[0031] The splined portion 212 of the drive pinion 202 is formed on an outer surface thereof adjacent the threaded portion 214 , intermediate a first end 216 and a second end 218 of the drive pinion 202 . When the pinion sleeve 204 is disposed on the drive pinion 202 , the pinion sleeve 204 may be spliningly engaged with the splined portion 212 .
[0032] The threaded portion 214 of the drive pinion 202 is formed on an outer surface of the drive pinion 202 adjacent the splined portion 212 . When the pinion fastener 206 is disposed on the threaded portion 214 , the pinion fastener 206 may be threadingly engaged with the threaded portion 214 . When the drive pinion 202 is disposed in the housing 208 , the end including the threaded portion 214 extends therefrom. A diameter of the threaded portion 214 is less than a diameter of the splined portion 212 .
[0033] The pinion sleeve 204 is a hollow annular body having a first end 220 and a second end 222 . The second end 222 has a diameter greater than the first end 220 ; however, it is understood that the first end 220 and the second end 222 may have other shapes and sizes. At least a portion of an inner surface 224 of the first end 220 has an inner splined portion 226 formed thereon corresponding to the splined portion 212 of the drive pinion 202 . When the drive pinion fastening assembly 200 is assembled, the inner splined portion 226 of the pinion sleeve 204 is in driving engagement with the splined portion 212 of the drive pinion 202 . At least a portion of an outer surface 228 of the second end 222 defines an outer splined portion 230 formed thereon. The outer splined portion 230 engages a power transmission component (not shown), such as a universal joint. A portion of the first end 220 defines a fastening flange 232 in the pinion sleeve 204 . The fastening flange 232 extends radially outwardly from the first end 220 of the pinion sleeve 204 . When the drive pinion fastening assembly 200 is assembled, the first end 220 of the pinion sleeve 204 abuts one of the bearings 210 and applies a force thereto to secure the drive pinion 202 within the housing 208 .
[0034] The pinion fastener 206 is a threaded fastener formed from a metal using any conventional process. The pinion fastener 206 is a conventional, hexagonally shaped, flanged nut; however, it is understood that the pinion fastener 206 may be another type of fastener and have another shape. The pinion fastener 206 is disposed within the pinion sleeve 204 , about the first end 216 of the drive pinion 202 , and is threadingly engaged with the threaded portion 214 of the drive pinion 202 when the drive pinion fastening assembly 200 is assembled. A thread 234 formed on an inner surface 236 of the pinion fastener 206 is engaged with the threaded portion 214 of the drive pinion 202 . When the drive pinion fastening assembly 200 is assembled, the pinion fastener 206 may be secured to the drive pinion 202 using a thread adhesive (not shown).
[0035] In use, the drive pinion fastening assembly 200 facilitates securing the drive pinion 202 within the housing 208 in a manner that isolates the pinion fastener 206 from torque applied to drive pinion 202 . Torque is applied to the drive pinion 202 through the pinion sleeve 204 . The outer splined portion 230 of the pinion sleeve 204 is in engagement with the power transmission component, and torque is then transferred to the drive pinion 202 through the engagement of the inner splined portion 226 and the splined portion 212 . Accordingly, the pinion fastener 206 is isolated from torque applied to drive pinion 202 .
[0036] When the drive pinion fastening assembly 200 is assembled, the drive pinion 202 is disposed through the pair of bearings 210 and the end of the drive pinion 202 including the threaded portion 214 extends from a perforation 238 formed in the housing 208 . Next, the pinion sleeve 204 is disposed on the drive pinion 202 and the inner splined portion 226 is engaged with the spline portion 212 . Next, the pinion fastener 206 is disposed within the second end 218 of the pinion sleeve 204 .
[0037] To secure the pinion fastener 206 to the drive pinion 202 , the thread 234 of the pinion fastener 206 is then engaged with the threaded portion 214 of the drive pinion 202 . The pinion fastener 206 is rotated until a predetermined level of torque or angle of rotation is reached, which secures the drive pinion 202 and the bearings 210 within the housing 208 , and the pinion sleeve 204 to the drive pinion 202 . Such an arrangement militates against rotation of the pinion fastener 206 as a torque applied to the drive pinion 202 passes through the pinion sleeve 204 and therefore prevents the pinion fastener 206 from becoming unfastened as the pinion sleeve 204 is in driving engagement with the drive pinion 202 .
[0038] In accordance with the provisions of the patent statutes, the present invention has been described in what is considered to represent its preferred embodiments. However, it should be noted that the invention can be practiced otherwise than as specifically illustrated and described without departing from its spirit or scope. | A drive pinion fastening assembly is provided. The drive pinion fastening assembly includes a drive pinion, a pinion sleeve, an external spline, and a pinion fastener. The pinion sleeve is disposed on and engaged with the drive pinion. The external spline is formed on one of the drive pinion and the pinion sleeve for engaging a power transmission component. The pinion fastener is disposed on and engaged with the drive pinion. The pinion fastener militates against axial movement of the pinion sleeve with respect to the drive pinion. The drive pinion fastening assembly is compact, able to handle increased torque loads, and is easy to manufacture. | 5 |
BACKGROUND
A time to digital converter (TDC) is a circuit known in the art to detect phase offset (such as jitter) between two signals, e.g., a control signal of a phase locked loop and a reference clock signal.
FIG. 1 is a block diagram of a known TDC in a configuration known as a Vernier delay line. The principles of this TDC 100 are described in U.S. Pat. Pub. No. 2009/0225631 by Shimizu et al., “Time-To-Digital Converter,” which is hereby incorporated by reference herein in its entirety. The TDC 100 has a first delay line in which a sequence of delay cells 114 are arranged to sequentially delay an original clock CK. Each delay cell 114 delays its input by a predetermined delay amount τ1, and a plurality of delay taps CK 1 , CK 2 , CK 3 , . . . are provided to the data (D) inputs of corresponding D-type flip flops 116 . A signal SC to be measured is provided to a second delay line in which each delay cell in a sequence of delay cells 115 delays its input by a predetermined delay amount τ2, where τ1 is typically greater than τ2. The first and second delay lines may be implemented using pairs of inverters, for example. Successive taps from the second delay line are provided as clock inputs SC 1 , SC 2 , SC 3 , . . . to corresponding flip flops 116 .
Because τ1>τ2, signals in the sequence SC 1 , SC 2 , SC 3 , . . . are advanced relative to signals in the sequence CK 1 , CK 2 , CK 3 , . . . . In other words, if a rising clock edge of CK 1 occurs before a rising clock edge of SC 1 , there will be a point along the first and second delay lines at which a delay tap from the second sequence 115 “catches up” to a corresponding delay tap from the first sequence 114 . In this example, the Q outputs from flip flops 116 are ‘1’ up to this point and ‘0’ thereafter. An encoder circuit 117 receives the Q outputs and encodes a position at which such crossover occurs, and the encoded result represents the jitter of the signal SC to be measured with respect to the reference clock CK. For example, if 2 N flip flops are employed, encoder 117 provides an N-bit encoded value representing a jitter of signal SC.
Conventional TDC 100 has certain deficiencies. Due to variations in process, voltage, and temperature, the total delay of a delay line may be different than the desired value, resulting in certain disadvantageous effects. For example, a variation in the total delay of delay cells 115 may result in undesirable phase noise in the encoded signal indicating jitter. Furthermore, mismatch between individual delay cells may result in other disadvantageous effects. For example, variations in the delays of delay cells 115 may result in harmonic “spurs” (spurious noise components) in a frequency response of the encoded jitter signal. Both these disadvantageous effects impair the ability to accurately measure jitter.
FIG. 2 is a block diagram of a known timing circuit 200 that seeks to address the phase noise and spur problems discussed above. Timing circuit 200 is fully described in Temporiti et al., “A 3 GHz Fractional All-Digital PLL With a 1.8 MHz Bandwidth Implementing Spur Reduction Techniques,” IEEE Journal of Solid-State Circuits, Vol. 44, No. 3, pp. 824-34, March 2009, and only a brief description of the principles of that circuit follows. Circuit 200 includes a TDC 230 as well as feedback to control delay cells in the TDC 230 . A signal CK DCO to be measured, provided by a digitally controlled oscillator, is provided to D inputs of D-type flip flops 240 - 1 , 240 - 2 , . . . , 240 -N (generally 240 ). A reference clock signal CK REF is provided to a clock doubler 210 that also receives input from a pseudorandom number generator (PRNG) 220 . The reason for the presence of the clock doubler 210 and the PRNG 220 will be apparent shortly. Much as in TDC 100 , the output from the clock doubler 210 is provided to delay cells 250 - 1 , 250 - 2 , . . . , 250 -N (generally 250 ), and successive delay taps are provided to clock inputs of corresponding D flip flops 240 . The output from TDC 230 is an encoded signal representing a jitter between CK DCO and CK REF , and this output is shown in FIG. 2 as emanating from the last flip flop 240 -N for convenience, although it is understood that an encoder (not shown) provides encoding much as in FIG. 1 .
A calibration module 260 , comprising a grouper 262 to process groups of bits, an adder 264 , a low pass filter 266 , and a quantizer 268 , provides a calibration signal based on the encoded output from TDC 230 . A correction module 270 provides N correction signals that are added to the calibration signal at adders 280 - 1 , 280 - 2 , . . . , 280 -N and used to control delay cells, e.g., via principles of variable capacitance. Thus, calibration and correction loops are present in a feedback configuration. The effects of the calibration and correction modules are to reduce phase noise and spurs, respectively. The clock doubler 210 is needed because 50% of available cycles are set aside for calibration. The PRNG 220 is used to inject pseudorandom jitter to improve performance, including by reducing unwanted periodicities.
The calibration loop in circuit 200 collects many input signals (groups of five signals for integration), resulting in a relatively long calibration time. Circuit 200 needs multipliers in correction module 270 , requiring large silicon area in a practical embodiment. Clock doubler 210 and PRNG 220 area also needed, resulting in high power consumption, which decreases performance in terms of noise. Because of the clock doubler 210 and the use of 50% of samples for calibration, the operation speed of circuit 200 is twice the input frequency.
FIG. 3 is a block diagram of another known timing circuit. Circuit 300 is described in Chang et al., “A fractional spur free all-digital PLL with loop gain calibration and phase noise cancellation for GSM/GPRS/EDGE,” IEEE Int. Solid-State Circuits Conf. (ISSCC) Dig. Tech. Papers, pp. 222-23, 598, February 2008. Circuit 300 includes a phase frequency detector and cyclic TDC 310 that receives a reference clock CK REF and a feedback signal CK FB . As part of a phase locked loop, circuit 300 provides a digital loop filter 330 , a digitally controlled oscillator 332 , and a divider 234 that provides the feedback signal CK FB . A sigma-delta modulator 340 is used to randomly change a frequency division value of the divider 234 to reduce spurious noise. Sigma-delta modulators are known in the art and are described at, e.g., U.S. Pat. No. 7,279,990, by Hasegawa, “Sigma-Delta Modulator for PLL Circuits,” which is hereby incorporated by reference herein in its entirety. Sigma-delta modulator 340 receives a numerator value F that is accumulated in a manner that causes the frequency division ratio of divider 234 to vary. A scale factor 370 , which is the ratio of an output clock period to the delay time of a delay cell, is used to update the phase locked loop. The scale factor replaces the calibration loop of circuit 200 for phase noise mitigation. Circuit 300 does not contain a correction loop, resulting in phase noise performance of circuit 300 being worse than that of circuit 200 . With adders 320 , 342 and 350 , delay element 360 , scale factor 370 , and multiplier 380 , the input to the digital loop filter 330 is controlled in a manner that provides some phase noise cancellation. The use of a cyclic TDC, in which the output of a last delay cell feeds back to an input of a first delay cell, reduces the number of delay cells but induces in-band phase noise. The use of a multiplier 380 increases silicon area. The performance of circuit 300 in terms of spurs and phase noise is worse than that of circuit 200 .
It is desirable to employ TDC timing techniques that reduce phase noise and spurs with reduced circuit complexity and increased efficiency.
SUMMARY
An embodiment discloses a timing circuit comprising a time to digital conversion (TDC) circuit, a calibration module, and a correction module. The TDC circuit is configured to provide a timing signal indicative of a timing difference between edges of a periodic reference clock signal and a variable feedback signal. The TDC circuit also is configured to provide a delay signal that is variably delayed relative to the reference clock signal. The calibration module is configured to receive the delay signal and a second feedback signal and provide a calibration signal to increase and decrease a total delay of the TDC circuit. The total delay of the TDC circuit is based on a time delay of the calibration signal plus a time delay of a correction signal. The correction module is configured to receive the timing signal and provide the correction signal. The correction module minimizes harmonic spurs in a frequency response of the timing signal by operating at a frequency of the reference clock signal.
The timing circuit may also include a digital loop filter (DLF), a digitally controlled oscillator (DCO), a divider, and a counter. The DLF is configured to provide a digital control signal based on the timing signal. The DCO is configured to tune a frequency of an output clock signal based on the digital control signal. The divider is configured to divide the output clock signal in frequency by an integer M or an integer M+1 and provide a divided signal that feeds back to the TDC circuit as the first feedback signal and that feeds back to the calibration module as the second feedback signal. The counter is configured to accumulate the first feedback signal and provide an increment signal. The increment signal causes the divider to divide by M+1 instead of M in an event that an accumulated sum of the first feedback signal exceeds a predetermined threshold.
Another embodiment discloses a method of controlling timing signals. A reference clock signal and first and second feedback signals are received. The reference clock signal is delayed via N delay cells to provide a delay signal. A timing signal is generated at a frequency of the reference clock signal. The timing signal is indicative of a timing difference between edges of the reference clock signal and of the first feedback signal. Delay cells are adjusted based on the delay signal, the second feedback signal, and the timing signal to calibrate a total delay of the delay cells and to reduce mismatch among delay cells.
The method may also include generating a digital control signal based on the timing signal via a low pass filtering operation. A frequency of an output clock signal is tuned based on the digital control signal. The output clock signal is divided in frequency by an integer M or an integer M+1 to provide a divided signal, which is fed back as the first and second feedback signals. The first feedback signal is accumulated, and the output clock signal is divided in frequency by M+1 in an event the accumulated first feedback signal exceeds a predetermined threshold.
The construction and method of operation of various embodiments, however, together with additional advantages thereof will be best understood from the following descriptions of specific embodiments when read in connection with the accompanying figures.
BRIEF DESCRIPTION OF THE DRAWINGS
The following will be apparent from elements of the figures, which are provided for illustrative purposes and are not necessarily to scale.
FIG. 1 is a block diagram of a known TDC in a Vernier delay line configuration.
FIG. 2 is a block diagram of a known timing circuit.
FIG. 3 is a block diagram of another known timing circuit.
FIG. 4 is a block diagram of a timing circuit in accordance with an exemplary embodiment.
FIG. 4A is a block diagram of a delay cell using tri-state buffers.
FIG. 5 is a block diagram of a calibration module in accordance with an embodiment.
FIG. 6 is a block diagram of a correction module in accordance with an exemplary embodiment.
FIG. 7 is a block diagram of an accumulator in accordance with an exemplary embodiment.
FIG. 8 is a block diagram of a comparator and a register in accordance with an exemplary embodiment.
FIG. 9 is a block diagram of a phase locked loop in accordance with an exemplary embodiment.
FIG. 9A is a block diagram of a counter used with a divider for fractional variation in accordance with an exemplary embodiment.
FIG. 10 is a block diagram of a digital loop filter in accordance with a phase locked loop embodiment.
FIG. 11 is a flow diagram in accordance with an exemplary embodiment.
DETAILED DESCRIPTION
FIG. 4 is a block diagram of a timing circuit in accordance with an exemplary embodiment. Circuit 400 includes a time to digital conversion (TDC) circuit 410 , a calibration module 420 for phase noise reduction, and a correction module 430 for spur reduction. Calibration module 420 and correction module 430 are arranged in feedback configuration to provide calibration and correction loops that can be implemented with simpler circuits than those found in prior art systems. As a result, silicon area and power are saved, and performance in terms of phase noise and spurs is increased relative to the prior art.
TDC circuit 410 includes a plurality of latches 412 configured to switch values of a feedback signal CK DIV based on a reference clock signal CK REF . Specifically, in an example where the latches are D-type flip flops, CK REF is provided to a delay line comprising delay cells 414 - 1 , 414 - 2 , 414 - 3 , . . . , 414 -N (generally 414 ), each of which may be a pair of inverters or composed of other suitable delay elements as known in the art. In an embodiment, N is 16, although other values may be used as well. Delay taps from delay cells 414 are provided to clock edges of the flip flops 412 . An output of delay cell 414 -N, referred to as DCDL OUT because it is the variably delayed output of a digitally controlled delay line, corresponds to CK REF delayed by one period of CK REF when calibration is achieved as described further below. Delay cells 414 are adjusted (increased or decreased in delay) based on signals from calibration module 420 and correction module 430 that are summed at adders 460 - 1 , 460 - 2 , 460 - 3 , . . . , 460 -N (generally 460 ), which may be implemented as multiple adders or as a single adder 460 . CK DIV may be coupled to a delay line, e.g., in a Vernier delay line configuration (not shown) as known in the art. TDC circuit also includes an encoder (not shown) that encodes a timing signal 415 indicative of a jitter of CK DIV relative to CK REF . Timing signal 415 may be a P-bit signal, where N=2 P . Delay cells 414 may be implemented using tri-state buffers known in the art, e.g., as described in Park et al., “All-Digital Synthesizable UWB Transmitter Architectures,” Proc. of the 2008 IEEE Int. Conf. on Ultra-Wideband (ICUWB2008), Vol. 2, p 30, 2008. FIG. 4A is a block diagram of a delay cell using tri-state buffers. Delay cell 414 - i may be any of the delay cells 414 in FIG. 4 . Delay cell 414 - i includes a buffer 416 and P tri-state buffers 418 - 0 , . . . , 418 -P ( 418 generally) coupled in parallel. The tri-state buffers 418 receive respective enable inputs from respective bits of the timing signal 415 . When turned off, the output of each tri-state buffer 418 is high-impedance (‘Z’), thereby switching to increased delay. Conversely, when a tri-state inverter 418 is turned on, delay time is decreased. Thus, delay between nodes IN and OUT may be tuned by P bits of the timing signal 415 . Calibration module 420 receives DCDL OUT and CK DIV1 , which is CK DIV shifted in time. CK DIV is a variable feedback signal provided by a phase locked loop, and the feedback signal arrives at different times at different portions of circuit 400 . Therefore, it is convenient to refer to CK DIV as a first feedback signal and CK DIV1 as a second feedback signal, as these are the same signal arriving at different times at different locations.
Calibration module 420 includes a phase detector 422 and a counter 424 , and the resulting calibration signal 425 is provided to each of the adders 460 . Correction module 430 receives the timing signal 415 . An array of accumulators 432 processes the timing signal to provide accumulation signals 433 to an array of comparators 434 . Comparators 434 provide comparison signals 435 to an array of registers 436 , which store the comparison signals and provide N correction signals 437 . Accumulation signals 433 , comparison signals 435 , and correction signals 437 may respectively be provided as multiple signals (as shown in FIG. 4 ) or as single signals, as is known in the art. The N correction signals 437 are provided to corresponding adders 460 to adjust different delay cells 414 differently so as to reduce delay mismatch among the delay cells 414 .
FIG. 5 is a block diagram of a calibration module in accordance with an embodiment. Calibration module 420 includes a phase detector 422 and a counter 424 as shown in FIG. 4 . The phase detector may be a latch, e.g., a D-type flip flop 422 . DCDL OUT is coupled to a D input of the flip flop 422 , and CK DIV1 is coupled to a clock input. Phase detectors employing flip flops are known in the art and are described at, e.g., U.S. Pat. No. 4,593,253 by McCabe et al., “Flip-Flop Phase Detector Circuit for Phase Locked Loop,” and at U.S. Pat. Pub. No. 2009/0041172 by Kim et al., “Phase Detection Circuit,” both of which are hereby incorporated by reference herein in their entirety. Phase detector 422 compares the phase of inputs DCDL OUT and CK DIV1 . If the phase of DCDL OUT leads CK DIV1 , flip flop 422 provides a Q output at a high level. If the phase of DCDL OUT lags CK DIV1 , flip flop 422 provides a Q output at a low level. The Q output from flip flop 422 is provided to an adder 526 , which provides a multi-bit output to a latch 527 , e.g., to a D input of a flip flop 527 . CK DIV1 is coupled to a corresponding clock input. A Q output of flip flop 527 is fed back to adder 526 , so that counter 424 accumulates the output of phase detector 422 . The accumulated multi-bit output is provided as calibration signal 425 , which is used to adjust a delay of each delay cell 414 . When the calibration loop is locked, the signals DCDL OUT and CK DIV1 are in phase, and the total delay time is equal to the phase difference between CK DIV and CK DIV1
FIG. 6 is a block diagram of a correction module in accordance with an exemplary embodiment. Multi-bit timing signal 415 is provided to each accumulator 432 - 1 , 432 - 2 , . . . , 432 -N (generally 432 ) in the array of accumulators 432 . The i th accumulator 432 - i , with i ranging between 1 and N, inclusive, also receives a constant value i−1. The output from each accumulator 432 - i is provided to a corresponding comparator 434 - i among comparators 434 - 1 , 434 - 2 , . . . , 434 -N (generally 434 ). The i th comparator 434 - i , with i ranging between 1 and N, inclusive, also receives a constant value i−1, and compares the value received from accumulator 432 - i with this constant value. Registers 436 - 1 , 436 - 2 , . . . , 436 -N (generally 436 ) store the comparison outputs from corresponding comparators 434 . Outputs from registers 436 are provided as corresponding correction signals 437 - 1 , 437 - 2 , . . . , 437 -N (generally 437 ). Details of accumulators 432 , comparators 434 , and registers 436 are provided below.
FIG. 7 is a block diagram of an accumulator in accordance with an exemplary embodiment. Accumulator 432 - i shown in FIG. 7 may be any of the N accumulators 432 . Timing signal 415 and a constant value i−1 are added at adder 710 , with the result provided to a logic gate 720 . In an embodiment, each bit of the output of adder 710 is fed to an input of a gate 720 that effects a logical NOR operation. An output of gate 720 is coupled to an input of an adder 730 , an output of which is coupled to a data input of a latch 740 , e.g., to a D input of a flip flop 740 . CK DIV is coupled to a clock input of flip flop 740 . A Q output of flip flop 740 is fed back to adder 730 and also provided as accumulation signal 433 - i , so that accumulator 432 - i is configured to accumulate the outputs of the TDC circuit 410 . In an embodiment, adder 710 is a subtractor, i.e., one of the inputs is negated prior to addition. Accumulator 432 - i increments an accumulated value if each input to gate 720 is at a low level (‘0’). When the value of the timing signal 415 is equal to the constant value i−1, the output of the adder 710 is zero, and the output of NOR gate 720 is at a high level. Thus, the accumulator 432 - i is increased by 1. Therefore, the distribution of timing signal 415 is recorded in accumulator 432 - i , similar to a histogram.
FIG. 8 is a block diagram of a comparator and a register in accordance with an exemplary embodiment. Comparator 434 - i shown in FIG. 8 may be any of the N comparators 434 . Accumulation signal 433 - i is compared to constant value i−1 using conventional techniques, e.g., an adder 810 configured to subtract i−1 from accumulation signal 433 - i and provide a resulting sign bit. The sign bit is coupled to an input of an adder 820 , a multi-bit output of which is coupled to a data input of a latch 830 , e.g., to a D input of a flip flop 830 . A clock input of flip flop 830 is not shown in FIG. 8 for convenience but may be CK DIV . An output of flip flop 830 is fed back to adder 820 and is also provided as correction signal 437 - i . Thus, comparator 434 - i compares the output from accumulator 432 - i with a constant value i−1, and register 436 - i records the output of the comparator.
FIG. 9 is a block diagram of a phase locked loop in accordance with an exemplary embodiment. Phase locked loop 900 , which may be used in frequency synthesizer applications and the like, comprises TDC circuit 410 , calibration module 420 , correction module 430 , and adder 460 described above, as well as additional elements described below. TDC circuit 410 receives an input clock signal CK IN , which may be the reference clock signal CK REF of FIG. 4 , and a feedback signal CK DIV . TDC provides a timing signal 415 , which is labeled TDC[3:0] in FIG. 9 to indicate that the timing signal 415 may be 4 bits when N=16 delay cells are used as in FIG. 4 .
Timing signal 415 is provided to a digital loop filter 920 via an adder 910 , which enables the timing signal 415 to be modified by a cancellation loop as described further below. Digital loop filters (DLFs) are known in the art and perform analogous processing for digital phase locked loops (PLLs) as analog loop filters perform in analog PLLs. For example, a DLF is described in detail at U.S. Pat. Pub. No. 2009/0302958 by Sakurai et al., “Digitally Controlled Oscillator and Phase Locked Loop Circuit Using the Digitally Controlled Oscillator,” hereby incorporated by reference herein in its entirety. Functional details of a DLF in accordance with an embodiment are provided further below in the context of FIG. 10 . DLF 920 provides control signals to tune a digitally controlled oscillator (DCO) 930 .
DCOs are known in the art for providing analogous functionality for digital PLLs as voltage controlled oscillators provide for analog PLLs and are described at, e.g., U.S. Pat. No. 5,727,038 by May et al., “Phase Locked Loop Using Digital Loop Filter and Digitally Controlled Oscillator,” which is hereby incorporated by reference herein in its entirety. DCO 930 adjusts the frequency of an output signal CK OUT so that clock frequencies may be matched (locked) by the phase locked loop 900 . DCO 930 may be implemented with nonlinear capacitors, active inverter stages, or other conventional DCO techniques as known in the art and described at, e.g., U.S. Pat. Pub. No. 2010/0013532 by Ainspan et al., “Phase-Locked Loop Circuits and Methods Implementing Multiplexer Circuit for Fine Tuning Control of Digitally Controlled Oscillators,” hereby incorporated by reference herein in its entirety. CK OUT is divided in frequency by a divider 940 , which divides by an integer M or M+1. Such variable division is known in the art of fractional-type PLLs and is described at, e.g., U.S. Pat. Pub. No. 2004/0223576 by Albasini et al., “Fractional-Type Phase Locked Loop Circuit with Compensation of Phase Errors,” hereby incorporated by reference herein in its entirety.
As is known in the art, providing fractional division enables greater accuracy and resolution for timing applications. A counter 960 provides an increment signal that is either 0 or 1 and that is added to constant integer value M at adder 950 to determine whether divider 940 divides by M or M+1. A counter 960 for fractional-type PLLs is known in the art and described at, e.g., U.S. Pat. No. 7,279,990 by Hasegawa. FIG. 9A is a block diagram of an example implementation of counter 960 . Referring to FIG. 9A , a numerator value F is accumulated using an accumulator 962 comprising adder 964 and flip flop 966 based on clock signal CKDIV. The most significant bit of the Q output of flip flop 966 is provided to another flip flop 967 and to an inverter 968 . An output of an AND gate 969 coupled to inverter 968 and flip 967 at its inputs is provided to divider 940 . In other words, when the accumulated value exceeds a denominator value (modulo value) corresponding to a predetermined threshold, an overflow condition is met, and the divisor is incremented by one to M+1. In an embodiment, the output of counter 960 is provided to a cancellation loop, illustrated depicted in FIG. 9 with a multiplier 970 corresponding to multiplier 380 of FIG. 2 , to further reduce phase noise.
The cancellation loop reduces phase noise similar to the cancellation loop in timing circuit 200 . In the following discussion, reference is made to elements of timing circuit 200 in FIG. 2 , although it should be understood that such elements are implemented in embodiments of the present subject matter as described below. The cancellation loop cancels the phase error between CK IN and CK DIV if the divisor is changed, which occurs during fractional variation for a fractional PLL. The counter 960 , which controls the divisor, can predict the phase error. For example, if an average divisor is 1.25 (fractional part=0.25), the divisor may be varied as follows: 1, 1, 1, 2 to achieve a cumulative effect of 5/4=1.25, i.e., the output of counter 960 over time (i.e., signal DSM as in FIG. 3 ) may be 0, 0, 0, 1 (to increment the divisor). The numerator value F is 0.25, 0.25, 0.25, and 0.25 in comparison. Regarding phase error, CK IN may develop a lag at each iteration, e.g., may be in phase with CK OUT during a first iteration, may trail CK OUT by 0.25 periods of CK OUT after one iteration, may trail CK OUT by 0.5 periods after another iteration, may trail CK OUT by 0.75 periods after another iteration, and may be in-phase again after another iteration. Subtracting DSM from F as at adder 342 yields cancellation factors of 0.25, 0.25, 0.25, −0.75. Adding these cancellation factors to the phase error described above yields a sum term of 0.25, 0.5, 0.75, 0, i.e., the phase error is canceled. Thus, this sum term multiplied by a scale factor equals the phase error, where the scale factor is the ratio between output period and TDC resolution (which is the delay time of a delay cell).
FIG. 10 is a block diagram of a digital loop filter (DLF) in accordance with a phase locked loop embodiment. DLF 920 provides a digital output that is used as a control signal to frequency tune DCO 930 , as is known in the art. Functionally, DLF 920 performs a low pass filtering operation as shown in FIG. 10 , and DLF 920 may be implemented in various ways known to one of ordinary skill in the art to achieve such functionality. An input signal 1005 may be represented as x[n]. Multipliers 1010 , 1020 , adders 1030 , 1050 , and delay element 1040 may be configured as shown in FIG. 10 to provide an output signal y[n]=βx[n]+α(x[n]+x[n−1]). Low pass filtering smooths the inputs to the DCO, which is beneficial due to digitization effects, as is known in the art. Thus, DLF 920 provides equivalent functionality as a series resistor-capacitor (RC) circuit for low pass filtering.
FIG. 11 is a flow diagram in accordance with an exemplary embodiment. After process 1100 begins, a reference clock signal and first and second feedback signals are received ( 1110 ). The reference clock signal is delayed ( 1020 ) via N delay cells to provide a delay signal. A timing signal is generated ( 1030 ) at a frequency of the reference clock signal. The timing signal is indicative of a timing difference between edges of the reference clock signal and of the first feedback signal. Delay cells are adjusted ( 1040 ) based on the delay signal, the second feedback signal, and the timing signal to calibrate a total delay of the delay cells and to reduce mismatch among delay cells. Although process 1100 is shown as subsequently ending in FIG. 11 , it should be understood that process 1100 may continue in iterative format in accordance with the principles of phase locked loops to provide continual timing adjustments.
Various embodiments find wide application in communications systems, e.g., in Bluetooth and wireless LAN systems. Advantageously, various embodiments provide timing circuitry with reduced circuit complexity relative to the prior art. No multipliers are needed in the correction loop, saving circuit area and reducing power consumption. Similarly, pseudorandom number generators and clock doubling circuits are not needed, resulting in additional space and power savings. Calibration using only two inputs is faster than prior art calibration techniques that group greater than two (e.g., five) input signals together, and there are no input duty cycle restrictions unlike in prior art techniques that reserve, e.g., half of all samples exclusively for calibration. Various embodiments use simple circuit components, e.g., phase detectors, counters, accumulators, comparators, and registers, with underlying switching provided by latches, e.g., D-type flip flops.
Various embodiments have been implemented with success. The total die area can be made at least as small as 1.4 mm in length by 0.8 mm in width, with the area of TDC and digital logic circuitry being about 0.025 mm 2 in accordance with a 65 nm CMOS process. Conventional techniques typically require an area of greater than 0.1 mm 2 for TDC and digital logic circuitry. Various embodiments accommodate fast calibration in about four input clock cycles, compared to greater than twenty input clock signals in prior art implementations that group multiple input signals.
Table 1 lists performance results associated with noise performance of various embodiments.
Divisor
40 (integral)
40 + 1/64
Case
Add
Add
cancellation
cancellation and
Conventional
Conventional
loop
calibration loops
DCO code
6
107
9
4
variation
Table 1 shows DCO code variation for various cases, where less variation in the digital code is better, indicative of tighter timing control. Table 1 shows performance for integral clock division (with division by 40) and fractional division by 40+1/64. Conventionally, code variation of 107 is exhibited with fractional operation, which is worse than code variation of 6 with integral operation. With a cancellation loop alone, code variation is reduced to 9, and with cancellation and calibration loops in accordance with various embodiments, code variation is reduced to 4. Thus, phase noise is reduced by 20 log(107/4)=28.55 dBc/Hz by the various disclosed embodiments. Power consumption is less than 2 mW with the various embodiments. Additionally, the use of a correction loop in various embodiments mitigates undesirable spurs. Thus, various embodiments advantageously provide superior performance in terms of phase noise and spurs relative to the prior art, provide increased efficiency in terms of power, area, and speed, and provide reduced circuit complexity.
The above illustrations provide many different embodiments for implementing different features. Specific embodiments of components and processes are described to help clarify the invention. These are, of course, merely embodiments and are not intended to serve as limitations beyond those described in the claims.
Although embodiments are illustrated and described herein in one or more specific examples, embodiments are nevertheless not intended to be limited to the details shown, since various modifications and structural changes may be made therein without departing from the spirit of the embodiments and within the scope and range of equivalents of the claims. | Methods and apparatuses for time to digital conversion (TDC) are disclosed. A timing circuit comprises a TDC circuit, a calibration module, and a correction module. The TDC circuit is configured to provide a timing signal indicative of a timing difference between edges of a periodic reference clock signal and a variable feedback signal. The TDC circuit is also configured to provide a delay signal that is variably delayed relative to the reference clock signal. The calibration module is configured to provide a calibration signal to increase and decrease a total delay of the TDC circuit based on a time delay of the calibration signal plus a time delay of a correction signal. The correction module, which is configured to receive the timing signal and provide the correction signal, minimizes harmonic spurs in a frequency response of the timing signal by operating at a frequency of the reference clock signal. | 6 |
FIELD OF THE INVENTION
The present invention relates to a method and a keyboard for inputting Chinese characters, which can input both simplified Chinese characters and their original complex forms.
BACKGROUND OF THE INVENTION
So far there are many methods for inputting Chinese characters, for example, Five-Stroke Character Form Code, Nature Code, etc. Most of the stroke-form codes and the combination codes of phoneme and stroke-form are difficult to learn and to bear in mind. The crucial question is that they are limited in the encoding method using radicals which are structural components of Chinese characters, so it is difficult for them to avoid the following shortcomings:
1. There are many, up to hundreds of, encoding elements. For example, Five-Stroke Character Form Code has more than 190 encoding elements, Nature Code has more than 250 encoding elements, Four-stroke Phoneme And Stroke-form Code has more than 440 encoding elements, both of Two-stroke Phoneme And Stroke-form Code and Zheng Code have up to 540 encoding elements, and Taiji Code has 152 encoding elements only in so far as the elements of pictographic character elements and mere character elements for exemplification(it is difficult to count up the actual total number of its encoding elements). Because of the large number of encoding elements, users have to remember a large amount when they learn to use these encoding methods.
2. The encoding rules are very complex. Since there are many encoding elements, it is not clarified how a character can be broken down into encoding elements. For example, Chinese character "" can be either broken down into "" or "". The rules for breaking down Chinese characters are very complicated and the theories thereof are not easy to understand. The rules for encoding and the corresponding keyboard arrangements of the encoding elements are also very complicated.
3. The codes are long. At present all the input methods which have lower rate of duplication codes and which can realize blind typing(typing without looking at the display) are four-code input methods, and the long codes cause the increasing of thinking levels for encoding a character and increasing the number of key-striking times, as well as the slowing down of input speed.
4. Their applications are limited in scope. Normally, the encoding methods now available are applicable only to a small collection of Chinese characters, e.g. 6763 Chinese characters in Chinese National Standard GB2312-80, but not applicable to a collection with 20,902 Chinese characters in the international standard ISO-10646 for China, Japan and Republic of Korea. When applying to the ISO-10646 Chinese character collection, it is difficult to encode the phoneme codes in the combination codes of phoneme and stroke-form because there are a large number of Chinese characters, which people do not know their pronunciation, in this large character collection, and it is also very difficult to avoid the high rate of duplication codes or the increase of code length when using mere stroke-form codes, therefore it causes inconvenience to the users.
SUMMARY OF THE INVENTION
The object of the present invention is to provide a method and a keyboard for inputting Chinese characters based on the two-stroke forms and two-stroke symbols which are used as basic codes for encoding Chinese characters. It is easy to learn to use and can be inputted with high speed, therefore it overcomes the disadvantages of the prior arts.
The keyboard of the present invention is realized by setting up keys corresponding to 25 two-stroke form code elements and 25 to 28 two-stroke symbol code elements and a code ending key on a standard keyboard.
Said two-stroke form code elements include: ##STR1##
The above two-stroke form code elements are arranged in three lines, with each line has at most 10 elements. The 5 elements beginning with a "horizontal" stroke are marked on the left 5 keys of the middle line; the 5 elements beginning with a "vertical" stroke are marked on the right 4 keys of the middle line, and the second right key of the lower line; the 5 elements beginning with a "left-falling" stroke are marked on the left 5 keys of the upper line; the 5 elements beginning with a "right-falling" stroke are marked on the right 5 keys of the upper line; and the 5 elements beginning with a "turning" stroke are marked on the left 5 keys of the lower line.
The code elements of said two-stroke symbols are:
If necessary, three code elements can be added to the code elements of said two-stroke symbols as follows:
Said two-stroke symbol code elements are arranged on corresponding keys according to the principle of minimizing the rate of duplication codes.
The Chinese character inputting method of the present invention includes following steps:
1. composing 25 two-stroke form code elements according to the basic strokes which construct Chinese characters, that is:
classifying the single strokes which construct Chinese characters into five types: horizontal, vertical, left-falling, right-falling and turning, which can be symbolized as:
;
combining every two of the above five strokes together to compose two-stroke form code elements, the total number of which are 5*5=25, and which are provided as follows: ##STR2## 2. selecting following 25 two-stroke symbol code elements among frequently used basic structural components of Chinese characters:
If necessary, the following additional elements can be further selected:
;
3. performing operations for inputting Chinese characters in following 3 manners:
i. for a character of four strokes or fewer, extracting the first and the last code elements of the character according to the handwriting sequence; for a single block character of 5 strokes or more, extracting the first, the second and the last code elements of the character; for a character which is made up of separated blocks and has 5 strokes or more, dividing it into two blocks, and extracting only the first code elements from the beginning block and the first and the last code elements from the end block, then striking the keys corresponding to these code elements; if the number of the code elements extracted is less than 3, striking the code ending key thereby completing the input of this Chinese character.
ii. for a character of four strokes or fewer, extracting the first and the last code elements of the character according to the handwriting sequence; for a single block character of 5 strokes or more, extracting the first, the second and the last code elements of the character; for a character which is made up of separated blocks and has 5 strokes or more, dividing it into two blocks, and extracting the first and the last code elements from each block, then striking the keys corresponding to these code elements. If the number of the code elements is less than 4, striking the code-ending key thereby completing the input of this Chinese character.
iii. for a character of 4 strokes or fewer, extracting the first letter from its standard phonetic alphabet combination, and the first code element of the character according to the handwriting sequence; for a character of 5 strokes or more, extracting the first letter of the standard phonetic alphabet combination, the first code element and last code element of this character, then striking the keys corresponding to these letters and code elements. If the number of the code elements is less than 3, striking the code-ending key thereby completing the input of this Chinese character.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a schematic diagram of the keyboard on which 25 two-stroke forms and 25 two-stroke symbols are marked according to the present invention;
FIG. 2 is a schematic diagram of the keyboard on which 25 two-stroke shapes and 28 two-stroke symbols are marked according to the present invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
The embodiments of the present invention will be described in detail with reference to the drawings hereinafter.
Chinese characters are made up of about 30 kinds of single strokes, which are classified in the present invention into five types: horizontal, vertical, left-falling, right-falling and turning, and symbolized as:
Every two of said five types of stroke are combined together to form a code element of the two-stroke form, thus there are altogether 5*5=25 two-stroke form code elements, which are shown as follows: ##STR3##
In order to enhance the efficiency for inputting Chinese characters and decrease the duplication codes, 25 two-stroke symbols are provided in the present invention as code elements. All the 25 two-stroke symbols are selected among the traditional Chinese character components and combinations of frequently used strokes by means of a number of tests. Using them can decrease the rate of duplication codes effectively. The actual strokes of a two-stroke symbol may have more than two stroke, but they all are deemed as having two stokes in the present invention, thus being so called two-stroke symbols. For example, Chinese character "" is defined as a two-stroke symbol, which has 4 strokes in reality, according to the present invention, therefore Chinese character "" is deemed as having 4 strokes. The purpose is to make the encoding rules simple, clear, easy to learn and to bear in mind. These 25 two-stroke symbols are:
According to different requirements of different object characters, some changes may be made on the basis of these 25 two-stroke symbols, for example, the following 3 code elements may be added:
Said 25 two-stroke forms and 25 two-stroke symbols are the code elements which are selected by the present invention for inputting Chinese characters. They are marked on the surfaces of 25 keys, as shown in FIG. 1.
On the basis of the 50 code elements, the present invention provides three kinds of methods for inputting Chinese characters: Four Code Input Method based on Mere Stroke-form (hereinafter referred to as MSFC input method); Three Code Input Method based on Mere Stroke-form (hereinafter referred to as MSTC input method); and Three Code Input Method based on the Combination Of Phoneme and Stroke-form (hereinafter referred to as CPSTC input method), wherein as the most important one of the three input methods, the MSFC input method comprises the following steps: dividing a Chinese character into two half-block characters; extracting the first and the last code elements from both half-block characters, totally 4 code elements, according to the handwriting sequence, then striking the keys corresponding to these 4 code elements, thereby completing the input of said Chinese character.
In the present invention, during extracting code elements from a character or a half-block character, the principle of "two-stroke symbol comes first, two-stroke form second" must be abided by. That is to say, if a two-stroke symbol can be extracted, this two-stroke symbol, instead of the two-stroke form, must be extracted. Only if the strokes of a part of a Chinese character do not form any two-stroke symbol, can 2 single strokes thereof be extracted to form a two-stroke form code element. For example, the first code element of Chinese character "" must be a two-stroke symbol "", instead of a two-stroke form "", because the two-stroke symbol "" is formed from the first stroke of the character, On the other hand, the first code element of Chinese character "" must be "", instead of "", because "" is not a two-stroke symbol defined in the present invention. The correct sequence of handwriting must be followed when code elements are extracted.
Chinese characters are classified into two types in MSFC or MSTC input method. One is called single-block characters, the other is called separated-block characters. When a separated-block character is inputted, it must be divided into two parts, the first one is called "the beginning block", the second one is called "the end block".
Separated-block characters are broken down in following manner:
i. For a character of Up-down construction, the group of strokes which are first completed from left to right in handwriting sequence is referred to as the beginning block, and the residual strokes form the end block, e.g., for Chinese character "", the first group of strokes which are written from left to right is "", therefore "" is the beginning block, and "" is the end block.
ii. For a character of Left-right construction, the group of strokes which are first completed from top to bottom in handwriting sequence is referred to as the beginning block, and the residual strokes form the end block, e.g., for character "", the first group of strokes which are written from top to bottom is "", therefore "" is the beginning block, and "" is the end block.
iii. For a character of Embracing construction, which means a group of strokes embracing another group of strokes from two, three or four directions of the character, and can be divided into a embracing block and a embraced block, the group of strokes which are completed first in handwriting sequence is referred to as the beginning block, the residual strokes form the end block. For example, for character "", "" is the block which are first written, therefore it is the beginning block, and the rest part "" is the end block.
iv. Characters other than the above three kinds of constructions are single-block characters.
Said MSFC, MSTC and CPSTC are names of three kinds of input methods of Chinese character in the present invention, wherein "Four Code" or "Three Code" does not represent the actual times of key-striking for each character, but means that at most four codes or three codes are provided for inputting a character. The MSFC and the MSTC inputting method will be described in detail below.
i. for a character of 4 strokes or fewer, extracting the first and the last code elements in handwriting sequence, and striking the keys corresponding to these elements successively.
ii. for a single-block character of 5 strokes or more, extracting the first, the second and the last code elements, and striking the corresponding keys successively.
iii. for a separated-block character of 5 strokes or more, dividing it into two blocks, extracting the first and the last code elements from each block, totally 4 code elements (for MSFC input method) or extracting only the first code element from the beginning block and the first and the last code elements from the end block, totally 3 code elements(for MSTC input method), then striking the corresponding keys successively.
For the above-mentioned MSTC input method, the code-ending key shall be struck when the number of the code elements is less than 3. For the above-mentioned MSFC input method, the code-ending key shall be struck when the number of the code elements is less than 4.
For example, the selected code elements of character "" are ", , , " (for MSFC) or ", , " for (MSTC).
Using CPSTC input method according to the present invention, a Chinese character is inputted in a manner as follows:
a) for a character of 4 strokes or fewer, extracting the first letter of the standard combination of the phonetic alphabet and the beginning code elements of the character, then striking the corresponding keys and the code-ending key successively.
b) for a character of 5 strokes or more, extracting the first letter of the standard combination of the phonetic alphabet, the beginning code element and the end code element, then striking the corresponding keys successively.
For example, the selected code elements of character "" are "B, , " in the CPSTC input method.
The MSFC input method is mainly used for encoding and inputting the characters of a large Chinese character collection including several ten thousand of characters.
The MSTC or CPSTC are mainly used for encoding and inputting commonly used Chinese characters the number of which is less than ten thousand.
The table below shows preferred embodiments of the input method according to the present invention based on the 25 two-stroke forms and the 25 two-stroke symbols.
Preferred embodiments of the input method using 25 two-stroke forms and 25 two-stroke symbols:
__________________________________________________________________________ CorrespondingChineseInput Number Blocks Extracting code keys of AlphabetCharacterMethod of Strokes Construction divided elements Keyboard__________________________________________________________________________CPSTC MSTC MSFC <4 XF FL FLCPSTC MSTC MSFC =4 MT TA TACPSTC MSTC MSFC =4 LK KK KKCPSTC MSTC MSFC =5 single block WGW GKW GKWCPSTC MSTC MSFC >5 single block WTW THW THWCPSTC MSTC MSFC >5 seperated- blocks (Up-down construction) BTA TTA TSTACPSTC MSTC MSFC >5 seperated blocks (Left-right construction) BJW JRW JFRWCPSTC MSTC MSFC >5 seperated blocks (Embracing construction) BPJ PMJ PDMJCPSTC MSTC MSFC >5 seperated blocks (Up-down construction) JKM KGM KKGM__________________________________________________________________________
With 25 two-stroke forms and 25 two-stroke symbols as code elements, the input method of the present invention are applicable to small Chinese character collection of 6,763 characters of Chinese national standard GB2312-80.
With 25 two-stroke forms and 28 two-stroke symbols as code elements, the input method of the present invention are applicable not only to the large character collection of 20,902 Chinese characters of ISO-10646, which includes simplified Chinese characters, their original complex forms, Japanese and Korean characters, but also to the large character collection of 60 thousand Chinese characters.
A special keyboard arrangement suitable for the input methods according to the present invention is provided.
The keyboard comprises at least 25 keys corresponding to the code elements, and a code-ending key. The spacebar of the keyboard shown in the Figures can be used as the code-ending key. These 25 keys are arranged in three lines, with each line has at most 10 keys. 25 two-stroke forms are marked on these 25 keys respectively. The 5 two-stroke forms beginning with a horizontal stroke are marked on the left 5 keys of the middle line. The 5 two-stroke forms beginning with a vertical stroke are marked on right 4 keys of the middle line, and the second right key of the lower line. The 5 two-stroke forms beginning with a left-falling stroke are marked on the left 5 keys of the upper line. The 5 two-stroke forms beginning with a right-falling stroke are marked on the right 5 keys of the upper line. The 5 two-stroke forms beginning with a turning stroke are marked on the left 5 keys of the lower line.
25 to 28 two-stroke symbols are marked on certain keys. Some of the keys are marked with multiple two-stroke symbols, while some of them with none.
The two-stroke form code elements and the two-stroke symbol code elements must be arranged in the keyboard according to the following combination rule: ##STR4## -(Without two-stroke symbol)-(Without two-stroke symbol)
When two-stroke symbol code elements are added, these three code elements are marked on the same key with code element "".
FIGS. 1 and 2 further provide the details of the keyboard in which 25 or 28 two-stroke symbol code elements and 25 two-stroke form code elements are arranged.
The above-mentioned keyboard is the preferred arrangement derived according to the structural features of Chinese characters, and having passed a number of encoding tests, and decreasing the rate of duplication codes greatly.
Because the present invention uses 25 two-stroke forms as the basis for encoding and combined with 25 two-stroke symbols, it breaks through the limit of the encoding method based upon components of Chinese characters, therefore it has following significant advantages as compared with prior arts:
i. The encoding elements are greatly decreased. As code elements, there are only 25 two-stroke forms which are made up of "" and 25 to 28 two-stroke symbols selected from frequently used character components. The amount of symbols which must be remembered is decreased by a factor of 8 to 20. So it is easy to learn and to remember for the operators.
ii. The encoding rules are simple. Because only the beginning and the end strokes or parts of characters are used for encoding, it is simple, clear and overcomes the problems occurred when characters are broken down in the prior arts.
iii. There are fewer codes as compared with prior arts. For small Chinese character collection of less than 10 thousand of characters, only three codes are used for inputting. It is one code fewer than that of prior arts. Using fewer codes cause the decrease of thinking levels for encoding a character and therefore decrease the times of key-striking.
iv. It can be applied more widely. The present invention can apply to encoding of Chinese, Japanese and Korean characters using the same methods and the same code elements. It can also encoding characters in ISO-10646 collection of characters world-wide used and in large collection of Chinese characters which has more than 60 thousand characters.
INDUSTRIAL APPLICABILITY
Because the 25 two-stroke symbols used in the present invention have an ability to greatly decrease the rate of duplication codes, the present invention has very low rate of duplication code. Among 20,902 Chinese characters in international standard ISO-10646, more than 17,000 of them can be directly inputted by MSFC input method of the present invention without having to select from characters represented by same codes. Among 6,763 Chinese characters in Chinese national standard GB2312-80, more than 5,000 of them can be inputted directly by CPSTC input method of the present invention without having to select from characters represented by same codes. In addition, since the default mode that frequently used characters are of priority are used, most of the characters that must be inputted through selection are rarely used words, characters that have to be selected from several characters represented by same codes are rarely met during ordinary inputting. Therefore, the present invention is not only easy to learn, but also can realize blind-typing with very high speed. | The present invention relates to a method and a keyboard for inputting Chinese characters, which can input both simplified Chinese characters and their original complex forms.
The invention defines 25 double strokes of the kind and 25-28 auxiliary roots containing the double strokes as codes for inputting Chinese characters, further, the invention also defines 25 common use words. Three methods for inputting Chinese characters will be disclosed in the invention. In the input method of which 4 simple shape codes will be used for the coding, a word that can be leaved each other may be broken down into 2 blocks and then 2 codes respective of the first and last double strokes or roots containing the double strokes of each block will be taken into the coding. The inputting methods of the invention are simple and easy for studying. | 6 |
[0001]
[0000]
TABLE 0.1
U.S. PATENT DOCUMENTS CITED
6,554,800 B1
April 2003
Nezhadian & Orchard
7,591,801 B2
September 2009
Brauker et al
7,976,492 B2
July 2011
Brauker et al
8,260,393 B2
September 2012
Kamath et al
8,292,810 B2
October 2012
Goode et al
8,346,338 B2
January 2013
Goode et al
8,460,231 B2
June 2013
Brauker et al
8,589,106 B2
November 2013
Engelhardt et al
61/913,962
December 2013
Matthews
8,690,820 B2
April 2014
Cinar & Oruklu
8,784,370 B2
July 2014
Lebel & Starkweather
FIELD OF THE INVENTION
[0002] The present invention relates to the field of closed loop diabetic insulin control using a Continuous Glucose Monitoring (CGM) system and an insulin pump. More specifically, the present invention relates to using a recursive filter for real-time prediction of the blood glucose level toward which a diabetic patient is being forced, after food or insulin intake.
[0000]
TABLE 0.2
OTHER REFERENCES CITED
Diabetes mellitus modeling and
Mathematical
F. Stahl &
short-term prediction based on
Biosciences 217,
R. Johansson
blood glucose measurements.
pp. 101-117
2009
In-Flight Spectral
Journal of
Matthews
Characterization and
Atmospheric and
2009
Calibration Stability
Oceanic Technology
Estimates for the Clouds and
26(9) pp. 1685-1716
the Earth's Radiant Energy
System (CERES).
BACKGROUND OF THE INVENTION
[0003] The following background paragraph makes reference to FIG. 1( a ) with its annotations numbered [ 1 ] to [ 5 ]. Like all systems, the blood glucose level in the human body responds with an infinite time impulse response function to an external forcing. Such forcing upwards can arise after food is broken down to chemical energy (sugar) by the stomach/digestive track[ 1 ]. Downward forcing typically occurs due to an amount of physical work being done by the body's muscles[ 2 ], which also requires the hormone insulin to mobilize or convert the blood sugar to energy[ 3 ]. In nondiabetics, a natural negative feedback mechanism[ 4 ] exists between the pancreas and liver that responds to these forcings as needed. For example an increasing blood sugar content will trigger a release of insulin from the pancreas beta cells, which allows the muscles to mobilize the sugar and convert [ 3 ] it into kinetic energy[ 2 ]. Typically a falling blood sugar will result in the release of glucagon also from the pancreas, which allows conversion of glycogen to glucose in the liver. This is then released into the blood to restore the glucose level[ 5 ], providing the extra energy needed for continued activity. In diabetics this mechanism has failed.
[0004] This background paragraph now makes reference to FIG. 1( b ), with its annotations numbered [ 6 ] to [ 11 ]. In medical cases known as type 1 (or juvenile) diabetics, the pancreas organ no longer produces sufficient insulin or glucagon that triggers glucose creation within the liver[ 6 ]. Without the hormone insulin needed to create energy from sugar, the type 1 diabetic must typically inject artificially produced insulin[ 7 ] so their muscles can make use of the energy from food digestion. This then prevents hyper-glycemia, or glucose from building up in their blood supply, which is the primary cause of serious health problems in later life. Equally challenging are then problems due to the lack of negative feedback[ 6 ] in the opposite direction, that triggers conversion of glycogen to glucose in the liver for release into the blood supply. This means that if the patient injects too much artificial insulin, there is no restoring forcing mechanism to maintain blood sugar at levels needed for human function. This can result in hypo-glycemia, or low blood sugar with might lead to coma and death.
[0005] Type 2 (or adult onset) diabetics typically develop the condition later in life, which is where the body develops a resistance to, or general lack of, the insulin created by the pancreas. This can hence also be considered a perturbation to the body's blood glucose forcing and feedback system, but can often be controlled with use of oral medications. Like type 1 diabetics, such patients would also benefit from added feedback control (e.g. from a closed loop insulin delivery system shown in FIG. 1( b )). As before however, care is needed to ensure too much medication is not delivered because the pancreatic/liver restoration system can also be diminished[ 6 ] in these medical cases.
[0006] As stated the system is summarized by figure FIG. 1 , which details the feedback mechanism that exists in the human body but breaks down in diabetics. The solution that is needed is a way to effectively and artificially re-create the natural system of FIG. 1( a ), as shown in FIG. 1( b ). This requires an algorithm[ 8 ] that takes data from a CGM [ 9 ] and predicts the blood sugar level to which the system is being forced from food digestion or insulin previously injected. This will allow a computer running the algorithm methodology developed herein[ 8 ] to calculate a further insulin dose[ 7 ] calibrated to the patient in question. This shall then restore the blood glucose level to the ideal range (between 80 and 120 mg/dl) in re-creation of the natural system of FIG. 1( a ). It must also be designed to operate safely in a system where no automated sugar increasing restoring feedback is present (i.e. without an equivalent of the pancreas releasing glucagon to restore sugar levels from the liver[ 6 ]). Today it is possible to equip an insulin pump[ 10 ] with a separate glucose chamber[ 11 ] also for injection that would serve this purpose. However the invention must be designed to have a sufficiently sophisticated insulin predictive model, such that the sugar restoration system need only be used in the event of an emergency.
[0007] To do this, both a practical and effective time impulse response of the human blood glucose level and its changes after food and insulin intake must be developed. The time domain response must be of a nature that it can be matched to CGM data in real-time. This is so to allow a computer to make timely predictions of the final sugar level to which the patient is headed (i.e. in the absence of any additional food or insulin injections).
OBJECTS OF THE INVENTION
[0008] It is an initial objective of this invention to design a mathematical representation of the human blood glucose time response to food and insulin intake (e.g. based on FIG. 2( a ) taken from Stahl & Johansson (2009)). This must operate with minimal unknown mathematical variables such that it can be matched in real-time to data received from a CGM device. The matching must allow for different food types with various glucose absorption/conversion rates (e.g. carbo-hydrates vs. protein). Then multiple types of insulin (both fast and slow acting) must be considered, along with how the patient blood sugar will respond in terms of amplitude and time (noting also possible variance depending on environment and exercise etc). To allow the model to be adaptive it will be represented using a recursive filter, which will ease fast matching and prediction of the future state to which the patient is headed.
[0009] Still further, other objects and advantages of the invention with respect to modeling and adapting to the human body will be apparent from the specification and drawings.
SUMMARY OF THE INVENTION
[0010] Time and environment dependant varying responses of the human blood glucose system to food, insulin and exercise must be adapted to. This will be done with a recursive filter based on a mathematical model of time response. Its construction shall use simple exponential functions to match the natures displayed in FIG. 2( a ).
[0011] The invention accordingly comprises the several steps of matching the recursive filter to CGM data in real-time, then calculating an appropriate insulin dose based on past calibration results. This is to be done in iterative steps so to ensure hypo-glycemia is not induced. The relation of the various steps with respect to each of the others will be based on mathematical constants that are determined with high confidence. These also remain subject to change however in the presence of updated data from the various apparatus embodying features of construction (e.g. CGM and insulin pump measurements). The combinations of elements and arrangement of parts that are adapted to affect such steps will be exemplified in the following detailed disclosure, and the scope of the invention will be indicated in the claims.
BRIEF DESCRIPTION OF THE DRAWINGS
[0012] For a more complete understanding of the invention, reference is made to the following description and accompanying drawings, in which:
[0013] FIG. 1 ( a ) Natural Feedback system in human body where pancreas controls blood sugar during eating and exercise. (b) Closed loop insulin delivery system in diabetic using a control algorithm[ 8 ] (developed herein), CGM[ 9 ], insulin pump[ 10 ] and emergency glucose supply[ 11 ];
[0014] FIG. 2 ( a ) Left: food absorption rates of fast and slow carbohydrates. Right: fast and slow insulin absorption rates—both graphs from Stahl & Johansson (2009). (b) Example exponential model curves for fast & slow food/insulin impulse response functions. (c) Convolution model of human response to food/insulin, where the patient blood sugar level G(t) is the area overlap between the functions F(t) and H(t′−t);
[0015] FIG. 3 ( a ) 2D landscape visualization of blood glucose change rate for three food events of fast carbohydrate at breakfast and dinner (j=1 & 3) and slow carbohydrate at lunch (j=2). (b) 2D landscape visualization of two insulin events caused by breakfast and lunch-time injections (j=4 & 5);
[0016] FIG. 4 Example CGM data and model fit after an insulin event; and
[0017] FIG. 5 Example CGM data and model fit after an insulin event.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0018] This invention considers that the blood glucose system of the human body responds with an infinite time impulse response function to a forcings. These can come from food digested in the stomach combined with an amount of insulin in the blood and must then be considered in conjunction with the present environment (e.g. the amount of exercise currently undertaken). In a diabetic the time t dependent forcing function F(t) is here not necessarily considered a prediction of where the sugar level will eventually go. Without a natural feedback mechanism, it is instead thought of as where the glucose system is trying to go baring intervention from insulin, more food, increased/decreased exercise or simple changes in environment. In practice the time domain impulse response of the patient glucose change rate due to forcing will not be a constant. As stated it may vary with exercise and environment. This algorithm however initially assumes that the function shape is constant and can be represented by a continuous mathematical distribution H(t). Examples of H(t) for different types of both food and insulin are shown in FIG. 2( a ) (from Stahl & Johansson (2009)). This indicates the rate at which either food is converted to blood sugar, or blood sugar converts to energy in the patient. It also illustrates that both food and insulin absorption rates go from zero to a maximum value within around an hour or more, then begin to reduce afterwards. The shapes shown in FIG. 2( a ) are hence continuous with only one zero gradient point, meaning that they could be well represented using a function that is the difference of at least two exponentials, as displayed in Eqn. 1:
[0000]
H
(
t
)
=
Φ
∏
i
=
1
N
(
-
b
i
t
-
-
[
a
i
+
b
i
]
t
)
(
1
)
∫
0
∞
H
(
t
)
t
=
1
(
2
)
[0000] a i & b i are positive and real reciprocal time constants that characterize the typical absorption rate of the patient to food or insulin (i.e. a i =1/τ i , with τ i an absorption time constants, typically around 60 minutes from FIG. 2( a )). Φ is simply a variable that depends on the values of a i & b i making the Eqn. 2 integral equal to one. It helps to initially consider simulation of a situation where a patient eats only a single type of food, with very specific gut absorption properties similar to one of those shown in FIG. 2( a )(left). For the case of this food absorption alone, it is assumed that the function H(t) can be represented using only single values of the a i & b i coefficients (i.e. N=1 in Eqn. 1). The FIG. 2( b ) dashed graph shows the model curve from Eqn. 1, with the values a i =1/200 & b i =1/33.33 minutes −1 respectively.
[0019] Ideally, a fast acting insulin might be manufactured that has exactly equal time response coefficients, but opposite amplitude to the absorption of the food eaten by the patient. This would mean that the effective food/insulin forcing function F(t) would undergo a positive change for food and an equally negative one for a corresponding insulin injection. The resulting rate of change in blood glucose level would be found by the convolution of the impulse response H(t) with the time differential of the forcing function F(t) as in FIG. 2( c ) & Eqn. 3:
[0000]
∂
G
(
t
)
∂
t
=
H
(
t
)
⊗
∂
F
(
t
)
∂
t
(
3
)
[0000] G(t) is therefore the blood glucose level of the patient at time t in mg/dL and the measurement retrieved by a CGM. In the event of an insulin injection or rapid sugar intake at time t k , the rate of change ∂F(t)/∂t could be considered a delta Dirac function A.∂(t−t k ). A is a constant proportional to the amount of insulin injected or food eaten (positive for food as in FIG. 2( c ) and negative for insulin as in FIG. 3( b )). In the case of fast and slow acting insulin types, FIG. 2( a ) (right) shows the rate of change of blood sugar level ∂G(t)/∂t after an injection (e.g. for Humalog or Insulatard insulin types from Stahl & Johansson (2009)).
[0020] The two constant form of this food/insulin impulse response is then found using Eqn. 4 (i.e. dashed curve in FIG. 2( b ) with two exponential time constants a and b because N=1 in Eqn. 1):
[0000] H ( t )=Φ e −bt (1− e −at ) (4)
[0000] Since CGM systems report sugar levels as digital data, it is also convenient to convert continuous functions to the digital time domain for each sample k. Digital time t k is then Δt.k where Δt is the sampling interval of a sensor (typically 5 minutes). A digital time domain version of the impulse response function H(t) for sample k is hence given by Eqn. 5.
[0000] H k =Φe −bΔt.k (1− e −aΔt.k ) (5)
[0000] Design of recursive filters for digital data is significantly simplified if performed in the z domain using the unilateral z transform (where z=e φ and φ is an imaginary number). This takes the form of Eqn. 6, which transforms Eqn. 5 to become Eqn. 7:
[0000]
H
(
z
)
=
∑
k
=
0
∞
H
k
×
z
-
k
=
Φ
∑
k
=
0
∞
[
(
-
b
Δ
t
z
-
1
)
k
-
(
-
(
a
+
b
)
Δ
t
z
-
1
)
k
]
(
7
)
(
6
)
[0000] It is important to note that Eqn. 7 represents an infinite geometric summation. This is convenient when considered that a geometric sum of a series h k =Φr k can be represented as in Eqn. 8 for n→∞:
[0000]
Φ
∑
k
=
0
∞
r
k
=
Φ
1
-
r
∈
r
<
1
(
8
)
[0000] In the case of the human food impulse response of Eqn. 7, there are two terms in the z transform summation with common factors r 1 =e −bΔt z −1 & r 2 =e −(a+b)Δt z −1 :
[0000]
H
k
=
Φ
(
r
1
k
-
r
2
k
)
(
9
)
H
(
z
)
=
Φ
(
1
1
-
r
1
-
1
1
-
r
2
)
=
Φ
(
1
1
-
-
b
Δ
t
z
-
1
-
1
1
-
-
(
a
+
b
)
Δ
t
z
-
1
)
(
11
)
=
Φ
(
-
b
Δ
t
-
-
(
a
+
b
)
Δ
t
)
z
-
1
1
-
(
-
b
Δ
t
+
-
(
a
+
b
)
Δ
t
)
z
-
1
+
-
(
a
+
2
b
)
Δ
t
z
-
2
(
12
)
=
Φ
c
0
z
-
1
1
-
c
1
z
-
1
+
c
2
z
-
2
(
13
)
=
Φ
c
0
z
-
c
1
+
c
2
z
-
1
(
14
)
(
10
)
[0021] The various exponential terms are simplified with the use of the constants c 0 to c 2 . As with both the Fourier and Laplace domains, the resultant z domain glucose level G(z) will be the product of the sugar forcing function F(z) and the human response function H (z):
[0000]
G
(
z
)
=
H
(
z
)
×
F
(
z
)
=
Φ
(
c
0
z
-
c
1
+
c
2
z
-
1
)
F
(
z
)
(
16
)
(
15
)
Φ
=
1
-
c
1
+
c
2
c
0
(
17
)
[0000] where, as before Φ is simply a constant given by Eqn. 17 that ensures the filter has a gain of 1 or that G ∞ =F ∞ .
[0022] The present invention takes advantage of the property of the z transform, that a general function h(z) when multiplied by z u transforms back to the digital time domain as the same original series but simply advanced by u samples (i.e. h k+u ):
[0000]
∑
k
=
0
∞
h
k
+
u
z
-
k
=
h
(
z
)
z
u
(
18
)
F
(
z
)
=
G
(
z
)
z
-
c
1
G
(
z
)
+
c
2
G
(
z
)
z
-
1
Φ
c
0
(
19
)
F
k
=
G
k
+
1
-
c
1
G
k
+
c
2
G
k
-
1
Φ
c
0
(
20
)
F
k
-
1
=
G
k
-
c
1
G
k
-
1
+
c
2
G
k
-
2
Φ
c
0
(
21
)
[0000] Eqn. 16 can be re-arranged to become Eqn. 19, which gives the sugar forcing function F(z) in terms of glucose level G(z). It is then simple to transform this into the digital time domain to give the recursive relationship of Eqn. 20 or 21.
[0023] This analysis is a simplified example that assumes the possibility of a constant and matched food/insulin time response, without instrument noise present. In such a case it would be straightforward to directly use CGM measurements in determining the ultimate sugar level (F k−1 ≈F ∞ ) that the patient is being forced to from Eqn. 21. In theory after eating food, with a perfect prediction of where the patients sugar level is being forced to and knowledge of the effective ‘gain’ g of the insulin, a required insulin dose I is calculated as I=(F ∞ −F T )/g. This would precisely counter the sugar forcing of the food and leave the patient with a final target sugar level of F T (typically desired to be around 100 mg/dL). The insulin gain ‘g’, in sugar units of mg/dL per ml of insulin injected, would be fairly constant but could also depend on environmental conditions to some extent. This example therefore shows how a recursive filter can be used to predict where a physically understood system is being forced to without the presence of instrument noise.
[0024] Building on the instrumental noise free premise given above, further variation and dimension will now be added to the model. This shall make it able to accurately represent real world changes to a patient glucose level when eating food and injecting artificial insulin during a typical day. In addition, actual data from a currently available CGM sensor must be used as the only input for the algorithm's design of insulin delivery amount.
[0025] To do this a discrete ‘food or insulin event’ of type j is considered as in FIG. 3 . Each event j has specific time constant characteristics a ij & b ij , such that its time response is given by Eqn. 22 with normalized characteristics of Eqn. 23:
[0000]
H
j
,
k
=
Φ
j
∏
i
=
1
N
(
-
b
ij
Δ
t
.
k
-
-
[
a
ij
+
b
ij
]
Δ
t
.
k
)
(
22
)
Δ
t
∑
k
=
0
∞
H
j
,
k
=
1
(
23
)
[0026] An event j could be eating breakfast or lunch, then injecting insulin of various types using a syringe or insulin pump (i.e. a bolus). It is expected that there could be dozens (or a number M) of such events during the course of the previous 24 hours. To graphically visualize this, the single dimension of FIG. 2 is expanded upon to two as in FIG. 3 . Here as before there is the dimension of time κ (temporary version of k) and also the j dimension of different food/insulin types or events. The past day can therefore be represented as a series of food/insulin events occurring at digital sample time k f j /k I j , of type j and amplitude A j,k f j /A j,k I j (in mg/dL/minute). The 2D landscape displayed in FIG. 3( a ) hence represents breakfast, lunch and dinner. FIG. 3( b ) then shows the corresponding breakfast and lunch-time insulin injections which are used to regulate the change in blood sugar. The glucose level of the patient at time sample k is then given by Eqn. 24, as the summation and convolution of all the A j,k & H j,k values over the previous day. FIG. 3 also shows the net rate of change from all food and insulin events j respectively along the κ or time axis.
[0000]
G
k
=
Δ
t
∑
k
′
=
0
k
∑
j
=
1
M
∑
κ
=
-
∞
k
′
A
j
,
κ
H
j
,
k
′
-
κ
(
24
)
F
k
-
1
=
Δ
t
∑
k
′
=
0
k
-
1
∑
j
=
1
M
A
j
,
k
′
(
25
)
[0027] For effective closed loop insulin delivery, a reliable estimate is needed of what blood sugar the patient is currently being forced to. This is given as F k−1 in Eqn. 25 and is the summation of all the forcing amplitudes A j,k which have occurred recently. This requires de-convolution of the delay effects in CGM data from stomach/insulin absorption that are characterized here by exponential functions H j,k from Eqn. 22. Practically this will be done using Eqn. 21 and by making time specific estimates of the forcing amplitudes A incurred by the patient throughout the day. The required insulin dose I to stabilize the patient at the target sugar level F T after eating food j can then be calculated simply as I j+1,k =(F k−1 −F T )/g≈(F j,∞ −F T )/g (see example later in FIG. 4 ).
[0028] The following seven paragraphs explain details of how estimates of F 3,∞ (and hence sum of amplitudes A) are made based on CGM data alone in a practical manner, using the recursive relationship defined in Eqn. 21 as a pre-estimate of the event occurring (i.e. either a food or Insulin intake). To do this however, there are two important practical issues that must first be addressed and which stem from the nature of the human time response to food & insulin (see FIG. 2( a ) & (b) and Eqn. 1). First note that H(t) has an initial start value of zero and as shown in Eqn. 21, this causes the estimate of forcing destination F k−1 to require use of CGM measurements made at times t k−2 , t k−1 & t k (i.e. past, present and future). Mathematically this also means that the recursive filter estimate will need to lag one sample behind the latest CGM measure. Second, the low initial values of the H(t) function could result in Eqn. 21 amplifying any CGM instrumental noise to unstable levels. In order to optimize diabetic closed loop control, the following processing of raw CGM data is necessary to counter these two effects.
[0029] Raw CGM data is defined here as G′ k , an example of which is displayed in FIG. 4 as diamond shaped data points. Only measurements up to sample k will exist, now in practice with instrument noise being present. Eqn. 21 requires low noise measurements of glucose levels up to and beyond sample k−1. The noted smooth exponential nature of the human food/insulin impulse response ( FIG. 2 ) means that it can also be represented using a Fourier series with minimal coefficients (or low frequency information). Hence a simple low pass filter can be applied to the raw data G′ k to remove instrument noise (which as discussed could make the Eqn. 21 result unstable). This low time frequency nature of human response then means that it can be well represented as a repeating Fourier series, with only a few low order coefficients. This also is shown as the G k function in FIG. 4 , repeating after one π half cycle. Such low pass filtering can of course be done in several ways depending on processing capabilities (e.g. time convolution with a Gaussian filter or simple attenuation in the Fourier domain as was used to give the solid curve function G k in FIG. 4 ). Since the low pass filtered result G k is considered a repeating Fourier series, it therefore allows a pre-estimate of the value to occur after sample k. This is convenient in the use of low pass filters which typically benefit from the presence of samples beyond that at the time desired (e.g. at k−1, see FIG. 4 where G k is assumed to repeat as the solid smooth curve after the first π half cycle).
[0030] Now the low pass filtered CGM result G k (created from the raw G′ k samples as in FIG. 4 ) can be used in the recursive relationship of Eqn. 21 to make an initial estimate of F k−1 . This hence predicts where the patients' blood sugar is currently being forced to and is temporarily considered representative (i.e. that the patient only eats one type of simple food and has perfect insulin that exactly counters its effects). Using pre-determined optimum time constants a & b, this estimate of where the patient is being forced to is gained from Eqn. 21 and shown as circles in FIG. 4 . In order to decide if a food event has occurred with confidence, this estimate is compared to the last recursive result, telling of where the patient was last being forced to (i.e. compare F k−1 to F k−2 ≈F j,∞ , looking for F k−1 −F k−2 to exceed a threshold value +ΔF and k f j becomes the sample at which the food event was decided to have occurred). As an example, in FIG. 4 it is assumed that the algorithm has been initiated with a new unknown patient, where 30 minutes of CGM data has been taken up to this point (i.e. k must be at least 6). In the start case only, F −1,∞ is set to G k (from Eqn. 21 assuming that there are no food or insulin forcings currently in the patients system). In the event that F j,k f j −F j−1,∞ ≧ΔF with new CGM data, the algorithm therefore decides that a food event has just occurred (where ΔF=20 mg/dL in this example but also may vary with different patients). FIG. 4 shows this, with results from a diabetic patient where a meal has recently been eaten. Thus the sugar level begins to rise and the curvature of G k also increases, causing a jump in the recursive result F k−1 (circles). The estimate of the food event amplitude is then found simply as A j,k f j =F j,k f j −F j−1,∞ (where the trigger sample k f f is typically k−1 but can be chosen from the 3 samples between k−3 & k−1 so to maximize the amplitude of A j,k f j ).
[0031] Since the time of the food event is unknown but certainly before to t k f j , a digital phase delay Δk j is used to represent how long ago food was eaten (typically chosen from 0→9 or 0-45 minutes). The food type is also unknown, so an estimate must be made of its time absorption characteristics. This uses an iterative fit to the actual CGM data (i.e. decide on some optimal values of a 1,j , b 1,j & Δk 3 in Eqns. 26 and 27, so to best match the data occurring after sample k f j −Δk j ).
[0000]
H
j
,
k
=
Φ
-
b
1
,
j
Δ
t
.
k
(
1
-
-
a
1
,
j
Δ
t
.
k
)
(
26
)
S
j
,
κ
=
∑
k
=
k
f
j
κ
A
j
,
k
f
j
×
δ
(
k
,
k
f
j
-
Δ
k
j
)
(
27
)
B
j
,
k
=
Φ
c
0
S
j
,
k
-
1
+
c
1
B
j
,
k
-
1
-
c
2
B
j
,
k
-
2
(
28
)
Ψ
j
,
k
=
∑
κ
=
k
f
j
-
Δ
k
j
k
(
G
κ
′
-
B
j
,
κ
)
2
(
29
)
[0000] The Kronecker delta function δ (k,k f j −Δk j ) in Eqn. 27 is zero everywhere except for at k=k f j −Δk j , where it has a value of one. Again note that the apostrophe on G′ k in Eqn. 29 indicates that it is the raw unfiltered CGM result, with a preserved temporal frequency response so to best match the model being iterated. This model estimate of the raw data G′ k is therefore generated with iterative estimates of forcing F, by simple re-arrangement of Eqn. 21 to give the recursive model result B j,k for food event j (Eqn. 28). A gradient descent algorithm as described by Matthews (2009) is then used to find the optimum values of a 1,j , b 1,j & Δk j that minimize the residue result Ψ j,k (Eqn. 29). An example of the optimal model fit B j,k is also shown as the dashed line in FIG. 4 . The next requirement is now to estimate the amount of insulin needed to counter this detected food event, which requires two more steps:
[0000] G′ k =m j B j,k +C j (30)
[0000] F′ j,∞ =?m j ×A j,k f j +C j (31)
[0000] I j,k =( F′ j,∞ −F T )/ g (32)
[0000] First the model result B j,k is linearly regressed against the actual data G′ k as in Eqn. 30, to give slope and offset values m j & C j (typically m j ≈1 & C j =G k f j −Δk j ). Then the new and more accurate estimate of the forcing destination F′ j,∞ (Eqn. 31) is again compared to the threshold sugar level F T (nominally 100 mg/dL). The variable g must be a conservative estimate of insulin gain, so to calculate an effective but safe dose I j,k from Eqn. 32 to then be injected from the insulin pump[ 10 ]. As the next sample G′ k+1 arrives from the CGM, the value of A j,k f j , is recalculated. If it and F k−1 have increased in value, they are updated and the gradient descent fit of Eqns. 26 to 29 is repeated, this time with the extra CGM data point. In the event that the resulting insulin dose I j,k+1 >I j,k , then the additional amount I j,k+1 −I j,k is simply then injected from the pump[ 10 ].
[0032] The recursive/iterative process continues and the model results are updated and stored to estimate the amount of both food and insulin in the patients system as more data arrives. Eventually the patient blood glucose G′ k ceases to rise and the continually calculated forcing values F k−1 then conversely drop a threshold value ΔF below the model destination (i.e. F k−1 −F′ j,∞ ≦ΔF). This indicates that an insulin event has occurred. FIG. 5 shows an example of this with further CGM data sampled beyond that in FIG. 4 , where an Insulin event is found to have occurred. Similar to the food event discussed above, the amplitude of this event A j,k I j is calculated as F j,k I j −F j−1,∞ (where like k f j , k I j is usually k−1 but can take a value between k−3 and k−1 if it maximizes the absolute value of A j,k I j ). As discussed earlier, detection of both food and insulin events is initiated using the simplistic assumption that both have time responses that are equal in shape but opposite in sign. (i.e. since insulin events lower blood sugar levels in the patient, their amplitudes are negative). However as also mentioned the algorithm must operate with the conservative expectation that a restoring injection from a sugar reservoir is to be used only in an emergency. In general the type of insulin being injected will be more of a constant than the type or frequency of food eaten. In order to proceed with extra caution, it is therefore optimum to use an extra term in Eqn. 1 for a representation of the insulin impulse response. This also helps to recreate the inflection points often observed as part of the insulin time response, in addition to allowing simulation of slower acting insulin (e.g. see solid curve of FIG. 2( b )). The following Eqns. 33 to 48 are hence simply slightly higher order versions of those presented in Eqns. 26 to 29, with three rather than two exponential terms:
[0000]
H
j
,
k
=
Φ
j
(
1
-
-
a
2
,
j
Δ
t
.
k
)
(
-
b
1
,
j
-
-
[
a
1
,
j
+
b
1
,
j
]
Δ
t
.
k
)
(
33
)
p
=
-
(
a
2
,
j
+
b
1
,
j
)
Δ
t
.
k
(
34
)
q
=
-
(
a
1
,
j
+
b
1
,
j
)
Δ
t
.
k
(
35
)
r
=
-
(
a
2
,
j
++
a
1
,
j
+
b
1
,
j
)
Δ
t
.
k
(
36
)
s
=
-
(
b
1
,
j
)
Δ
t
.
k
(
37
)
d
0
=
r
+
s
-
p
-
q
(
38
)
d
1
=
2
(
p
+
q
-
s
+
r
)
(
39
)
d
2
=
s
+
q
+
r
+
p
+
s
+
r
-
p
+
s
+
q
-
p
+
q
+
r
(
40
)
d
3
=
p
+
q
+
r
+
s
(
41
)
d
4
=
p
+
q
+
p
+
r
+
p
+
s
+
q
+
r
+
q
+
s
+
r
+
s
(
42
)
d
5
=
p
+
q
+
r
+
s
+
q
+
r
+
p
+
s
+
r
+
p
+
s
+
q
(
43
)
d
6
=
p
+
q
+
r
+
s
(
44
)
Φ
j
=
1
-
d
3
+
d
4
-
d
5
+
d
6
d
0
+
d
1
+
d
2
(
45
)
S
j
,
κ
=
∑
k
=
k
I
j
κ
A
j
,
k
I
j
×
δ
(
k
,
k
I
j
-
Δ
k
j
)
(
46
)
B
j
,
k
=
Φ
j
(
d
0
S
j
,
k
-
1
+
d
1
S
j
,
k
-
2
+
d
2
S
j
,
k
-
3
)
+
d
3
B
j
,
k
-
1
-
d
4
B
j
,
k
-
2
+
d
5
B
j
,
k
-
3
-
d
6
B
j
,
k
-
4
(
47
)
Ψ
j
,
k
=
∑
κ
=
k
f
j
-
Δ
k
j
k
(
G
κ
′
-
B
j
,
κ
)
2
(
48
)
[0033] Again a Kronecker delta function δ (k,k I j −Δk j ) is zero everywhere except for at k=K I j −Δk j where it has a value of one (Eqn. 46) and as before the apostrophe on the G′ k indicates that is the raw unfiltered CGM result (preserving the true frequency response). The model estimate of the raw data G′ k is now generated as the recursive result B j,k for insulin event j from Eqn. 47 (i.e. using iterated model estimates S j,k of net forcing F). Optimum values of a 1,j , b 1,j , a 2,j & Δk j are also determined from a slightly higher order gradient descent algorithm so to again minimize the residue result ψ j,k in Eqn. 48 (see Matthews (2009)). Greater confidence is again obtained by re-performing the regression of Eqns. 30 and 31 (where as before m j ≈1 but now C j =G k I j −Δk j ) . Such an example of an insulin event optimal model fit B j,k is shown in FIG. 5 as the dashed curve occurring after a time of 160 minutes.
[0034] This document details the basis behind use of a recursive filter to model, fit and predict a diabetic response to either food or insulin intake in real-time. The algorithm allows a computer to design an insulin pump dose to safely restore blood glucose levels to normal, through what is typically known as a closed loop insulin control system. The process has been demonstrated using computer code written in the IDL language.
[0035] It will thus be seen that the objects set forth above, among those made apparent from the preceding description, are efficiently attained and, because certain changes may be made in carrying out the above method and in the construction(s) set forth without departing from the spirit and 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.
[0036] 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 there between. | Presented is a computational system for predicting the blood glucose level to which a diabetic patient is being forced based solely on continuous glucose monitor (CGM) data that then allows optimum and safe calculation of a stabilizing dose to be applied by an insulin pump. This invention hence operates as part of a closed loop insulin delivery system. Included are recursive filters for estimating forthcoming blood glucose levels in real-time. Designed to match typically observed human blood glucose rates of change due to food digestion and insulin injection, these filters are two and three term exponential functions respectively. Such filters are applied to low pass filtered CGM data before being iteratively matched to the raw CGM data in order to yield greater confidence in the recursive predictions. All filters also have infinite response curves with monotonically decreasing amplitudes over time. The recursive and iterative process repeats with the arrival of further CGM measurements, allowing on-going calculation and delivery of optimum and safe insulin by an infusion pump in a close loop insulin delivery system. | 0 |
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates generally to a cover plate arrangement for a well such as a water well and, more specifically, to a cover plate arrangement for a well which is quickly and easily centered above an exposed well bore and which is held securely in place by an associated well pump once in position on the well.
2. Description of the Prior Art
Modern water wells are drilled into the ground with the well bore either being uncased, or being protected by a casing which is sunk into the well. Typically, a submersible pump is then run down the well bore on either rigid or flexible tubing and submerged in water located at the bottom of the well. The pump provides water to the surface through the flexible tubing which is connected to the pump and which leads up the well bore to the well surface. Although various types of flexible tubing are known, the most commonly used tubing today is a polyolefin, such as polyethylene. In certain of the prior art practices, a separate safety rope or cable is also provided, connected to the pump and extending the length of the bore to assist in withdrawal of the submersible pump from the well bore if the pipe were to separate or break. In addition, since the submersible pump is electrically driven, a power cord or cable also typically extends from the well surface down the bore to the pump where it is attached to the flexible tubing, as by taping the cable to the tubing.
The present invention has general applicability to “cased” wells of the type described above where cylindrical tubing in the form of steel pipe is inserted into the well shaft which has been formed to serve as the side walls of the well. Typically a short portion of this casing is either flush with, or extends slightly above the ground as the upper terminal of the well, which must be covered to prevent foreign matter from entering the well. Although a cased well of the type previously described is commonly encountered in the field, it will be understood upon further reading of the present specification that the invention being described also has applicability to uncased wells which must also be covered with some type of well cover plate arrangement, or to well heads which have a concrete pad or the like poured at the well surface to form the well opening.
In any event, whatever the particular configuration of the well head or well opening, a well cover plate arrangement of some type is generally needed to provide security for the well to prevent the entry of foreign matter, and also to provide provision for passing the flexible tubing, electrical cable, and other accessory lines to the down hole pump which is submerged in the well. Since the well cover plate provides provisions for passing tubing to the pump, which is submerged in the well, the cover must be easily removed so that the pump can be replaced or repaired when necessary, and the cover must be generally centered on the casing in order to center the pump in the well.
While simple devices such as a plate with the required openings conceivably could be permanently welded or otherwise affixed to the top end of a well casing, the fact that the submersible pumps fail and sometimes must be replaced dictates that some form of removable seal or cap be provided. As a result, a variety of different types and styles of removable well cover plates have been provided in the industry, such as those shown in Zanin, U.S. Pat. No. 2,735,697, Medina, U.S. Pat. No. 3,631,895, Martin, U.S. Pat. No. 3,963,054, Henson, U.S. Pat. No. 4,129,151, Forsell, U.S. Pat. No. 4,202,376, and Henson, U.S. Pat. No. 4,972,905. However, the devices shown in the prior art, such as those included above, have all generally involved complicated and sophisticated clamping and centering means, which are prohibitively expensive for use in many instances, such as in a single family water well. In addition the complexity of these devices greatly adds to the difficulty in installing and removing the cover, and results in a high rate of failure when the cover is repeatedly removed and installed.
Some well casings use successive threaded sections of pipe, while others have successive sections welded together. While it is theoretically possible in threaded casing installations to provide a removable well cap which threadedly engages threads provided at the upper end of the well casing, caps which thread onto the well casing are deemed impractical for a number of reasons. Turning a threaded cap to install it would undesirably twist the electrical cable which must pass through it, unless the cable passed through an opening in the cap so large that insects or rainwater could also pass through the opening. Also, prohibitively great forces often would be required to unscrew a threaded cap which had been exposed to weather for some years. For such reasons, practical removable well caps cannot be threaded onto the upper ends of well casings.
It is also advantageous that well cover plate arrangements not employ a plurality of bolts or nuts in securing the cover plate to the well head since the bolts and nuts frequently must be installed under adverse weather conditions. If bolts or nuts are accidentally dropped they are frequently lost in mud, snow or the like at a well side. Where some sort of bolt and nut arrangement is spaced about the well cover, their threads sometimes become jammed or may be inadvertently stripped, sometimes ruining the whole assembly unless it is re-bored and re-tapped with a larger threaded hole, or sometimes requiring that spare bolts or nuts be obtained. A further disadvantage of seals using plural bolts and nuts spaced around the cover plate is that they must be tightened evenly, i.e. by tightening a given bolt only partially and then proceeding to similarly tighten each of the other bolts before further tightening the given bolt. This is a time consuming and somewhat tedious procedure at best.
It is the object of the present invention to provide an improved well cover plate arrangement which overcomes the various mentioned disadvantages of the prior art by providing a combination U-plate and door element of unique design which are economical to manufacture and which can be easily installed under field conditions.
It is a further object of the present invention to provide an improved combination U-plate and door element, each of which is of a “single-piece” nature, the plates being formed from readily available materials utilizing simple manufacturing techniques.
It is a further object of the invention to provide an improved well cover plate arrangement which does not require sequential tightening of a plurality of bolts and/or nuts in order to install the assembly.
The provision of such a well cover plate arrangement allows a well cover assembly to be installed or removed much more rapidly than prior assemblies, generally requiring only a single worker, thereby providing a significant savings in labor costs.
SUMMARY OF THE INVENTION
The well cover arrangement of the invention provides an improved device and method for covering the exposed opening of a well where the well has a submersible pump supported on a well tubing string suspended downwardly in the well where the well string has at least one support collar formed thereon. The improved combination device of the invention includes a U-plate having an upper planar surface, a lower planar surface and a thickness there between. The upper and lower planar surfaces are circumscribed by an outer peripheral edge. The U-plate has a U-shaped opening formed at one point in the outer peripheral edge. The combination device of the invention also includes a door element having an upper planar surface and a lower planar surface, the door element being sized to approximately cover the U-shaped opening formed in the peripheral edge of the U-plate when the U-plate is in place on a well string. The assembled U-plate and door element form the combination base plate of the invention.
Engageable locking elements are present on the U-plate and on the door element which, when engaged, allow the door element to slide into position on the U-plate by movement in a general horizontal plane parallel with a plane defined by the upper planar surface of the U-plate. The locking elements also serve to prevent movement of the door element in a vertical direction off the U-plate once the locking elements are engaged.
Preferably, the door element has a leading edge and a trailing edge, and wherein the leading edge forms a semi-circular opening which is sized to form an opening of the approximate diameter of the well tubing string so that a collar present in the well string will rest upon the upper planar surface of the door element and lock the plate in position as weight of the well string bears against the U-plate and door element. The locking elements can comprise, for example, spaced notches and slots formed adjacent the U-shaped opening on the U-plate which are engageable with mating spaced notches or slots formed on the door element. The preferred door element also has a pair of spaced side rails running on either of two sides thereof between the leading edge and the trailing edge, the side rails having tapered leading surfaces which assist in locating the well string within the U-shaped opening of the door element.
The preferred U-plate can be equipped with a raised strip formed on the upper planar surface thereof which spans two opposing peripheral edges thereof adjacent the U-shaped opening, the raised strip serving to brace and reinforce the U-plate in use. The door element which is used as a part of the well cover arrangement of the invention will also typically be provided with a fitting which communicates the upper and lower planar surfaces thereof, the fitting being adapted to receive an electrical conduit for providing electrical power to the submersible pump being suspended in the well. The U-plate is also typically provided with a carrying handle affixed to the upper planar surface thereof.
While the cover plate arrangement of the invention can be used with a variety of submersible pump installation devices, it finds particular utility when used in an installation piocedure for installing and removing a submersible pump from a well bore where the pump is supported on a length of a flexible tubing string which is initially wound up on a take up reel, the tubing string having at least one collar located in an upper extent thereof. One preferred apparatus of this type includes a pivot frame which is mounted on a portable base frame which is transportable from one well location to another. The portable base frame is supported in a horizontal plane with respect to a surrounding support surface, and wherein the pivot frame is capable of pivoting movement in a plane generally parallel to the plane of the base frame. A pair of oppositely arranged support arms are mounted on the pivot frame, each of the support arms being pivotally mounted at an inner extent at a pivot point on the pivot frame and having an opposite outer extent.
A cylindrical take up reel is also provided having opposing sides separated by a central region for accumulating the flexible tubing string, each of the opposing sides of the cylindrical take up reel being supported on the portable base frame by connection to a selected one of the respective support arms. A primary pivot mechanism has a first extent pivotally attached to the pivot frame and has a second extent pivotally attached to a respective one of the support arms whereby actuation of the primary pivot mechanism serves to pivot the support arm and, in turn, the cylindrical take up reel between a collapsed position on the base frame and an extended, upright position.
The previously described installation apparatus is used by first transporting the base frame to a well site adjacent a well bore having a vertical well axis. Next, the primary pivot mechanism is actuated to raise the support arms and, in turn, the take up reel from a collapsed position to a work position which is vertically oriented with respect to a vertical axis of the well bore with the submersible pump being centered up as much as possible with respect to the well bore vertical axis. The take up reel is then actuated in order to dispense a required length of flexible tubing string so that the submersible pump is gradually lowered into the well bore. The well tubing string has a support collar which is connected to an upper end of the flexible tubing string, the collar having a greater external diameter than the flexible tubing string at the connection.
The previously described U-plate and door element which make up the well cover assembly of the invention is then provided at the well site. A worker slides the U-shaped opening of the U-plate about the tubing string below the collar. The door element is then moved into position on top of the U-plate with the U-shaped opening formed in the U-plate approximately covering the U-shaped opening in the U-plate and contacting the well tubing string so that the tubing string passes through the remainder of the opening formed between the door element and U-plate. The door element can then be secured in position on top of the U-plate by setting down weight on the tubing string and, in turn, upon the door element and U-plate.
To remove the submersible pump from the well, weight is first lifted off the door element and U-plate by pulling upwardly on the tubing string. The door element can then be slid off the U-plate and the above described procedure basically repeated in reverse fashion.
These and other aspects of the invention will be better appreciated and understood when considered in conjunction with the following description and the accompanying drawings. It should be understood, however, that the following descriptions, while indicating preferred embodiments and numerous specific details thereof, are given by way of illustration and not of limitation. Many changes and modifications may be made within the scope of the embodiments herein without departing from the spirit thereof, and the embodiments herein include all such modifications.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a perspective view of a well servicing operation in which a submersible well pump is about to be pulled from the well bore on a cable, the well being covered with the cover plate arrangement of the invention.
FIG. 2 is an isolated view of the U-plate and door element which make up the cover plate arrangement of the invention, showing the exposed submersible pump collar resting upon the cover plate arrangement.
FIG. 3A is a view of the improved U-plate of the invention showing the first step in installing the well cover arrangement of the invention with the U-plate being positioned about an upper portion of the well tubing string, the tubing string collar being removed for ease of illustration.
FIG. 3B shows the next step in the assembly of the cover plate arrangement of the invention in which the improved door element is installed on the U-plate.
FIG. 3C is a view similar to FIG. 3B , but showing the next step in the installation of the well cover of the invention with the door element being installed in its final position.
DETAILED DESCRIPTION OF THE INVENTION
The embodiments herein and the various features and advantageous details thereof are explained more fully with reference to the non-limiting embodiments that are illustrated in the accompanying drawings and detailed in the following description. Descriptions of well-known components and processes and manufacturing techniques are omitted so as to not unnecessarily obscure the embodiments herein. The examples used herein are intended merely to facilitate an understanding of ways in which the invention herein may be practiced and to further enable those of skill in the art to practice the embodiments herein. Accordingly, the examples should not be construed as limiting the scope of the claimed invention.
In order to understand the particular utility of the combination U-plate and door element which make up the well cover arrangement of the invention, the general environment surrounding the installation of a submersible well pump will first be described. Turning to FIG. 1 of the drawings, there is shown an apparatus 11 for raising and lowering a submersible pump 13 in a well bore where the pump is run on a length of a flexible well tubing string 15 . In the example illustrated in FIG. 1 , the flexible tubing string 15 is polyethylene tubing. As will be appreciated from FIG. 1 , the particular well installation apparatus 11 includes a portable base 17 of a generally polygonal configuration, in this case a rectangular frame. The frame is made up of front and rear elongate members and elongate side members. The frame 17 can be made of any convenient sturdy material, e.g., channel iron or the like. As will be appreciated from FIG. 1 , the frame 17 is supported on a pair of axles 27 , 29 and associated wheels 31 , 33 , so that the frame can be transported from one well location to another.
FIG. 1 shows the frame 17 as it would be equipped to be towed from the trailer hitch of a pickup. The frame could also be transferred in other ways as, for example, by being skid mounted, or truck or trailer mounted. As also will be appreciated from FIG. 1 , the wheels 31 , 33 and axles 27 , 29 support the frame 17 in a horizontal plane with respect to a surrounding support surface 35 , which in this case is a section of roadway. Hydraulic struts or stabilizers 18 are provided to support the frame in the position shown in FIG. 1 once the base frame has been temporarily positioned.
Referring again to FIG. 1 , it can be seen that a pair of oppositely arranged support arms ( 63 shown) are each pivotally mounted at an inner extent 65 on a pivot frame 37 . Each of the support arms also has an opposite outer extent 69 . A cylindrical take up reel ( 81 in FIG. 1 ) is supported on the support aims 63 and has opposing sides and a central region 87 for accumulating the continuous roll of flexible tubing 15 . Each of the opposing sides of the cylindrical take up reel is supported on the portable base frame 17 by connection a respective one of the support arms 63 . The pivot frame 37 allows pivoting movement in the horizontal plan while the pivot arm 63 allow pivoting movement about the pivot point 65 .
As can be seen in FIG. 1 , an outer extent of the support arm 63 mounts to a commercially available gear reduction unit 89 . While a variety of commercially available gear reduction units might be utilized, the particular unit illustrated utilizes a planetary gear system in which a hydraulic motor (not shown) drives the center gear of the unit on either side of the take up reel. A ring gear is turned by a set of planetary gears to provide a desired gear reduction. The ring gear is, in turn, attached to the main hub upon which the cylindrical drum is mounted. There is an identical arrangement on the opposite side of the cylindrical drum and hub.
It will be appreciated with respect to FIG. 1 of the drawings that the support arms 63 are each pivoted between a retracted or collapsed position and the extended or vertical work position shown in FIG. 1 by a primary pivot mechanism. In the example illustrated, the primary pivot mechanism is comprised of at least one hydraulic cylinder 101 which is attached to the pivot frame and to the support arms at pivot points 93 , 95 , respectively, whereby actuation of the primary pivot mechanism serves to pivot the support arms and, in turn, the cylindrical take up reel between the collapsed position resting on the base frame, and the extended, upright position. The hydraulic cylinder 101 is of conventional design and is commercially available from a number of convenient sources. It is hydraulically powered by a hydraulic motor (not shown in FIG. 1 ) as will be well understood by those skilled in the relevant arts. The pivot mechanism allows the position of the cylindrical drum to be accurately centered with respect to a vertical axis of a well bore to be accessed for raising and lowering the submersible pump into the well bore.
FIG. 1 shows a string of flexible well tubing 15 being used to either raise or lower a submersible pump from a well bore. The tubing string includes at least one support collar (generally at 97 in FIGS. 1 and 2 ) formed therein.
With reference now to FIGS. 2-3C , there is shown the improved well cover plate assembly of the invention. The cover plate assembly includes a U-plate ( 99 in FIG. 2 ) having an upper planar surface 101 , a lower planar surface 103 and a thickness “t” there between. The upper and lower planar surfaces 101 , 103 are circumscribed by an outer peripheral edge 105 . As can perhaps be best seen from FIG. 3A , the U-plate 99 has a U-shaped opening 107 formed at one point in the outer peripheral edge 105 . The U-shaped opening 107 is an elongate recess in the U-plate formed by parallel sidewalls 109 , 111 , and terminating in an arcuate end region 113 . The width of the opening 107 is selectively sized to closely receive the outside diameter of the well tubing string ( 115 in FIG. 3A ). It will also be appreciated from FIG. 3A that the U-shaped opening has at least one notch 117 formed in the sidewall 111 . The top surface 101 of the U-plate also has a pair of tabs 119 , 121 affixed thereto which form slots 123 for receiving and matingly engaging a cooperating U-shaped U-plate.
As can be seen in FIG. 3B , the door element 125 has an upper planar surface 127 and a lower planar surface 129 . The door element 125 is sized to approximately cover the U-shaped opening 107 formed in the peripheral edge of the U-plate 99 when the door element is in place on a well string. The door element 125 also has a side tab 131 which is adapted to be received in the notch 117 of the U-shaped opening 107 , and has end tabs 133 , 135 which engage the slots 123 formed on the U-plate adjacent the U-shaped opening. The side tab 131 and end tabs 133 , 135 , together with the notch 117 and slots 123 on the U-plate, form engageable locking elements present on the U-plate and on the door element which, when engaged, allow the door element to slide into position on the U-plate by movement in a general horizontal plane parallel with a plane defined by the upper planar surface of the U-plate. When in position shown in FIG. 3C , the tabs 133 , 135 prevent the door element 125 from being raised up at the back. FIGS. 3B and 3C generally illustrate this action. The locking elements also serve to prevent movement of the door element in a vertical direction off the U-plate once the locking elements are engaged.
As can be seen in FIG. 3B , the door element 125 has a leading edge 137 and a trailing edge 139 . The leading edge 137 preferably forms a semi-circular opening which is sized to form an opening of the approximate diameter of the well string so that a collar (such as collar 97 in FIG. 2 ) which is present in the well string will rest upon the upper planar surface 127 of the door element and lock the plate in position as weight of the well string bears against the U-plate and door element. Preferably, the door element has a pair of spaced side rails 143 , 145 running on either of two sides thereof between the leading edge 137 and the trailing edge 139 thereof which support the door element above the U-shaped opening 107 . The side rails have tapered leading surfaces 147 , 149 (see FIG. 3B ), which assist in locating the well string within the U-shaped opening of the U-plate.
As can be seen in FIG. 3C , the door element 125 will typically be provided with a fitting 151 which communicates the upper and lower planar surfaces thereof, the fitting being adapted to receive an electrical conduit for providing electrical power to the submersible pump being suspended in the well. A nut 152 is provided to receive and secure an electrical ground wire. As will be apparent from FIG. 3C , when the door element 125 is removed, the associated electrical wiring travels with the door element. It will also be appreciated from FIG. 3C that the U-plate 99 in the version of the invention shown has a raised strip 153 formed from angle iron or channel iron on the upper planar surface 101 thereof which spans two opposing peripheral edges thereof adjacent the U-shaped opening. The raised strip 153 serves to brace and add strength to the U-plate. This allows the U-plate to be formed of lighter weight material, for example ½ inch thick steel plated. The U-plate 99 will also typically be provided with a carrying handle 155 for convenience.
The general operation of the apparatus of the invention will now be briefly described. The apparatus of the invention can be used in an improved method for lowering and pulling a submersible pump from a well bore where the pump is supported on a length of flexible tubing initially wound up on a take up reel. While the operation of the invention will be described with respect to a length of flexible tubing, it will be understood that it could be used with a string of rigid tubing, as well. The previously described portable base frame 17 is moved into position at the well site, as shown in FIG. 1 . The primary pivot mechanism 101 is then actuated to raise the support arms 63 and, in turn, the take up reel 81 from a collapsed position to a work position which is vertically oriented with respect to the vertical axis of the well bore with the submersible pump being centered up as much as possible with respect to the well bore vertical axis. Pivot frame 37 helps to provide a fine adjustment for the centering action.
The take up reel 81 is then actuated to dispense a required length of flexible tubing so that the submersible pump is gradually lowered into the well bore. When the desired depth is reached, the upper end of the flexible tubing is secured at the well head using the improved well cover assembly of the invention. This is conveniently accomplished by connecting a support collar ( 97 in FIG. 2 ) to an upper end of the flexible tubing string, the collar having a greater external diameter than the flexible tubing string at the connection. The U-plate 99 is then slid into the position shown in FIG. 3A with the well tubing string engaged within the U-shaped opening 107 . The support collar 97 is shown removed in FIG. 3A for ease of illustration. However, it will be understood that the U-plate 99 will be slid beneath the support collar 97 to the position shown in FIG. 2 .
The door element 125 is then slid into position, as shown in FIGS. 3B-3C to approximately cover the U-shaped opening 107 in the U-plate 99 and to come into contact with the tubing string so that the tubing string passes through the remainder of the opening formed between the door element and U-plate. The door element is then secured in position by setting down weight on the tubing string and, in turn, upon the door element and U-plate. This position is shown at FIG. 2 of the drawings. It will be appreciated that the engageable locking elements present on the U-plate and on the door element, when engaged, allow the door element to slide into the position shown in FIG. 3C on the U-plate by movement in a general horizontal plane parallel with a plane defined by the upper planar surface 101 of the U-plate. The locking elements also serving to prevent movement of the door element in a vertical direction off the U-plate once the locking elements are engaged. The semi-circular opening ( 137 in FIG. 3B ) at the leading edge of the door element 125 which is sized to form an opening of the approximate diameter of the well tubing string so that a collar present in the well tubing string will rest upon the upper planar surface of the door element and lock the plate in position as weight of the well string bears against the U-plate and door element.
An invention has been provided with several advantages. The combination U-plate and door element of the invention work together to provide a secure well cover assembly. Once the door element is moved into position and weight is set down upon the support collar of the tubing string, the cover plate assembly is securely locked into position and can only be removed by first removing weight from the well string. The assembly of the invention is economical to manufacture and can be easily installed under field conditions. The assembly of the well cover plate of the invention does not require sequential tightening of a plurality of bolts and/or nuts in order to install the assembly. The present well cover plate arrangement allows a well cover assembly to be installed or removed much more rapidly than prior assemblies, generally requiring only a single worker, thereby providing a significant savings in labor costs.
While the invention has been shown in only one of its forms, it is not thus limited but is susceptible to various changes and modifications without departing from the spirit thereof. | A well cover arrangement is shown for covering the exposed opening of a well where the well has a submersible pump supported on a collared well string which is suspended downwardly in the well. The cover arrangement includes both a U-plate with a U-shaped opening therein and a door element which fits within the U-plate opening. Once the door element is properly positioned on the U-plate, cooperating locking elements maintain its proper position. The ultimate weight of the well tubing string further secures the door element as the collar in the well string contacts a portion of the door element, making removal of the door element only possible by first lifting the well string. | 4 |
REFERENCE TO PRIOR APPLICATIONS
[0001] This application claims the benefit of U.S. Provisional Application No. 60/501,428, filed Sep. 10, 2003.
BACKGROUND OF THE INVENTION
[0002] 1. Field of the Invention
[0003] The present invention relates to a protective coating for various surfaces. In particular, the present invention relates to a protective coating for concrete, steel and wood.
[0004] 2. Description of the Related Art
[0005] The use of polymer coatings to protect surfaces and enhance functional properties of materials is well known. The development of many different polymer systems has led to many new applications and materials. Some of these systems like epoxies, nylon, polyurethanes and polyureas have very useful properties. The useful properties of many of the plastic coatings mentioned above cannot be obtained on substrate surfaces, however, due to the difficulty in formulating easily applied coatings. Overcoming this problem would be of great advantage to the industry.
[0006] One particular surface to which coatings are often applied is that of wood. The coating of wood with various polymer products has been well established and is currently a very large worldwide industry. Wood is a major construction material but must be protected from degradation by weather, sunlight, abrasion from use, and many other factors. The application of coatings to wood has provided a method of extending the useful life of wood products and has also provided many, varied aesthetic improvements.
[0007] Typical major drawbacks in the use of coating products is the presence in most instances of a carrier or solvent that allows the paint or coating to be applied in a liquid form. The coating then needs to be dried to provide a continuous coating or film on the wood. The presence of this carrier or solvent leads to significant quantities or organic chemicals that are allowed to evaporate into the atmosphere and thus become pollutants which is a very undesirable situation.
[0008] In addition to paints and coatings there are many treatments that have been developed for the preservation of wood. One of these treatments, in particular, is referred to as the CCA treatment, which involves copper, chromium and arsenic. The arsenic in particular has been demonstrated to be linked with certain diseases such as cancer, particularly in children. Thus the use of this type of wood treatment has nearly been completely halted. However, there are large amounts of structures in place that contain CCA treated wood that need to be addressed.
[0009] It is therefore an object of the present invention to provide a novel, enhanced protective coating for various surfaces, especially concrete, steel and wood, which coating can help overcome many of the aforediscussed problems and issues.
SUMMARY OF THE INVENTION
[0010] The present invention provides a polyurethane/polyurea protective coating produced by reacting an isocyanate with a polyol in the presence of a diamine or triamine, preferably a low molecular weight diamine or triamine, and a catalyst. Preferably, the polyol is a polyester polyol, a polyether polyol, an acrylic polyol or mixtures thereof. The catalyst is preferably a metal based catalyst such as a tin, zirconium or bismuth based catalyst.
[0011] The protective coatings of the present invention are intended for use in high pressure impingement mixing spray systems. These systems can utilize 100% solids fluids which do not contain a solvent and thus are zero (or near zero) VOC coatings. One of the surprising results that has been obtained is that several amines utilized in other cured systems can be formulated into sprayable fluids and provide an excellent coating with very useful properties.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0012] The coatings of the present invention are targeted for the protection of many different surfaces. Materials such as concrete, steel, aluminum, wood and others degrade when exposed to UV radiation, humidity and various chemicals. The protective coatings of this invention dramatically reduce or eliminate the detrimental effects of exposure to these conditions. It has been found that several low molecular weight, highly reactive amines can be combined with polyols and isocyanates to yield very useful and easy to apply protective coatings. These final coatings are hybrid polyurethane/polyurea coatings.
[0013] The polyol employed in preparing the coatings of the present invention can be any suitable polyol reactive with an isocyanate, and is preferably a polyester polyol, polyether polyol, an acrylic polyol or mixture thereof. Indeed, it is most preferred that a mixture of polyester polyols, together with a polyether polyol be employed. The amine can be any suitably reactive diamine or triamine, preferably an aliphatic diamine or triamine. The presence of primary amines can render the composition too reactive so that when the components are mixed the coating cannot be easily applied. Thus, the presence of primary amines is not desirable. Preferred aliphatic amines include polyoxypropylenetriamine, menthanediamine, 2-methylpentamethylenediamine, those available under the trademark Clearlink 1000™ or the like. The amount of diamine or tramine that is present in the final coating generally ranges from 0.5 to 20 percent by weight of total solids.
[0014] The protective coating is generally applied by preparing a first formulation, e.g. formulation A, comprised of the isocyanate compounds. The isocyanate compounds can comprise any suitable isocyanate, especially dimers and trimers. In a preferred embodiment a mixture of isocyanate dimer and trimer is preferred. Among the preferred diisocyanates is 4-4′-diphenyl methane diiocyanate. A formulation B comprising the polyol and amine is also prepared, and then mixed with formulation A for application onto the substrate. A suitable catalyst can be placed in either formulation, or both if desired
[0015] Since the formulations are of solids, and no solvent is employed, the mixing can involve a static mixer and the formulation and the coating are applied by a brush or squeegee. As well, in a most preferred embodiment, however, it has been surprisingly found that the system can be formulated into sprayable fluids, even though comprised of solids, with the coating being sprayed onto the substrate to be coated. A high pressure impingement mixing/spray system is most preferred for applying the protective coatings of the present invention. Most preferred is a zero solvent high pressure spray process for application of the coating. Such high pressure impingement spray apparatus are commercially available, for example, from Gusmer, Graco, Glas-Craft and other companies. The high pressure spraying is generally conducted at a NCO/NH 2 —OH ratio from about 0.9 to 1.3, and most preferably at a ratio from about 1.05 to 1.10. Once the coating has been applied, it is generally utilized in a thickness of from 0.1 mil to 100 mil.
[0016] The coatings of the present invention are useful in coating wood, concrete, steel and other surfaces as a protective coating. The coating on structures, articles or items made of such materials provide an environmentally friendly approach to preventing degradation by weather, UV radiation, abrasion, and other factors, thereby preserving the overall structure. The coating also adheres well to the various surfaces. For wood, the protective coating of the present invention can have an elongation of at least 100% well adhered to the wood surface, a Shore D hardness of 30 or greater well adhered to wood surfaces, and/or an adhesion to CCA pressure treated wood and other types of wood of greater than 1 MPa (140 psi) in adhesion strength.
[0017] In one embodiment, the coatings of the present invention are used to coat an encapsulate wood, and wooden structures. The present invention provides a system for coating wooden structures or articles with a barrier coating that both prevents further degradation of the wood and also when needed provides an encapsulation coating for containing dangerous chemicals within the barrier coating and wood structure. The coating system in addition does not use any solvents and thus generates zero VOC or near zero VOC (VOC is volatile organic chemicals). The coatings in the present invention can be spray applied, brush applied, or applied by other typical painting implements. The coatings of the present invention do not utilize the traditional solvent carrier method in which a polymerizable formulation is applied to the wood surface or impregnated into the wood structure followed by during and then polymer formation. The coatings of the present invention utilize materials that are fluid during application and react instantaneously or very rapidly after being mixed and then adhere to the wood surface during final curing and hardening. During this process there is zero or near zero release of any organic chemicals into the atmosphere, all of the applied material is reacted into the final coating layer.
[0018] The coatings in the present invention have also been designated to yield a barrier layer that resists the migration of previously employed wood preservative chemicals out of the wood structure and into the environment or into contact with humans. Specifically, the barrier coatings of the present invention have been shown to contain dangerous elements such as arsenic within the wood structure. This is of high value since there is a large number of wood structures that exist using CCA (chromium, copper and arsenic) treated wood, which now must be dealt with by removal or some other method. These chemicals are often found in pressure treated wood.
EXAMPLES 1-4
[0019] The coatings described are all two part fluids that were combined during application and cured to give hard durable surfaces. There was an “A” formulation containing the isocyanate materials and a “B” formulation containing the amines and polyols. The catalyst can be placed in either the “A” or “B” formulations depending on the catalyst used. The “A” and “B” formulations were combined via high pressure impingement mixing, static tube mixing or some other rapid mixing device. Immediately after mixing, the fluids were applied to the desired surface by high pressure spraying, squeegee spreading or some other method or combination of methods. The same isocyanate “A” formulation was used for all four coatings, each with a different B formulation. The coatings were prepared as follows:
[0020] “A” formulation for Examples 1- 4
% by Weight in Final Coating Isocyanate Trimer 40.0 Isocyanate Dimer 9.0 Zirconium catalyst 2.0 Example 1 “B” formulation 1,3-Bis-Aminomethyl Cyclohexane 8.0 Polyether polyol 20.0 Polyester polyol 1 10.5 Polyester polyol 2 10.5 Example 2 “B” formulation Menthanediamine 5.0 Polyether polyol 21.0 Polyester polyol 1 11.5 Polyester polyol 2 11.5 Example 3 “B” formulation Polyoxypropylenctriamine 5.0 Polyether polyol 21.0 Polyester polyol 1 11.5 Polyester polyol 2 11.5 Example 4 “B” formulation 2-methylpentamethylenediamine 5.0 Polyether polyol 21.0 Polyester polyol 1 11.5 Polyester polyol 2 11.5
[0021] The “A” and “B” formulation fluids were combined via a static mixing apparatus and applied to a desired surface and then spread with a squeegee, or the “A” and “B” formulation fluids were combined via a high pressure mixing unit such as the Glas-Craft MX Probler mixing gun. The final coating thickness in each case was from about 2 Omil to 4 Omil.
EXAMPLE 5
[0022] Four samples of pressure treated wood were tested for arsenic at the wood surface. Samples 1 and 2 were pieces of wood pressure treated in a laboratory, with Sample 1 being uncoated and Sample 2 having a polyurethane/polyurea protective coating of the present invention. Samples 3 and 4 were pieces of pressure treated decking from a test site, with Sample 3 being uncoated and Sample 4 being coated with a polyurethane/polyurea protective coating in accordance with the present invention. Each of Samples 1-4 were wiped with a test wipe from a testing kit for arsenic treated wood, and then analyzed using SW-846 Test Methods for Evaluating Solid Waste Physical/Chemical Methods, with the arsenic determination being by EPA Method 7060A, Atomic Absorption, Furnace Technique, September 1994. The amount of arsenic detected at the surface of each wood sample by the wipe was determined to be as follows:
Sample 1 - uncoated 101.7 mg/100 cm 2 of arsenic Sample 2 - coated 0.7 mg/100 cm 2 of arsenic Sample 3 - uncoated 49.7 mg/100 cm 2 of arsenic Sample 4 - coated <0.3 mg/100 cm 2 of arsenic
[0023] The foregoing results show the effectiveness of the protective coating of the present invention in containing the arsenic from a pressure treatment within the wood.
[0024] While the invention has been described with prepared embodiments, it is to be understood that variations and modification may be resorted to as will be apparent to those skilled in the art. Such variations and modifications are to be considered within the purview and the scope of the claims appended hereto. | An aliphatic hybrid polyurethane/polyurea protective coating intended for use on concrete, steel, wood and other surfaces is provided, which coating exhibits excellent properties of durability and flexibility. The protective coating uses chemical components from urethane/urea systems in a unique way to generate beneficial systems. | 8 |
This is a continuation of application Ser. No. 07/271,538, filed Nov. 15, 1988 which is now U.S. Pat. No. 4,968,522.
BACKGROUND OF THE INVENTION
Browning agents for foodstuffs have been prepared and, when added to or coated onto foodstuffs, facilitate the browning thereof during cooking. Browning agents generally are intended to achieve the effect of natural browning reactions of food during conventional cooking as caused by the well known Maillard reaction which is the reaction between reducing sugars and amino acids of the proteins in the food. The Maillard reaction occurs at normal cooking temperatures and is dependent on a number of factors such as temperature, pH, concentration, water activity, oxygen supply, and nature of the raw materials, among other factors. A number of patents have issued directed to browning agents for foodstuffs having carbonyl-containing components for the browning reaction and, in particular, as microwavable browning coatings including U.S. Pat. No. 4,448,791; Japanese Patents 46-30772 (1971) and 48-16179 (1973); and European Patent Application 0 203 725 (1986). These patent publications are directed to browning agents and compositions that depend upon the reaction of an amino acid and sugar, especially as the reaction may be catalyzed by the addition of alkali to allow the reaction to take place at lower temperatures.
The present state of the art demands further improvements to be made in browning agents. Browning agents are needed that do not introduce an undesirable flavor into the foodstuff being browned. Furthermore, foodstuffs that contain available browning ingredients tend to discolor upon storage prior to use. It is not uncommon for even frozen foodstuffs that are flour-based to start discoloration in frozen storage, and some even turn black thereby tending to look spoiled. There is a definite need for storable foodstuffs containing browning agents that look attractive and yet may be quickly heated and browned even under the most demanding conditions of microwave ovens.
SUMMARY OF THE INVENTION
This invention is directed to a browning agent for foodstuffs having a carbonyl-containing browning reactant that overcomes the several problems confronting browning compositions according to the current state of the art. The browning agent of this invention is a water-in-oil emulsion containing water in the discontinuous phase and oil in the continuous phase. A surfactant is present for stabilization of the emulsion and an edible base is contained in the aqueous phase to induce the browning reaction upon heating foodstuffs having the carbonyl-containing reactant. The emulsion is adapted for incorporation into or coating onto foodstuffs that contain the carbonyl reactant that induces browning upon heating.
In a preferred form of the invention, the water-in-oil emulsion contains an edible base that provides a pH on the order of about 8-13 in the emulsion to obtain a desired browning reaction within a reasonable time and to provide an edible product. Below a pH of about 8, the reaction is slower at a given temperature and, above pH 13, the product would not have current governmental food approval. Foodstuffs having carbonyl-containing browning reactants that may be browned include natural ingredients such as flours, carbohydrates and the like, having the necessary reactants such as reducing sugars, reducing sugars and amino acids, carbonyls derived from lipids, and the like components that may react under heat. These reactants are well known and may also be present in other foodstuffs such as meats. Biscuits, pizza, hash brown potatoes, and other such foodstuffs may be browned with the browning agent of this invention. Furthermore, it has been found that the browning agent of this invention may be incorporated into or coated onto such foodstuffs, placed in colder frozen storage at about -30° C. to 10° C., and removed for direct microwave browning. It has been found that discoloration normally occurring in prior art foodstuffs upon storage is eliminated.
This invention will be further understood along with its benefits and advantages with reference to the following detailed description.
DETAILED DESCRIPTION
The browning agent of this invention is suitable for use with foodstuffs having carbonyl-containing browning reactants exemplified by those foodstuffs naturally containing brownable mono- and polysaccharides, especially reducing sugars with or without amino acids, that are known to induce browning. The water-in-oil or inverted fat emulsions suitable for use according to the principles of this invention contain water in the discontinuous phase and oil in the continuous phase. A surfactant stabilizes the emulsion and an edible base is contained in the aqueous phase. The edible base is protected in the inverted emulsion against transfer into the surrounding matrix and reaction with a carbonyl or carbonyl-amino acid reaction system in the foodstuff until cooking. Under the action of heat during the normal cooking cycle, the emulsion breaks down causing the base to come into contact with the browning reactants whereby browning occurs upon cooking. Thus, the very desirable features of preventing a pre-reaction of reactants upon storage are achieved by the encapsulated browning agent of this invention. The colored or spoiled appearance normally associated with products provided according to known techniques is avoided by the utilization of browning agents of this invention.
The oil or fat suitable for use in the inverted emulsions of this invention include any edible oil or fat. As suitable examples, vegetable oils or vegetable fats can be employed. Any edible base may be used including potassium carbonate, sodium carbonate, trisodium phosphate or the like. Such edible bases in aqueous media provide pHs on the order of about 8-13. In its most preferred form, the water-in-oil (W/O) emulsion is made with a concentrated solution of the materials so as to provide long term stability to the product. The term "emulsion" is used herein to define the inverted state of water in oil, but it is to be understood that such state may be a dispersion, especially where the phases are not as distinct such as in microemulsions. The inverted emulsions are made according to well known fat or oil emulsification techniques that form no particular part of this invention. Preferably, emulsification or dispersion is achieved such that the inverts are opaque or as transparent as possible, normally in a state of emulsification or dispersion achieved in microemulsions. Emulsions thus may exist as soft solids or viscous liquids at room temperature and would tend to be off-white or clear in color. The relatively colorless nature of the browning agents of this invention offers a substantial advantage over those compositions that have been dyed in the past or provide undesirable colors to the foodstuffs that are being prepared. The agents of this invention provide neutral colors and neutral flavors that are undetectable in the prepared and stored foodstuffs and yet provide a desirable browning effect during cooking. As indicated above, the browning agents of this invention are especially suitable for use under the demanding conditions of microwave heating. They may also be heated in a conventional oven. An edible surfactant is necessary in the composition in order to stabilize the emulsion. Any available surfactant is suitable for this purpose especially nonionic surfactants including mono- or poly-fatty acid esters of glycerol as exemplified by mono- or di-(C 10 -C 18 ) fatty acid glycerides that are well known and available for use. Other ionic surfactants such as soaps of fatty acids and phospholipids (e.g., lecithin) may be employed.
In this specification, the terms "oil" and "fat" are used synonymously. Such fatty materials may be liquid, soft solid, or solid at room temperature, and would soften or liquify upon heating. Fats, however, may include hard fats selected from animal fats and vegetable or fish oils. Hard fats may be selected from coconut oil, corn oil, cottonseed oil, fatty-pork tissue, lard, palm oil, shortenings, safflower oil, sunflower oil, tallow or any mixtures or equivalents thereof. It is to be understood, however, that the fat may have liquid oils ultimately mixed with hard fats so long as they are capable of forming the inverted fat emulsion of this invention. Preferred liquid oils include coconut oil, corn oil, cottonseed oil, safflower oil, soybean oil, sunflower oil, or mixtures or equivalents thereof. It is to be understood when it is desirable to confer certain animal flavor notes to foodstuffs, in addition to browning, fatty materials may be selected from those fats derived from animals. On the other hand, where more neutral or other flavoring is to be achieved, vegetable oils may be employed.
In preparing the browning agent emulsions, the amounts of ingredients may be varied by including on a parts by weight basis about 10-90% fat, and about 10-30% water, and about 5-10% base. These ingredients vary over wide ranges depending upon the food being browned. The above ingredients are emulsified stabilized with a surfactant on the order of about 1-50% by weight. Preferably, stabilized browning emulsions may be formulated containing about 67.5% fat, 21% water, 9% base, and 2.5% surfactant. It will become apparent to a person of ordinary skill in the art that variations of ingredients in the emulsions may be achieved. Specific operating examples of this invention that illustrate its practice are as follows.
EXAMPLES
A browning agent emulsion of this invention was prepared by mixing the ingredients listed below.
TABLE I______________________________________ Example (% By Weight)Ingredients A B C______________________________________Fat 67.5 64 65.5Water 21 21 21Base 9 9 9Water Soluble Surfactant .5 -- --Santone 8-1-0Fat Soluble SurfactantDurem 204 2.0 -- 2.0Lecithin -- -- 2.5Sodium Caprylate -- 6 -- 100.0 100 100.0______________________________________
According to the above listing, the fat employed was a vegetable fat having a melting point of about 92° F. as supplied by Anderson Clayton. The base employed was a food grade potassium carbonate as made up in a solution with the water. The surfactants employed were Durem 204 supplied by Durkee and Santone 8-1-0 supplied by Durkee. Santone 8-1-0 is an octaglycerol monooleate. Durem-204 is about 50% glycerol monooleate in the α position with the remainder being monooleate in the β position as well as some mono, di and triglycerides containing palmitic, stearic and oleic acids.
The browning agent emulsion was manufactured by heating the fat and fat soluble surfactant to about 102° F. in order to provide a melt. In Example A, the potassium carbonate was added to water followed by the addition of Santone 8-1-0 with blending until the Santone 8-1-0 was dissolved. Then, the fat mixture with Durem 204 was slowly added to the water/carbonate/Santone 8-1-0 ester solution while agitating until all of the fat mixture had been added. In Examples B and C, each fat mixture was slowly added to the water and base. Mixing of each Example continued with removal of the source of heat until room temperature was reached. The finished products had the consistency of soft margarine and appeared white in color. The browning agent emulsions can be stored at room temperature for up to several months.
In order to determine the affect of browning agents made in accordance with Examples A-C and the principles of this invention, pizza dough and potpie crusts were prepared for coating with the browning agent. The pizza dough compositions were prepared by combining the following ingredients.
TABLE II______________________________________ Weight (g)Component (1) (2)______________________________________Wheat Flour 618.2 618.2Water 346.1 346.1Vegetable Oil 9.3 9.3Sugar (Sucrose) 13.7 --Yeast 5.9 5.9Salt 6.8 6.8Dextrose -- 13.7 1000.0 1000.0______________________________________
The dry components of the Table II were combined and mixed in a commercial mixer unit to form a uniform blend. To this blend was added the oil with mixing, then the water at low mixing speed until the flour became wet. The total mixture was then kneaded at medium to high speed for about 5 or 6 minutes and fermented 1 to 1.5 hours. The dough was let to stand for about 3 minutes, followed by formation of the shaped pizza base.
The browning agents made according to the above TABLE I were then brushed onto the pizza shaped dough and then introduced into frozen storage that may extend up to about six months. The frozen pizzas were then cooked in a microwave oven. The pizza crust containing the browning agent had a very attractive appearance upon removal from storage and, upon microwave cooking, developed an excellent browning appearance upon microwave heating.
Fruit and potpies containing a covering of a flour base foodstuff were prepared from a pie covering formulation listed below.
TABLE III______________________________________Flour 52.0Salt 1.5Dextrose 2.5HydrogenatedShortening 26.0Water 18.0 100%______________________________________
The ingredients for this formulation were combined in the following manner. The dry components were weighed and mixed until uniform. The shortening was then folded into the dry mix and stirred until uniform. Then, water was added and thoroughly mixed with the dry mix containing shortening. The resulting dough mass for each formulation was then formed into a circular top crust, added to a conventional 8 oz. potpie and then stored in a freezer for at least about 48 hours. The frozen potpies were later removed from storage and cooked in a 600 watt microwave oven for about 9 mins. Optionally the formulations may contain flavoring. Prior to the introduction into frozen storage and microwaving, the potpies were coated by brushing on the browning agent of TABLE I produced above. The cooked crust sheets were then evaluated for their appearance after removal from storage and upon microwave cooking. Upon removal from storage, the crust looked very attractive and, after microwave cooking, the crusts provided an excellent browned appearance. The browning agent thus produces excellent results on high fat dough products of the pot pie, tater tot and the like variety.
Having described the invention and its various parameters, other modifications will become apparent to a person of ordinary skill in the art without departing from the scope of this invention. | A browning agent for foodstuffs having a carbonyl-containing browning reactant is disclosed comprising a water-in-oil emulsion, a surfactant and an edible base in the aqueous phase adapted to enduce a browning reaction in the foodstuff upon heating. The browning agent may be coated onto foodstuffs such as biscuits, pizza, pie coverings or hash brown potatoes, stored at temperatures from about -30° C. to about 10° C. thereafter immediately microwaved to enduce browning. | 0 |
FIELD OF THE INVENTION
The present invention relates to a process for the preparation of 13-cis isomer of Vitamin A acid, commonly known as isotretinoin, in a single step.
BACKGROUND OF THE INVENTION
Isotretinoin (13-cis retinoic acid) belongs to a family of Vitamin A (retinol) related compounds. It inhibits sebaceous gland function and keratinization and is used for the treatment of dermatological diseases like acne. It is extremely effective in very severe and nodulocystic acne and prevents scarring. More recently, isotretinoin has also been evaluated for its potential use in certain cancerous conditions.
Structurally, isotretinoin is a highly conjugated molecule consisting of a substituted cyclohexene moiety and a nine-carbon polyene side chain with a terminal carboxy group. All but one of the double bonds (C-13 double bond) in the side chain are trans and it is the stereospecific construction of this polyene side chain which has challenged synthetic organic chemist for the last almost three decades. Commercially and readily available β-ionone has been conveniently used for the construction of the cyclohexene part of isotretinoin. The synthetic prior art approaches for the construction of the polyene side chain are summarized below.
In general, a convergent approach, involving stereospecific coupling of the appropriate C 15 (synthesized from β-ionone) and C 5 synthons, has been utilized. (however, a linear sequence comprising of seven steps, starting from β-ionone, has also been described; J Org. Chem. 54, 2620-2628, 1989). For example, Patternden and Weedon, J. Chem. Soc.(C), 1984-97 (1968) have disclosed a procedure for the preparation of 13-cis retinoic acid by reacting a C 15 -triarylphosphonium salt (Wittig salt) and a C 5 -butenolide in diethylether to produce an isomeric mixture (of the cis and trans isomers at C-11 double bond) of 13-cis retinoic acid in 66-75% yield; the desired 11-trans-13-cis content is only about 36% and the rest being the corresponding 11,13-di cis isomer. Selective isomerization of the 11-cis double bond in the presence of 13-cis double bond proved extremely difficult to accomplish. A great deal of effort has been directed to affect selective isomerization of 11-cis double bond (without isomerizing the 13-cis double bond) in 11,13-di cis retinoic acid. The methods include photoisomerisation by using either iodine (J. Chem. Soc. (C) 1982, 1968), transition metal catalysts (U.S. Pat. No. 4,556,518) or photosensitizers such as erythrosin B, rose Bengal etc. (U.S. Pat. No. 5,424,465). These processes suffer from the following limitations and for various reasons are not suitable for commercial production of isotretinoin. For example, the process for selective photoisomerization using iodine under diffused light is extremely difficult to accomplish without affecting the 13-cis double bond. This results in the generation of all trans retinoic acid (tretinoin) as a major impurity in isotretinoin produced by this process. Although, U.S. Pat. No. 5,424,465 describe that use of photosensitizers enhances selectivity of photoisomerisation of C 11 -cis double bond, no data, however, is provided for the extent of tretinoin formation in this process.
The use of the palladium catalysts, as described in U.S. Pat. No. 4,556,518, could potentially lead to the contamination of the desired isotretinoin with traces of transition metals and thereby might lead to problems with the stability. In addition, the process involves an elaborate extraction procedure for the work-up.
U.S. Pat. No. 4,916,250 describes a process involving use of a phosphonate ester (as a C 15 synthon), which is first generated in several steps starting from β-ionone. The phosphonate ester is then reacted with 5-hydroxy-4-methyl-2- (5H)-furanone (C 5 synthon) to afford isotretinoin. Although this approach does not involve the cumbersome photoisomerization step, it is uneconomical at a commercial manufacturing scale because of the large number of steps.
Cainelli et al, Gazz. Chim. Ital, 103, 117-125 (1973) reported the synthesis of isotretinoin by reacting a dienolate of sodium 3,3-dimethyl acrylate (C 5 -synthon) with β-ionylideneacetaldeyhyde (C 15 synthons) at −78° C. for twelve hours to give a hydroxy acid intermediate. The hydroxy acid intermediate on conversion to intermediate lactone and subsequent treatment with base afforded isotretinoin. This approach suffers from the following limitations two different bases (sodium hydride and lithium diisopropylamide) are required and moreover generation of dienolate requires maintaining low temperatures (−78° C.) for extended periods of time, which would entail very high energy costs at the commercial scale. Furthermore, the purification of the intermediate lactone by preparative High Performance Liquid Chromatography, as suggested, is not commercially feasible.
SUMMARY OF THE INVENTION
It is an object of the present invention to solve the problems associated with the prior art and to provide an efficient method for the synthesis of isotretinoin of high purity in one single step (stereospecific coupling of C 15 and C 5 synthons) using conditions which are convenient to operate on a commercial scale.
It is a further object of the present invention to provide a process which affords isotretinoin while controlling the levels of tretinoin to <0.1%. Various pharmacopoeias have prescribed a 1-2% limit of this impurity in isotretinoin.
The present invention is directed to a process for the preparation of isotretinoin, which comprises the condensation of dienolate of methyl-3,3-dimethylacrylate of Formula I:
with β-ionylideneacetaldehyde of Formula II:
in a suitable solvent at (I) −60° C. to −80° C. for 1-2 hours and (ii) 25° C.-45° C. for 1-24 hours, followed by aqueous acidic work up to give isotretinoin in a single step.
The condensation reaction proceeds via the formation of the intermediate lactone of Formula III:
which is not isolated. Lactonization results in the release of a methoxide ion which in turn opens the lactone to afford isotretinoin (as carboxylate salt); the reaction of methoxide and lactone is facilitated by higher temperatures (25-45° C.) and by carrying the reaction for longer time. Aqueous acidic work up thus produces isotretinoin in one single step starting from β-ionylidene acetaldehyde.
Generally, the initial condensation of dienolate of methyl-3,3-dimethyl acrylate of Formula I shown above with β-ionylidene-acetaldehyde of Formula-II above is carried out at −60° C. to −80° C. for 1-2 hours. Preferably, it is carried out at −65° C. to −75° C. Temperature is later raised to about 25° C.-45° C., preferably between 30-40° C. and is maintained for 1-24 hours and the progress of the reaction is monitored. Suitable solvents include tetrahydrofuran, 1,4-dioxane, hexanes, diisopropyl ether, hexamethyl-phosphoramide, tetramethylurea, and mixtures thereof. Tetrahydrofuran is a preferred solvent.
Aqueous acidic work up involves the adjustment of pH with mineral acids and extraction with organic solvents. Acids may include hydrochloric acid, sulfuric acid, and phosphoric acid. Sulfuric acid being the preferred acid. Any organic solvent may be used for extraction and such solvents are known to a person of ordinary skill in the art and include: water-immiscible solvents, such as chloroform, dichloromethane, 1,2-dichloroethane, hexane, toluene, ethyl acetate and the like.
Other features of the invention will become apparent in the course of the following description of exemplary embodiment, which is given for illustration of the invention, and are not intended to be limiting thereof.
DETAILED DESCRIPTION OF THE INVENTION
EXAMPLE 1
Under an atmosphere of nitrogen, a solution of n-butyl lithium in hexane (321 ml, 15%) was added to a solution of diisopropylamine (48.6 g, 0.48 mole) in tetrahydrofuran (1000 ml) at −30° C. and the mixture was stirred for one hour. The reaction mixture was then cooled to −72° C. and methyl 3,3-dimethyl acrylate (55 g, 0.48 mole) was added to it. Stirring was continued at −65 to −75° C. for 30 minutes. To the resulting mixture, a solution of β-ionylidene acetaldehyde (100 g, 0.458 mole, 9-trans content: 80%) was added and the reaction mixture was stirred at −65 to −75° C. for one hour. The reaction mixture was then warmed to 40° C. and stirred at this temperature for three hours. Solvent was removed under vacuum and the reaction mixture was diluted with water (700 ml) and methanol (300 ml). Activated charcoal (4 g) was then added and the mixture was refluxed for 30 minutes. The heterogeneous mixture was filtered through hyflo and the hyflo bed was washed with methanol (300 ml) and water (150 ml). The aqueous methanolic layer was then extracted with hexanes (2×500 ml) and acidified with 10% sulfuric acid to pH 2.8±0.5. The desired product was then extracted with dichloromethane (2×500 ml). The combined dichloromethane layer was washed with water (2×300 ml) and concentrated in vacuo to afford the desired isotretinoin. Crystallization from methanol (200 ml) afforded isotretinoin (44 g) in greater than 99% HPLC purity; the tretinoin content was less than 0.1% by HPLC.
EXAMPLE 2
Under an atmosphere of nitrogen, a solution of n-butyl lithium in hexane (20 ml, 15%) was added to a solution of diisopropylamine (2.7 g, 0.027 mole) in diisopropyl ether (10 ml) at −74° C. and the reaction mixture stirred for 0.5 hour. To this, methyl 3,3-dimethyl acrylate (2.51 g, 0.022 mole) was added at −74° C. Stirring was continued at −70° C.±2° for 30 minutes and the reaction mixture was added to a solution of β-ionylidene acetaldehyde (5 g, 0.022 mole, 9-trans content: 80%) in diisopropyl ether (20 ml) at −74° C. The reaction mixture was stirred for 1 hour at −72° C.±2° and then slowly allowed to warm to room temperature. The reaction mixture was stirred at ambient temperature overnight and worked up as per the procedure given in example 1 to afford 1.03 g of pure isotretinoin.
While the present invention has been described in terms of its specific embodiments, certain modifications and equivalents will be apparent to those skilled in the art and are intended to be included within the scope of the present invention. | The present invention relates to a process for the preparation of 13-cis isomer of Vitamin A acid, commonly known as isotretinoin, in a single step. | 2 |
FIELD OF INVENTION The present invention relates to a rotor for an aircraft and to a helicopter.
BACKGROUND OF THE INVENTION
[0001] Rotor blades of a helicopter can be rigidly fastened to a rotor mast by means of a resilient blade neck. The resilient blade neck can permit defined movements in an impact, pivot or rotational direction. Conventionally, a sleeve is attached over the resilient blade neck, the outside of which sleeve is firmly connected to the profile of the blade. A control rod is also arranged inside said sleeve, close to the rotor mast, the movements of which control rod causes the sleeve to rotate and the profile of the blade to change. The control movements of the control rod can be produced by a compound gear and a swashplate.
[0002] The German patent document DE 197 45 330 C1 relates to a rotor blade connection comprising a support arm which connects the rotor blade to the rotor hub, wherein the support arm has an open convex cross section and comprises piezoelectric solid elements fastened to the support arm.
[0003] DE 10 2008 036 760 A1 relates to a rotary actuator comprising at least one strip-shaped passive support layer which can be bent in a reversible manner The support layer comprises, in the support layer longitudinal direction, an active actuator coating that is applied to the support layer and can expand and/or contract in the support layer longitudinal direction upon activation.
[0004] US 2004/0017129 A1 relates to electroactive devices comprising an electroactive structure which extends along a minor axis and is curved around a main axis. This electroactive structure comprises electroactive parts which extend around the minor axis.
[0005] DE 10 2010 042 223 A1 describes a torque-generating device which comprises a torque-generating element that is substantially spirally and/or helically arranged about an axis of rotation of the torque to be generated and that comprises at least one piezo element for generating the torque.
BRIEF SUMMARY OF THE INVENTION
[0006] The invention relates to a helical actuator for controlling a rotor blade of an aircraft. The actuator comprises a plurality of piezo elements arranged in series in order to adjust the rotor blade when a control voltage is applied to the piezo elements.
[0007] The helical actuator is an actuator in the shape of a helix. A helix can be described as a curve that winds around the lateral surface of a cylinder at a constant pitch.
[0008] The aircraft may be a helicopter, an aeroplane or an airship.
[0009] Propellers of aircraft can also be controlled by means of the helical actuator.
[0010] Piezo elements are understood to mean components that perform a mechanical movement, particularly an expansion or a contraction, when an electrical voltage is applied. These piezoelectric elements are for example piezo crystals or piezoelectric ceramics.
[0011] A serial arrangement of piezo elements means for example a stacked arrangement of the piezo elements, in which the piezo elements are arranged in series one on top of the other. In other words, a “serial arrangement” means a layered arrangement of piezo elements. Electrodes are for example arranged between the individual piezo elements. This means that an electrode is arranged between two adjacent piezo elements in each case. In order to actuate the actuator, a voltage is applied between two adjacent electrodes in each case.
[0012] For example, the actuator comprises a cascading of piezo elements in that a plurality of thin piezo elements having electrodes arranged therebetween are joined together. This results in a mechanical series arrangement actuated by an electric parallel connection. To achieve this, the following pattern can be applied: Firstly, an electrode (e.g. a cathode), a piezo element, then another electrode (e.g. an anode), and finally another piezo element having a modified direction of polarisation are arranged one on top of the other in an alternating manner. This arrangement can be repeated a number of times.
[0013] An advantage of a serial, stacked or layered arrangement is that the mechanical expansions of the individual piezo elements are added together. This means that the overall expansion of the actuator can be approximately equal to the expansion of an individual piezo element multiplied by the number of piezo elements. Therefore, an expansion of the actuator can be produced which is great enough to cause the rotor blade to be adjusted.
[0014] One advantage of a helical actuator for controlling a rotor blade of an aircraft can be considered to be that a large part of the mechanical control installation, for example the compound gear or the swashplate, is not required. Furthermore, an actuator consisting of piezo elements can be operated very quietly, and therefore the noise generated by the rotating rotor blade can be minimised. Moreover, owing to the helical actuator consisting of piezo elements, it is possible to control a rotor blade in a highly dynamic manner Actuating the rotor blades by means of an electrically operated actuator consisting of piezo elements involves few components and can be achieved in an economical manner.
[0015] According to one embodiment of the invention, each of the piezo elements has an expansion direction which is parallel to a helical direction of the actuator.
[0016] The expansion direction corresponds for example to the direction in which the piezo elements expand when a control voltage is applied. This means that the piezo elements of the actuator expand in the helical direction when the control voltage is applied. By way of example, the expansion direction of the piezo elements is a thickness direction.
[0017] This means that the thickness direction of the piezo elements is parallel to the helical direction.
[0018] In this case, the helical direction is the direction of the helical actuator, i.e. the direction of the helix in which the actuator is arranged. In other words, the helical direction at each point on the helix is a direction which is tangential to the helix.
[0019] Since the expansion direction of the piezo elements can be substantially parallel to the helical direction, the helical actuator as a whole also expands in the helical direction. A movement of the rotor blade substantially in the helical direction can be produced by means of the actuator. This means that a rotor blade to which a helical actuator is connected can rotate about a central axis of the actuator, about which the actuator winds.
[0020] According to another embodiment of the invention, the actuator winds around a volume of space along a central axis of the actuator.
[0021] In this case, the central axis is an axis in the longitudinal direction of the helical actuator. In other words, the helical actuator winds around its central axis.
[0022] A resilient rotor blade neck of a rotor can for example be located in this volume of space. This means that a further element, e.g. a rotor blade neck, can be located in the volume of space of the helical actuator.
[0023] According to another embodiment of the invention, the actuator comprises at least 100 piezo elements.
[0024] By way of example, the actuator comprises piezo elements which each have a thickness of between 0.2 mm and 1.0 mm in the helical direction. In other words, the actuator contains stacked small plates or discs consisting of piezo elements which are arranged perpendicularly to the helical direction, i.e. the plane which defines each of the small plates is arranged perpendicularly to the helical direction. In each case, the piezo elements expand in the thickness direction of said piezo elements.
[0025] According to another embodiment of the invention, the piezo elements are surrounded by a fibre composite material. This could for example be a matrix made of a fibre composite fabric.
[0026] In this case, the fibre composite material surrounding the piezo elements defines the helix shape of the actuator. Furthermore, the fibre composite material is flexible, and therefore the piezo elements can expand and the actuator as a whole can also expand. Moreover, wires or other electric conductors can be built into the fibre composite material in order to apply the control voltage to the piezo elements.
[0027] According to another embodiment of the invention, the actuator comprises at least three turns.
[0028] According to another embodiment of the invention, applying a control voltage to the piezo elements causes the actuator to expand in a helical direction of the actuator.
[0029] The invention also relates to a rotor for an aircraft, comprising at least one rotor blade. The rotor further comprises a rotor blade connection which is designed to connect the rotor blade to the rotor mast. The rotor further comprises a resilient blade neck which connects the rotor blade to the rotor blade connection and allows the rotor blade to rotate about an axis of rotation in the longitudinal direction of the rotor blade. The rotor also comprises a helical actuator as described above and below which is arranged so as to wind around the rotor blade neck.
[0030] In general, the rotor may also be a propeller.
[0031] By way of example, the rotor comprises a rotor mast and four rotor blades which are each connected to the rotor mast.
[0032] The rotor blade connection may be a component to which the rotor blade is connected by means of the rotor blade neck. Alternatively, the rotor blade connection can also be an end of a rotor blade which connects the rotor blade to the rotor mast or at which the rotor blade can be connected to the rotor mast. The rotor blade connection is connected to the rotor mast by screws or bolts for example. On the other hand, the rotor blade neck can be a component which is arranged between the rotor blade connection and the rotor blade, and therefore the rotor blade neck connects the rotor blade to the rotor blade connection. The rotor blade, rotor blade neck and rotor blade connection can also be different regions of a one-piece component.
[0033] In the process, the rotor blade neck permits a movement in the rotational direction about an axis of rotation of the rotor blade. The axis of rotation of the rotor blade is an axis of the rotor blade which extends in the longitudinal direction of the rotor blade. In other words, the rotor blade expands to the greatest degree in the direction of the axis of rotation. For example, the axis of rotation of the rotor blade can be substantially perpendicular to a rotation axis of the rotor mast. A rotational movement of the rotor blade can also be a rotary movement of the rotor blade about the axis of rotation of the rotor blade.
[0034] Such a rotational movement of the rotor blade about the axis of rotation of the rotor blade can be produced by means of the helical actuator. The lift and/or forwards thrust of the rotor can thus be controlled by means of this actuator.
[0035] According to the invention, the helical actuator is fastened by a first end to the rotor mast and by a second end to the rotor blade.
[0036] In other words, the actuator is firmly connected to the rotor mast and the rotor blade, and therefore a force from the actuator is transmitted to the rotor mast and/or the rotor blade. For example, owing to this connection, the actuator pushes away from the rotor mast and transfers its expansion to the rotor blade, thus producing a rotational movement of the rotor blade.
[0037] According to another embodiment of the invention, the helical actuator is fastened to the rotor blade at a distance from the axis of rotation of the rotor blade, which axis extends in the longitudinal direction of the rotor.
[0038] Owing to this distance between the fastening of the actuator to the rotor blade and the axis of rotation of the rotor blade, the actuator has a lever for rotating the rotor blade about the axis thereof. This lever corresponds to the distance between the point where the actuator is fastened to the rotor blade and the axis of rotation of the rotor blade.
[0039] According to another embodiment of the invention, the helical actuator circulates around the blade neck at least three times.
[0040] According to another embodiment of the invention, the rotor blade is made to rotate when a control voltage is applied to the helical actuator.
[0041] The invention also relates to a helicopter comprising at least one rotor as described above and below.
[0042] For example, it relates to an electrically driven helicopter which comprises electric motors for driving one or more rotors. The helicopter may also be a fuel-operated helicopter, the rotor blades of which are actuated by means of helical actuators. The helicopter may also be a model helicopter or a drone.
[0043] Further features, advantages and possible uses of the invention can be found in the following description of the embodiments and figures. Here, all the described and/or illustrated features form, per se and in any combination, the subject matter of the invention, regardless of how they are combined in the individual claims or their dependency references.
BRIEF DESCRIPTION OF THE DRAWINGS
[0044] FIG. 1 shows a helical actuator according to an embodiment of the invention.
[0045] FIG. 2 shows a rotor having a helical actuator according to an embodiment of the invention.
[0046] FIG. 3 shows a helicopter according to an embodiment of the invention.
[0047] The figures are schematic and are not true to scale. If, in the following description, the same reference numerals are used in different figures, said reference numerals identify identical or similar elements. However, identical or similar elements can also be identified by different reference numerals.
DETAILED DESCRIPTION
[0048] FIG. 1 shows a helical actuator 100 according to an embodiment of the invention. The helical actuator 100 is shaped like a helix which is arranged about a central axis 101 . At the same time, the central axis 101 also defines the longitudinal direction 101 of the helical actuator 100 . Furthermore, the helical actuator defines a helical direction 102 which points in the direction of the helix, in which direction the actuator 100 is arranged. Moreover, a volume of space 103 is located inside the actuator 100 along the central axis 101 of the actuator, around which volume of space the actuator 100 winds.
[0049] The helical actuator comprises a plurality of piezo elements arranged in series, i.e. one on top of the other. By way of example, three piezo elements 104 , 105 , 106 arranged one on top of the other are shown.
[0050] In the present embodiment, the helical actuator has three complete turns 107 , 108 , 109 and one half turn adjacent to the turn 109 .
[0051] Applying a control voltage to the piezo elements 104 , 105 and 106 causes the individual piezo elements 104 , 105 , 106 to expand in the helical direction 102 . As a whole, this results in an expansion 110 of the actuator 100 in the helical direction 102 , which expansion is for example equal to the expansion of an individual piezo element multiplied by the number of piezo elements. In FIG. 1 , the expansion 110 of the actuator is shown by a dashed line.
[0052] When the control voltage is applied to the actuator 100 , the actuator expands such that the shape thereof includes the solid line and the expansion 110 represented by the dashed line. If no control voltage is applied, the actuator 100 has the shape as shown by the solid line.
[0053] FIG. 2 shows a rotor 200 according to an embodiment of the invention. The rotor may comprise a rotor mast 204 to which a rotor blade 201 is connected. In this case, a rotor blade neck 202 connects the rotor blade 201 to a rotor blade connection 203 which is connected to the rotor mast 204 . In the present embodiment, the rotor blade connection is an end of the rotor blade neck 202 and is clamped between a lower fastening plate 205 and an upper fastening plate 206 . Furthermore, the rotor blade connection 203 is connected to the lower fastening plate 205 and the upper fastening plate 206 by bolts 208 and 209 .
[0054] In addition to the rotor blade 201 , three further rotor blades (not shown) can be attached to the rotor mast 204 .
[0055] A helical actuator 100 is arranged around the rotor blade neck 202 and winds around the rotor mast 204 . Furthermore, the actuator 100 is fastened to the rotor mast 204 . In the present embodiment, the actuator is fastened to the upper fastening plate 206 by means of a fastening element 212 . The actuator 100 is also fastened to the rotor blade 201 by means of a fastening element 213 . The rotor blade has an axis of rotation 210 which extends in the longitudinal direction of the rotor blade. The helical actuator 100 is arranged at a distance 214 from this axis of rotation 210 of the rotor blade 201 , and therefore the helical actuator applies a leverage force to the rotor blade 201 relative to the axis of rotation 210 .
[0056] FIG. 2 shows different axes and directions. The rotor mast comprises a rotation axis 207 , about which the rotor mast rotates. The rotor blade also comprises an axis of rotation 210 as described above which extends in the longitudinal direction of the rotor blade. The rotation axis of the rotor mast 207 and the axis of rotation 210 of the rotor blade 201 are arranged substantially perpendicularly to one another. The helical direction 102 of the actuator is also shown which extends along a helix along which the actuator is arranged. A rotational direction 211 which the rotor blade 201 can follow is also shown. The rotational direction or rotational movement 211 corresponds substantially to a rotational movement and/or rotary movement about the axis of rotation 210 of the rotor blade 201 . A rotational movement 211 of the rotor blade 201 is produced by the control voltage being applied to the piezo elements 104 , 105 and 106 of the actuator 100 .
[0057] FIG. 3 shows a helicopter according to an embodiment of the invention. The helicopter 300 comprises a rotor 200 which, in this case, is a main rotor. The rotor 200 comprises for example four rotor blades, the three rotor blades 201 , 301 and 302 being visible in the present embodiment. The rotor blade 201 can be controlled by means of a helical actuator 100 , and the rotor blade 301 can be controlled by means of a helical actuator 303 . The additional rotor blades can also be controlled by means of helical actuators.
[0058] For completeness, it should be noted that “comprising” or “having” does not preclude other elements and “a” or “one” does not preclude a plurality. It should further be noted that features which have been described with reference to one of the above embodiments may also be used in combination with other features of other embodiments which are disclosed above. Reference numerals in the claims should not be considered to be limiting.
[0059] While at least one exemplary embodiment of the present invention(s) is disclosed herein, it should be understood that modifications, substitutions and alternatives may be apparent to one of ordinary skill in the art and can be made without departing from the scope of this disclosure. This disclosure is intended to cover any adaptations or variations of the exemplary embodiment(s). In addition, in this disclosure, the terms “comprise” or “comprising” do not exclude other elements or steps, the terms “a” or “one” do not exclude a plural number, and the term “or” means either or both. Furthermore, characteristics or steps which have been described may also be used in combination with other characteristics or steps and in any order unless the disclosure or context suggests otherwise. This disclosure hereby incorporates by reference the complete disclosure of any patent or application from which it claims benefit or priority. | A helical actuator includes a plurality of piezo elements for controlling a rotor blade of an aircraft. In this case, the actuator is designed to be arranged so as to be wound around a rotor blade neck and to be fastened to a rotor mast and a rotor blade in each case. Applying a control voltage to the piezo elements causes the actuator to expand, which, in turn, causes the rotor blade to rotate. | 1 |
FIELD OF THE INVENTION
The invention relates to a vehicle wash system comprising a plurality of wash units.
BACKGROUND OF THE INVENTION
As a rule, a vehicle wash system also has, apart from one or more horizontal height-adjustable wash units, such as, for example, roof brushes, additional height-adjustable treatment units in the form of horizontal drying nozzles or the like. Such horizontal treatment units are commonly moved by means of separate hoist drives independent of each other. As a rule, this occurs via a winder drive by means of cable drives or flat belt drives or by means of toothed belt drives with corresponding deflection means and counterweights. In this connection, each of the units, such as roof brushes or horizontal drying nozzles, is equipped with a dedicated hoist motor, that admittedly requires a correspondingly high cost for the drive and control thereof.
SUMMARY OF THE INVENTION
The problem of the invention is to create a vehicle wash system of the aforementioned type that, at a low cost for the control and drive thereof, enables a reliable cleaning and drying of a vehicle.
This problem is solved by means of a vehicle wash system having the features as set forth in the independent claim(s). Expedient improvements and advantageous embodiments of the invention are the object of the dependent claims.
An essential advantage of the vehicle wash system according to the invention is that a plurality of treatment units can be moved via a traction mechanism drive by means of a single drive motor. This can reduce the number of drive motors and lower the expenditure for control. In addition, the simplified drive concept enables a cost savings.
In a particularly expedient embodiment, the traction mechanism drive comprises a traction member and deflection rolls, via which the traction member is guided to one of the treatment units by a drive element set into rotation by the drive motor. Guidance of the traction member designed, for example, as a cable, belt or chain can be configured so that the drive motor is fastened in a stationary manner to the frame, wherein the traction member, starting from the drive motor, is guided first via a deflection roll on one of the treatment units in the manner of a loose roll of a pulley and furthermore deflected a second time via stationary deflection rolls on the frame and subsequently fastened to the second treatment unit.
In an alternative execution, the drive motor can however also be fastened to one of the two height-adjustable treatment units and the traction member guided from there to the second treatment unit only via stationary deflection rolls on the frame.
The drive can be designed, for example, as a winder drive, with one end of the traction member being wound on a drive roll set into rotation by the drive motor and the other end of the traction member being connected to the first treatment unit. The drive can also occur, particularly with the use of a chain or toothed belt as the traction member, via one deflection and a positive-fit drive element in the form of a sprocket wheel, belt pulley or the like.
Allocated to at least one of the treatment units is a locking arrangement, by means of which the respective treatment unit can be arrested in a preset end position, preferably the upper end position. Provided there is a sufficiently large weight difference between the treatment units, the locking arrangement can be provided only for the heavier treatment unit. However, corresponding locking arrangements can be mounted to both treatment units.
For a portal wash system the frame can be designed, for example, as a movable portal, wherein during cleaning, the wash brushes and drying nozzles, apart from a horizontal shifting, are also moved in the longitudinal direction of the vehicle. In the event of a vehicle wash plant in which a vehicle is moved in the longitudinal direction of the vehicle during cleaning, for example by means of a belt conveyor or chain conveyor, the frame can also be of a stationary execution.
BRIEF DESCRIPTION OF THE DRAWINGS
Additional distinctive features and advantages of the invention arise from the following description of two embodiments with the aid of the drawing. Shown are:
FIG. 1 , a schematic side view of one part of a vehicle wash system comprising a horizontal wash brush and a horizontal drying arrangement in a first operating position;
FIG. 2 , a schematic side view of the part of the vehicle wash system from FIG. 1 , in a second operating position;
FIG. 3 , a schematic of one part of an additional vehicle wash system comprising a horizontal wash brush and a horizontal drying arrangement in a first operating position and
FIG. 4 , a schematic side view of the part of the vehicle wash system from FIG. 3 in a second operating position.
DETAILED DESCRIPTION OF THE INVENTION
The vehicle wash system represented schematically in different positions in side view in FIGS. 1 and 2 comprises a frame 1 , executed here as a portal, on which are arranged in a height-adjustable manner a first treatment unit 2 executed as a horizontal brush and a second treatment unit 3 designed as a drying arrangement. The first treatment unit 2 comprises a wash brush 4 that is rotatable about a horizontal axis and driven by a motor and that is guided to be vertically sliding on the frame 1 by means of vertical guides 5 and guide blocks 6 . For the execution shown, the second treatment unit 3 is realized as a horizontal roof dryer having a housing 7 and a nozzle head 8 directed downward, which run crosswise to the longitudinal direction of the vehicle across the entire vehicle width and which, by means of vertical guides 9 and guide blocks 10 allocated thereto, are likewise guided to be vertically sliding on the frame 1 executed as a portal. After a vehicle has been washed, an air flow produced by a blower and introduced into the housing 7 can be directed to the upper side of the vehicle by means of the nozzle head 8 in order to dry the vehicle. The vehicle wash system comprises, apart from the horizontal brush, side brushes as well and side dryers that, however, are not depicted here. These likewise can be arranged on the portal-like frame 1 or on an additional portal or frame.
For the embodiment depicted in FIGS. 1 and 2 , a drive motor 11 is arranged on the frame 1 executed as a portal; said drive motor is coupled to the two treatment units 2 and 3 by means of a traction member 12 executed as a cable, belt or chain and diverse deflection rolls. The traction member 12 is guided by means of a first deflection roll 13 on the second treatment unit 3 and two stationary deflection rolls 14 and 15 on the frame 1 , where one end of the traction member 12 is wound upon a drive roll 16 that rotates by means of the drive motor 11 and the other end of the traction member 12 is fastened to the first treatment unit 2 .
Additionally fastened to the frame 1 is a locking arrangement 17 by means of which the second treatment unit 3 can be arrested in an upper end position. For the embodiment shown, the locking arrangement 17 comprises a pivoting stop 18 that can be made to pivot, via a lever 20 , by means of a pneumatically or hydraulically activated actuating cylinder or other suitable actuating drive 19 , between a downward-folded release position according to FIG. 1 and an upward-folded stop position according to FIG. 2 . In the upward-folded stop position, the stop 18 rests against the underside of the block 10 and prevents lowering of the second treatment unit 3 . Also fastened to the frame 1 is an upper stop 21 for the first treatment unit 2 .
For the execution shown, there is a weight difference between the two treatment units 2 and 3 , wherein the first treatment unit 2 is lighter than the second treatment unit 3 and the difference in weight is selected such that the first treatment unit 2 is drawn against the stop 21 by the heavier second treatment unit 3 according to FIG. 1 , provided that the second treatment unit 3 is not arrested.
If for the position depicted in FIG. 1 the traction member 12 is rolled up by a corresponding rotation of the drive roll 16 , the second treatment unit 3 is raised and can be moved from a lower position depicted by solid lines to an upper end position depicted by dashed lines. If by activating the locking arrangement 17 the second treatment unit 3 is arrested in the upper end position according to FIG. 2 , the deflection roll 13 acts as a stationary deflection roll and the first treatment unit 2 can be moved upward or downward by means of a corresponding rotation of the drive roll 16 .
Provided that the difference in weight of the treatment units is sufficiently great, a locking device is required only on the heavier treatment unit since when activating the drive motor, only the heavier treatment unit will move and the lighter one is drawn against the mechanical end stop. However, for other weight relationships, locking devices can also be provided on both treatment units.
This drive principle can be used to mutually adjust both treatment units by means of one single drive motor. If the first treatment unit is a matter of, for example, a wash brush and the second treatment unit is a matter of a drying arrangement on one portal, this in no way whatsoever represents a restricting of the operation of the vehicle wash system, since the wash brush and the drying arrangement are effective in any case in separate passes over the portal.
The second embodiment of a vehicle wash system represented in FIGS. 3 and 4 differs from the first embodiment only in that the drive motor 11 with drive roll 16 , rather than being in a stationary arrangement on the frame 1 , is arranged on the vertically sliding second treatment unit 3 . Since the basic construction otherwise corresponds to the embodiment of FIGS. 1 and 2 , corresponding components also are given the same reference numbers. Here, the traction element 12 is guided only via two deflection rolls 14 and 15 in a stationary arrangement on the frame 1 , wherein one end of the traction member 12 is fastened to the first treatment unit 2 and the other end of the traction member 12 is wound upon the drive roll 16 of the drive motor 11 fastened to the second treatment unit 3 .
If for the position depicted in FIG. 3 , the drive roll 16 is rotated by the drive motor 11 in order to roll up the traction member 12 , the second treatment unit 3 also is raised here and can be moved from a lower position represented in solid lines to an upper end position represented in dashed lines. If the second treatment unit 3 , by means of activating the locking arrangement 17 , is arrested in the upper end position according to FIG. 4 , the treatment unit 2 can be lowered and raised afresh by means of a corresponding rotation of the drive roll 16 .
The invention is not limited to the embodiments described above and represented in the drawings. It thus goes without saying that in lieu of a horizontal wash brush and horizontal drying arrangement, other treatment units can also be moved by means of the aforementioned drive concept. | The invention relates to a vehicle wash system comprising a first treatment unit ( 2 ) arranged on a frame ( 1 ) so as to be height-adjustable and at least one second treatment unit ( 3 ) arranged on the frame ( 1 ) so as to be height-adjustable. In order to reduce the components required for driving and controlling the treatment units ( 2, 3 ) the latter are coupled to a common drive motor ( 11 ) via a traction mechanism drive ( 12, 13, 14, 15 ) for their mutual adjustment. | 1 |
BACKGROUND OF THE INVENTION
The present invention relates to a signal processing circuit for FM signal receiver, and more particularly to a combined circuit of a tuning level indication, a muting operation and an AFC (Auto Frequency Control) signal information.
In addition to the fundamental construction for receiving an FM signal, such as a tunner, a radio-frequency (RF) amplifier, a mixer, an intermediate-frequency (IF) amplifier, an FM demodulator, an audio-frequency (AF) and power amplifiers, and a loud speaker, recently FM radio receivers generally provide a tuning indicator for aiding a listener to select a broadcasting station, a level muting function which attenuates or interrupts an output when there is no received signal or when a received signal level is so low that good receiving characteristics cannot be obtained, a band muting function which attenuates or interrupts an output when precise tuning to a receiving signal frequency is not attained and hence a good demodulated output cannot be obtained, and/or an AFC function which automatically reduces variation of an oscillation frequency of a local oscillator due to variations of an environmental temperature and a power supply voltage. Consequently, an FM receiver requires many circuits for achieving the associated functions such as a drive circuit for a tuning indicator, a signal strength detector circuit, a frequency deviation detector circuit for detecting whether tuning is made precisely or not, a muting control circuit responsive to the outputs of the signal strength detector circuit and the frequency deviation detector circuit, for controlling a muting operation of the receiver, an output control circuit responsive to the output of the muting control circuit for deriving the output of the FM receiver or cutting off the output by attenuating or interrupting the output under the action of muting, an AFC signal deriving circuit, etc.
In the conventional FM radio receiver, the signal strength was detected from IF amplifier stage and indicated by an indicator such as moving coil type ammeter, as taught in U.S. Pat. No. 3,673,499. The listener could detect the precise tuning condition from the indication of the signal strength indicator. The muting operation was made by the peak-to-peak detection output from the angle modulation detector, and AFC operation by the output derived from the output amplifier, as taught in U.S. Pat. No. 3,714,583. Thus, each operation was made by the individual circuit associated to the individual fundamental circuit block, and so the conventional FM radio receiver had a disadvantage that its construction was extremely complex.
SUMMARY OF THE INVENTION
Therefore, it is one object of the present invention to provide a signal processing circuit for use in an FM signal receiver which has a simple circuit construction.
Another object of the present invention is to provide the above-described signal processing circuit which is suitable for constructing in an integrated circuit.
According to the present invention, there is provided a signal processing circuit comprising an amplifier circuit for providing an amplified signal, a current switching circuit selecting a current flowing path for an amplified signal flowing from the amplifier and a constant current signal from a constant current source and controlled by a muting signal, current mirrors receiving signals from the current switching signal and producing an output current proportional to the received signals from the selected current path from the switching circuit, a reference voltage terminal coupled to a bias voltage, a coupling point to the output of one of the current mirrors and an output of the amplifier circuit, and a tuning indicator positioned between the reference voltage terminal and the coupling point.
The present invention can provide a signal processing circuit having an audio frequency amplifier circuit, a tuning indicator drive circuit, a tuning frequency deviation detector circuit, an AFC signal output circuit and an audio signal switching circuit for muting which can be constructed in a single circuit block with a simple circuit construction that is free from the above-described disadvantage. Also, the signal processing circuit according to the present invention is suitable for constructing in an integrated circuit.
BRIEF DESCRIPTION OF THE DRAWINGS
The above and further objects, features and advantages of the present invention will become more apparent from the following detailed description of embodiments taken in conjunction with the accompanying drawings, wherein:
FIG. 1 is a circuit diagram showing one preferred embodiment of the signal processing circuit according to the present invention;
FIG. 2 is a circuit diagram showing another preferred embodiment of the present invention; and
FIG. 3 is a circuit diagram showing still another preferred embodiment of the present invention.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
Referring now to FIG. 1, all the circuit components of one preferred embodiment according to the present invention are formed on a single semiconductor chip, except for a null-centered tuning indicator 26, resistors 27 and 30, and a capacitor 29. The semiconductor chip has a power supply terminal 35, a ground terminal 22, first and second audio signal input terminals 1 and 2, first and second switching control input terminals 13 and 14, an audio signal output terminal 20, a tuning signal output terminal 25, a tuning detection output terminal 36, and terminals 33 and 34. It can be designed to supply a bias voltage from an external bias voltage source 37 through a terminal 28. A first audio signal input terminal 1 and a second audio signal input terminal 2 are connected respectively to a base of a transistor 3 and a base of another transistor 4, and the emitters of the transistors 3 and 4 are connected in common to a constant current source 7 through resistors 5 and 6, respectively. The collector of the transistor 4 is connected to the emitters of the transistors 8 and 9 which have their emitters connected in common. In addition, there are provided another pair of transistors 10 and 11 having their emitters connected in common, and a current switching circuit is composed of these transistors 8, 9, 10 and 11. The common emitters of the transistors 10 and 11 are connected to constant current source 12, and the current value supplied from this constant current source 12 is equal to one-half of the current value supplied from the constant current source 7. The bases of the transistors 9 and 10 are connected in common to a first switching control input terminal 13, while the bases of the transistors 8 and 11 are connected in common to a second switching control input terminal 14. The collectors of the transistors 8 and 10 are connected in common to an input point 16 of a current mirror circuit 15. Also, the collectors of the transistors 9 and 11 are connected in common to an input point 18 of another current mirror circuit 17. The first output point 19 of this current mirror circuit 17 is connected to an audio signal output terminal 20, and is also connected via a load resistor 21 to a ground terminal 22. The output point 23 of the current mirror circuit 15 and the second output point 24 of the current mirror circuit 17 are connected in common to the collector of the transistor 3, and are further connected to a tuning signal output terminal 25.
The tuning signal output terminal 25 is connected through a null-centered tuning indicator 26 and a resistor 27 to a bias terminal 28. The junction between the null-centered tuning indicator 26 and the resistor 27 is connected to the ground terminal 22 via a capacitor 29, and is connected to an AFC voltage supply terminal 31 via a resistor 30. The opposite ends of the resistor 27 are respectively connected to first and second detector terminals 33 and 34 of a potential difference detector circuit 32. In addition, reference numeral 35 designates a power supply terminal, numeral 36 an output terminal of the tuning detection circuit, and numeral 37 a bias voltage source.
The term "current mirror circuit" as used throughout this specification implies a circuit which detects a current flowing through an input point and which makes an output current proportional to the input current to be derived from an output point, and it can be constructed by employing a diode 38 and a transistor 39, connecting a junction between one terminal of the diode 38 and the emitter of the transistor 39 to the power supply terminal 38, using the junction between the other terminal of the diode 38 and the base of the transistor 39 as the input point 16 of the current mirror circuit 15, using the collector of the transistor 39 as the output point 23 of the same current mirror circuit 15, and detecting the current flowing through the diode 38 by means of the transistor 39, as is the case with the current mirror circuit 15 shown in FIG. 1. The current ratio of the input and output currents is determined by the PN junction area ratio of that of diode 38 and the base-emitter junction of transistor 39.
The other current mirror circuit 17 is likewise constructed by means of a diode 40 and transistors 41 and 42, which are matched to each other. The output current at the output point 19 is determined by the PN junction area ratio of that of diode 40 and base-emitter junction of transistor 42, and the output current at the output point 24 by the PN junction area ratio of that of diode 40 and base-emitter junction of transistor 41.
The tuning detection circuit 32 operates so as to detect the absolute value of the difference between the terminal potentials at the first and second detector terminals 33 and 34, and for instance, it is illustrated as encircled by a dotted line in FIG. 1. More particularly, there are provided a transistor 43 and a transistor 44 having their collectors connected in common, the common collectors are connected to the power supply terminal 35, the respective bases of these transistors 43 and 44 are connected to the first and second terminals 33 and 34, respectively, and the emitter of the transistor 43 is connected via a diode 45 to a current source 46, while the emitter of the transistor 44 is connected via a diode 47 to another current source 48. There are provided additional transistors 49 and 50 of different conductivity type from the transistors 43 and 44, the base of the transistor 49 is connected to the junction between the diode 45 and the current source 46, and the emitter of the transistor 49 is connected via a resistor 51 to the emitter of the transistor 44, while the base of the transistor 50 is connected to the junction between the diode 47 and the current source 48, and the emitter of the transistor 50 is connected via a resistor 52 to the emitter of the transistor 43, and the collectors of the transistor 49 and 50 are connected in common to be used as an output terminal 36 of the tuning detection circuit 32.
To the first and second audio signal input terminals 1 and 2 are respectively applied demodulated audio frequency signals which have inverted phases each other, superposed on D.C. bias voltages and which are fed from a FM demodulator stage. Otherwise, to one input terminal is applied a demodulated output signal superposed on a D.C. bias voltage, and to the other input terminal is applied a D.C. bias voltage.
If the FM receiver is precisely tuned to a center frequency of a receiving signal, then D.C. components of the input signals applied to the first and second signal input terminals 1 and 2 are equal to each other.
The input voltages at the first and second input terminals 13 and 14 are controlled by a muting control circuit (not shown). The muting control circuit produces a control signal when no signal or a weak signal is received or when precise tuning is not attained. In the case where an output is derived from the FM receiver without muting, the output voltage on the first current switching control signal input terminal 13 is made sufficiently higher than the input voltage on the second current switching control signal input terminal 14, and thereby the transistors 8 and 11 are cut off, while the transistors 9 and 10 are made conducting. An input signal applied between the first and second signal input terminals 1 and 2 is amplified by the transistors 3 and 4, the amplified signal is applied from the collector of the transistor 4 via the transistor 9 to the input point 18 of the current mirror circuit 17, and an amplified signal is derived from the first output point 19 of the current mirror circuit 17 and is transferred to an output terminal 20. From the second output point 24 of the current mirror circuit 17 is derived a current equal to one-half of the current flowing through the input point 18. This operation can be achieved by making the PN junction area of the transistor 42 half of the PN junction area of the diode 40. On the other hand, a current supplied from the current source 12 is applied via the transistor 10 to the input point 16 of the current mirror circuit 15. From the output point 23 of the current mirror circuit 15 is derived a current equal to one-half of the current flowing through the input point 16 from the current source 12.
Assuming now that the FM receiver is precisely tuned to the received signal frequency and hence the D.C. components of the input voltages of the first and second audio signal input terminals 1 and 2 are equal to each other, then the D.C. components of the currents flowing through the transistors 3 and 4 are equal to each other, and they are equal to the current value supplied from the current source 12. Since the ratio of the current flowing through the input point 16 of the current mirror circuit 15 to the current flowing through the output point 23 is selected at 1:1/2, and since the ratio of the current flowing through the input point 18 of the current mirror circuit 17 to the current flowing through the second output point 24 is selected at 1:1/2, the D.C. component of the sum of the current flowing through the output point 23 of the current mirror circuit 15 and the current flowing through the second output point 24 of the current mirror circuit 17 and the D.C. component of the current flowing through the transistor 3 become equal to each other and are balanced, and hence the current flowing through the null-centered tuning indicator 26 contains no D.C. component. The null-centered tuning indicator 26 is composed of, for example, a moving-coil type ammeter which indicates an average value of a current flowing therethrough and in the above-assumed case, it points the null center to indicate that the FM receiver is precisely tuned.
If the tuning of the FM receiver deviates from the receiving signal frequency, then a difference arises between the D.C. components of the input voltages at the first and second audio signal input terminals 1 and 2, and thereby the FM signal processing circuit is deviated from the above-described balanced state. For instance, if the tuning is deviated in such a manner that the D.C. component of the input voltage at the first audio signal input terminal 1 may become higher than the D.C. component of the input voltage at the second signal input terminal 2, then the D.C. component of the current flowing through the transistor 3 is increased, and on the other hand the D.C. component of the current flowing through the transistor 4 is decreased by the amount equal to the increment. Consequently, the DC component of the current flowing from the collector of the transistor 4 to the input point 18 of the current mirror circuit 17 via the transistor 9 is decreased, so that the D.C. component of the current derived from the second output point 24 of the current mirror circuit 17 is also decreased. Since the currents in the current mirror circuit 15 are not varied, a current corresponding to the sum of the increment of the D.C. component of the current flowing through the transistor 3 and the decrement of the D.C. component of the current flowing through the second output point 24 of the current mirror circuit 17 appears as a D.C. component of a current flowing to the tuning signal output terminal 25. The direction of the D.C. component of the current in this case is the direction flowing from the bias terminal 28 through the resistor 27 and the null-centered tuning indicator 26 to the tuning signal output terminal 25. In this way, a D.C. component appears in the current flowing through the null-centered tuning indicator 26, and hence the null-centered tuning indicator 26 is driven so as to deviate from the null center point indicating that the tuning of the FM receiver is not correctly achieved. On the contrary, in the case where the tuning of the FM receiver has been deviated from the received signal frequency so that the input voltage at the first audio signal input terminal 1 becomes lower than the input voltage at the second audio signal input terminal 2, then likewise a D.C. component in the opposite direction appears in the current flowing through the null-centered tuning indicator 26, and thereby the null-centered tuning indicator 26 is driven so as to deviate the opposite direction. In this manner, the D.C. component of the current flowing through the null-centered tuning indicator 26 will vary depending upon the value and direction of the deviation in tuning of the FM receiver. The signal component of the current flowing through this null-centered tuning indicator 26 is removed as by-passed via the capacitor 29 to the ground, and only the D.C. component of the current is detected as a voltage drop by the resistor 27. The voltage detected in this way is derived as an AFC voltage from the terminal 31 via the resistor 30, and also the absolute value of the voltage is detected by the tuning detection circuit 32 and is derived from the output of the tuning detection circuit 32 to be used as a band muting control signal of the FM receiver. In this way a center frequency deviation detector circuit is composed of the resistor 27, the capacitor 29 and the tuning detection circuit 32.
In the case where an output is not derived from the FM receiver under muting control, the control input voltage at the second current switching control signal input terminal 14 is made higher than the control input voltage at the first current switching control signal input terminal 13, and thereby the transistors 8 and 11 are made conducting so as to operate in a grounded base mode, while the transistors 9 and 10 are cut off. Consequently, the current supplied from the current source 12 is applied to the input point 18 of the current mirror circuit 17 via the transistor 11, so that the output current derived from the first output point 19 of the current mirror circuit 17 contains only a D.C. component. Since the value of the output current is identical to that in the case of not subjecting the FM receiver to muting control where the input voltages at the first and second audio signal input terminals 1 and 2 are equal to each other, the shock noise appearing at the output when the muting signal is applied to or released from the FM receiver can be reduced.
The signal applied between the input terminals 1 and 2 is amplified by the transistors 3 and 4, and the current flowing from the transistor 4 is switched to the current mirror circuit 15 at the muting operation or to the current mirror circuit 17 to derive an output from the output terminal 20 in non-muting operation.
As described previously, since the ratio of the current flowing through the input point 16 of the current mirror circuit 15 to the current flowing through its output point 23 and the ratio of the current flowing through the input point 18 of the current mirror circuit 17 to the current flowing through its second output point 24 are both preset at 1:1/2, even if the input points 16 and 18 of the current mirror circuits 15 and 17, respectively, are interchanged by switching, there occurs no change in the operation of deriving a current through the common connection of the output point 23 of the current mirror circuit 15 and the second output point 24 of the current mirror circuit 17. With regard to the other operations also, the FM receiver operates in a similar manner to the case of deriving an output without applying muting action to the FM receiver. This results in a very small shock noise at muting change.
As described above, according to the above preferred embodiment of the invention, an audio frequency amplifier circuit, a current switching circuit, a tuning indicator drive circuit, an AFC voltage detector circuit and a center frequency deviation detector circuit can be composed in a single circuit block with a simple construction, and therefore, the present invention has an advantage that the entire construction of an FM receiver can be simplified. In addition, since a control signal for band muting is derived by directly detecting a D.C. component of a current flowing through a null-centered tuning indicator 26, the null center point of the null-centered tuning indicator 26 and the center of the band muting coincide with each other. Furthermore, conventional precise tuning as shown in U.S. Pat. No. 3,673,499, for example, was made by reference to the signal strength indicator and the listener searched an optimum tuning point by manual operation. It was difficult for the listener, however, to obtain a precise tuning point, because the precise tuning was at the peak signal strength which the listener did not know until the tuning frequency was passed. And a long term was required until the listener obtained the optimum tuning point. However, the present invention has the null-centered tuning indicator teaching a precise tuning point by a null-centered point, and therefore the listener can find the precise tuning point rapidly and precisely. Also there is an advantage that the shock noise upon applying or releasing the muting control can be reduced. Furthermore, there is an additional advantage that the circuit construction according to the present invention can be easily constructed in an integrated circuit.
According to modified embodiments of the present invention it is possible to regulate the detection sensitivity for an AFC voltage or to preset upper and lower limits of an AFC voltage.
In FIG. 2 is shown one example of the modified embodiments. This circuit is different from the circuit shown in FIG. 1 only in that serially connected resistors 53 and 54 are connected in parallel to a resistor 27 and an AFC voltage is derived from the junction point between the resistors 53 and 54, the remainder of the circuit being indentical to that in FIG. 1, and the operations are also similar to those of the circuit in FIG. 1. According to this modified embodiment, the detection sensitivity for an AFC voltage can be lowered, to a preferable level by selecting the resistance of the resistors 53 and 54 without any affect on the other operations.
FIG. 3 shows another modified embodiment. This circuit is different from the circuit shown in FIG. 1 only in that an additional resistor 55 is connected between a resistor 27 and a null-centered tuning indicator 26, that between a bias terminal 28 and a tuning signal output terminal 25 are connected serially connected diodes 56 and 57 and further serially connected diodes 58 and 59 which are connected in parallel to the diodes 56 and 57 and in the opposite polarity to the diodes 56 and 57, and that an AFC voltage is derived from the junction point between the resistor 55 and the null-centered tuning indicator 26. The remainder of the circuit being identical to that in FIG. 1, and the operations are also similar to those of the circuit in FIG. 1. In this modified embodiment, a detection sensitivity for an AFC voltage is raised by means of the resistor 55, and by making use of the diodes 56, 57 and the diodes 58, 59, upper and lower limits are preset for the variation range of the AFC voltage so that the transistor 3 or the output transistors in the current mirror circuit 15 and 17 may not be saturated.
It is apparent for the skilled in the art, if the band muting function is not necessary, the tuning detection circuit 32 may be removed from the circuit blocks of the embodiments shown. Further, if the AFC operation is not required, the resistors 30, 53 and 54 and capacitor 29 can be omitted. However, even in this case, it is preferable to retain the capacitor 29 for reliable operation of the null-centered tuning indicator 26. | A signal processing circuit for an FM signal receiver suitable for constructing in an integrated circuit is disclosed. The signal processing circuit comprises a differential amplifier circuit receiving first and second demodulated signals of the frequency modulated signal and providing first and second output signals. A current switching circuit has a first input point for receiving the second output signal of the amplifier and a second input point for receiving the output of a constant current source. The current switching circuit switches current paths from the first and second input points to first and second output points in response switching control inputs. A first current mirror has an input point coupled to the second output point of the current switching circuit and an output point coupled to the first output signal of the amplifier circuit. A second current mirror has an input point coupled to the first output point of the current switching circuit, a first output point coupled to the output point of the first current mirror and a second output point coupled to an output terminal. A null-centered indicator is connected between a reference voltage terminal and the junction of the output point of the first current mirror and the first output point of the second current mirror. A potential difference detector can be inserted between the reference voltage terminal and the null-centered indicator. | 7 |
BACKGROUND OF THE INVENTION
The present invention relates to clocks having audio reproductions provided thereby and, more particularly, to clocks providing multiple displays and selected audio reproductions.
Music by machine, such as bell striker assemblies, music boxes and the like, has been used for centuries to annunciate the passage of increments of time. Typically, individual clocks providing such music have used a variety of mechanically or electronically generated audio passages to provide this result. For instance, the famous "Big Ben" at the Houses of Parliament in London, England, uses a centuries old mechanically actuated mechanism to strike bells in a prescribed sequence and at prescribed times to produce the well-known Westminster chimes. That clock mechanism enjoys distinction and fame primarily for two reasons: the particular music passage provided, and the particular sound characteristics of the bells used therein. Back to Renaissance times, and even before, equally distinctive clocks have been constructed in many countries of the world, each playing either a music specifically originated therefor, or playing music with a novel mechanical playing arrangement, or both. However, even though many clocks could play different musical compositions on the music playing arrangement therein, each was restricted to its music playing arrangement.
Typically, in conjunction with the annunciation of time increments by music, and also long before such annunciations, the passage of time increments was displayed by the analog movement of a structure ("hands") over some sort of dial face. Usually (until relatively recently), this was a mechanical arrangement using appropriate gearing to divide days into hours, hours into minutes, and minutes into seconds to an extent depending on the time resolution desired to be displayed. In nearly all of these arrangements, all of the analog structure used for movement in the displays, and everything needed to result in such movement, was operated by a single motor so that accurate synchronization between each element involved was preserved. This approach is efficient if only relatively simple gear arrangements are required, or if only a very small number of different time related displays are used. However, the method becomes cumbersome and expensive if more complex gear arrangements are required to display, for instance, the ordinary time of the day and, simultaneously, the position of the moon with respect to the earth. The use of mechanical gear arrangements also limits where the analog structures in the displays can be placed due to the requirement that all of the gears directly interact in some manner while being driven by a single rotary motion device, or motor, in conjunction with physical size limitations of the gears used. Thus, there is the desire for a clock system permitting access to a variety of different music passages from which to select one to annunciate increments of time, and to permit providing a variety of time related displays.
SUMMARY OF THE INVENTION
The present invention provides a timekeeping system for providing selected ones of a plurality of audio signal portions, obtained from stored audio information, to be synchronized with selected time events even though the audio signal portions are of durations differing from one another. The audio information is stored in a memory means as a plurality of duration data assemblages each corresponding to an audio signal portion and each comprising an audio data assemblage from which the audio signal portion can be obtained and a blank data assemblage which provides the remaining time for the duration data assemblage to fill a passage time duration of a selected length. A controller is capable of directing a memory means to provide the duration data assemblage at its output based on the number of cycles provided to the controller means from a timing signal generator having an output signal with cycles provided at a fundamental frequency.
The timekeeping system may also have a rotator having an output structure which is rotated at a selected angular value periodically if electrically energized. The rotator is operated through a power switch by the controller to selectively supply electrical power to the rotator which rotates the output structure typically for display purposes. The rotator, operating with independent rotation timing, can be synchronized to the timing generator output signal by at least temporarily removing power from the rotator before the rotation period thereof drifts by more than a selected fraction of the period of the timing generator output signal. Further, the rotator rotation period for the angular rotation of the output structure can be effectively increased by selectively removing power from the rotator.
The audio signal selections, obtained from audio information stored in a memory, is acquired by recording acoustic signals, removing unwanted components therefrom and storing the resulting audio signal portions as the audio data assemblages in the memory. Thus, thereafter selecting the audio signal selection desired leads to the appropriate audio data assemblage being retrieved in conjunction with a selected time event, determined from cycles in the timing signal, at a time fixed with respect to that time event.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a block diagram of the timekeeping system of the present invention;
FIG. 2 is a block diagram of an alternate embodiment of the timekeeping system of the present invention;
FIG. 3 is a block diagram of a subsystem used in the present invention;
FIG. 4 is a representation of a possible situation in a subsystem used in the present invention;
FIG. 5 is a block diagram of a subsystem useable in the present invention;
FIGS. 6A and 6B are a block diagram of a subsystem used in the present invention;
FIGS. 7A and 7B show waveforms representing possible events occurring during use of the present invention; and
FIGS. 8A and 8B show a flow chart describing operations in the system of the present invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
FIG. 1 shows a block diagram of the timekeeping system of the present invention including its audio system and its display arrangement. This timekeeping system is operated by a system controller, 10, and supplied electrical power through a battery system, 11, which can be continuously charged from an alternating current electrical power line if the user does not desire to operate on battery alone.
A user may provide commands to the system controller through a control panel, 12, having a liquid crystal (or other kind) digital display, 13, and a keypad, 14, which can receive manual circuit switching inputs from the user. A pair of potentiometer based day and night audio volume controls, 15 and 16, respectively, also accept manual commands from the user.
System controller 10 operates four different analog time displays, 17, including a main clock, a moon position clock, a moon phase clock, and a day of the week clock. System controller, 10, also operates the audio system including an audio information storage compact disc player 18, and three loudspeakers, 19.
FIG. 2 shows an alternative timekeeping system in which audio storage compact disc player 18 in FIG. 1 is replaced by an audio information storage programmable read-only memory, 18'. Some changes are required in system controller 10 to accommodate this audio information storage subsystem substitution, and the audio data stored must substantially different, but both in concept and implementation the accommodation is not too difficult. Similarly, other kinds of audio information storage systems could be used, such as tape or a computer hard disk, with suitable accommodations within the timekeeping system although no attempt will be made to also describe such other storage system types as they are also well known.
Any conventional compact disc player may be used as audio storage compact disc player 18 in which the electronic control apparatus for the player is accessible so that control signals can be supplied from system controller, 10, to manage and control that player. Similarly, any kind of programmable read-only memory may be used for audio storage programmable readonly memory 18' provided it has sufficient capacity and has sufficient operating speed to store and retrieve audio information data from which musical passages can be reproduced.
Loudspeakers 19 consist of two conventional mid-range loudspeakers and a conventional bass loudspeaker connected in a conventional arrangement to permit a pair of stereophonic analog audio signals to be supplied thereto for broadcast. Other circuit arrangements may or will be used therewith such as crossover circuits, equalizers or the like.
FIG. 3 shows a clock motor and internal control arrangement forming an independently controlled clock motor for operating each of the analog time displays in analog display 17. One such independently controlled clock motor is used with each analog display (typically a driven mechanical indicator such as a minute hand, hour hand, dial carry pertinent pictorial scenes, or the like).
The independently controlled clock motor of FIG. 3 is a self-contained unit operated by its independent and self-generated time base formed by a crystal controlled oscillator, 20, therein having an oscillatory output signal with an oscillation frequency of 32.768 kHz. This oscillatory output signal is provided to a clock divider and control circuit, 21, which provides electrical power pulses alternating between two outputs which go to supply alternately positive current and negative current to a clock motor coil, 22. Thus, the upper output of circuit 21 in FIG. 3 provides an electrical power pulse to cause a positive electrical current to flow in the positive current flow direction in clock motor coil 22 every even numbered second, while the lower output of circuit 21 provides a electrical power pulse every odd second to cause negative current to flow in the negative current flow direction of the clock motor coil 22.
As a result, the magnetic field developed in clock motor coil 22 forces a rotor in an output actuator, 23, incorporating a gear reduction arrangement, to rotate a selected angular amount to in turn cause a corresponding movement of the motor second hand output shaft sufficient for an increment of one second. The gear reduction arrangement in actuator 23 rotates several output shafts at differing angular rotation rates, including concentrically mounted cylindrical shell output shafts. Thus, this output assembly arrangement in actuator 23 allows synchronous rotation of a second hand (completing a full rotation in a minute), a minute hand (completing a full rotation in a hour), and an hour hand (completing a full rotation in 12 hours) through the gear reduction arrangement having proper effective gear ratios of these output shafts with respect the rotor, and its two second period full rotations, due to its being directly driven by clock motor coil 22.
The independently controlled clock motor of FIG. 3 thus will operate continually if clock control power is provided to clock divider and control circuit 21, and so to oscillator 20. That is, the supplying of clock control power immediately (within milliseconds) causes the rotor in actuator 23 to rotate its standard angular amount corresponding to one second upon the motor coil receiving a suitable current pulse, and then causes the rotor to continue doing so every second thereafter. On the other hand, removal of the clock control power immediately prevents further motion of the rotor in actuator 23.
As indicated above, the passage of time increments is often annunciated with chimes, i.e. a musical interlude, followed, at least at the hour, by bell strikes in number sufficient to match the hour number. Thus, the audio system that is part of the timekeeping system of FIGS. 1 and 2, maintains stored audio information from which can be reproduced corresponding chimes, or musical interludes, and strikes. Because different compact discs can be used with audio storage compact disc player 18, and because different programmable read-only memories can be used for audio storage programmable read-only memory 18', the timekeeping system of FIGS. 1 and 2 has the ability to play recordings of a variety of chimes annunciating the passage of increments of time each associated with one of many different and, if desired, well known clocks. Alternatively, other kinds of music could be played.
Thus, the present invention provides for a far wider and richer variety of chimes, or other music, then has been heretofore available for a single clock. The use of interchangeable music storage media in player 18, or in memory 18', allows for a wide variety of chimes, or other music, that can be easily changed to suit the listener or environment, and thus provides the ability to control and adjust the ambiance of the environment by the choice of recorded chimes or other music.
Thus, to obtain recordings for publicly played chimes, or of clock chimes in museums or in private hands, the timekeeping systems of FIG. 1 and FIG. 2 obtain the corresponding audio information by first recording the acoustic signals from the clock and its musical annunciation arrangement through a pair of conventional monaural microphones, 30 and 31, in a standard electrical signal recording arrangement, 32. The use of two microphones allows obtaining right and left audio information as the basis for providing stereophonic reproductions of those signals.
Rather than use both microphones 30 and 31, an alternative method is to use a single directional microphone to obtain a single monaural signal, and then form a second signal therefrom which is delayed typically 25 to 30 milliseconds from the first recorded signal to simulate some acoustic signals reaching the listener later than others due to reflections from buildings and the like. Such an arrangement may well provide a more realistic experience for the listener than the use of two monaural microphones as the basis for providing a stereophonic reproduction result.
The raw recorded audio information signals from the acoustic signals recorded in recorder 32 can then be later converted to digital signal form by an analog-to-digital converter, 33, and then sent to a computer, 34, to remove unwanted components from these signals. Such unwanted components in publicly recorded acoustic signals may include street noises, birds, mechanical movement noises from the clock or associated music provision arrangement, and the like.
This unwanted signal component removal can be done in alternative ways, including recording the same chimes at different times, and thereafter correlating between the various recordings using averaging methods to keep the signals which are common to each and to eliminate spurious signals present in each. Another way is to have one familiar with audio reproduction look at the frequency spectrum of the recorded acoustic chime signals and eliminate clearly unwanted components recognized by that person.
The audio signals remaining after removal of unwanted components are either stored in the computer, or stored in another memory means, or an electrical signal recording means, 35. From there, the audio information captured in signal recording means or memory 35 must be stored appropriately in compact discs or programmable read-only memories for use in player 18 or in memory 18'. However, significant problems arise in doing so where the recorded chime audio signals involve a broad array of chime selections each with different time durations and timing requirements.
For instance, some well known clocks chime each quarter hour while others sound only each hour, and some sound only every third hour. Some well known clocks have chimes of long durations while others are of rather short duration. Further, it is very important to allow interchangability among various compact discs containing data for different chimes, or among various programmable read-only memories containing data for different chimes, but any of which must play in the timekeeping systems of FIGS. 1 and 2 at exactly the correct time to correctly annunciate the passages of increments of time.
In order to have consistency among different chime selections, a convention must be chosen relating to whether such musical annunciation of a time increment begins at, or ends at, the time event separating one increment from the next. For instance, music selections for the first quarter hour following an hour could begin at exactly 15 minutes after the hour, or could begin earlier so that they end exactly 15 minutes after the hour. Herein, we will describe a system which uses the latter convention of ending prior to time events indicating separations between adjacent time increments, but the alternative convention could just as well have been used.
Again, on the hour, many chimes play music followed by striking the number of hours at that time. Typically, the first strike marks the exact hour, and that is the convention chosen in the following description but an alternative could just as well be used. Such convention choices affect the particular formats followed in providing and playing chime selection tracks on a compact disc, and in locating and retrieving chime data in programmable read-only memories. Hence, the conventions must be kept the same so that compact discs with chime data are interchangeable, and so that programmable read-only memories with chime data are interchangeable, while preserving timing accuracy.
To provide a large range of chime, or musical interlude, choices on one compact disc or in one programmable read-only memory, the particular format chosen and described herein accommodates four chimes and three melodies. Other compact disc formats, or programmable read-only memory formats, could alternatively have been chosen containing a greater or lesser number of chimes depending on the size and cost of the particular memory storage system used. Each time a chime or musical interlude is to be played in connection with a time event, the computer instructs player 18 to go to a particular track or series of tracks on the compact disc therein which contains the music for that time event in the compact disc example to be described here. Since the timekeeping system of FIGS. 1 and 2 will not be able to distinguish between alternative disc formats, the same disc format must be maintained for every disc of alternative chimes, or musical interludes, to be developed thereafter for use in the system of FIGS. 1 and 2. This disc format is represented in the following tabulation:
______________________________________ Chime SelectionTime 1 1C 1H 2 2C 2H 3 3C 3H 4______________________________________12o'c 14:40 60 60 14:53 4 4 32 32 29:10 61 61 29:45 5 5 33 33 44:40 6 6 34 34 62 62 59:00 63 63 59:15 76 59:30 8 7 8 36 35 36 59:59 64 64 --1o'c 14:40 60 60 14:53 4 4 32 32 29:10 61 61 29:45 5 5 33 33 44:40 6 6 34 34 62 62 59:00 63 63 59:15 77 59:30 10 7 10 38 35 38 59:59 65 65 --2o'c 14:40 60 60 14:53 4 4 32 32 29:10 61 61 29:45 5 5 33 33 44:40 6 6 34 34 62 62 59:00 63 63 59:15 78 59:30 12 7 12 40 35 40 59:59 66 66 --3o'c 14:40 60 60 14:53 4 4 32 32 29:10 61 61 29:45 5 5 33 33 44:40 6 6 34 34 62 62 59:00 63 63 59:15 79 59:30 14 7 14 42 35 42 59:59 67 67 --4o'c 14:40 60 60 14:53 4 4 32 32 29:10 61 61 29:45 5 5 33 33 44:40 6 6 34 34 62 62 59:00 63 63 59:15 80 59:30 16 7 16 44 35 44 59:59 68 68 --5o'c 14:40 60 60 14:53 4 4 32 32 29:10 61 61 29:45 5 5 33 33 44:40 6 6 34 34 62 62 59:00 63 63 59:15 81 59:30 18 7 18 46 35 46 59:59 69 69 --6o'c 14:40 60 60 14:53 4 4 32 32 29:10 61 61 29:45 5 5 33 33 44:40 6 6 34 34 62 62 59:00 63 63 59:15 82 59:30 20 7 20 48 35 48 59:59 70 70 --7o'c 14:40 60 60 14:53 4 4 32 32 29:10 61 61 29:45 5 5 33 33 44:40 6 6 34 34 62 62 59:00 63 63 59:15 83 59:30 22 7 22 50 35 50 59:59 71 71 --8o'c 14:40 60 60 14:53 4 4 32 32 29:10 61 61 29:45 5 5 33 33 44:40 6 6 34 34 62 62 59:00 63 63 59:15 84 59:30 24 7 24 52 35 52 59:59 72 72 --9o'c 14:40 60 60 14:53 4 4 32 32 29:10 61 61 29:45 5 5 33 33 44:40 6 6 34 34 62 62 59:00 63 63 59:15 85 59:30 26 7 26 54 35 54 59:59 73 73 --10o'c 14:40 60 60 14:53 4 4 32 32 29:10 61 61 29:45 5 5 33 33 44:40 6 6 34 34 62 62 59:00 63 63 59:15 86 59:30 28 7 28 56 35 56 59:59 74 74 --11o'c 14:40 60 60 14:53 4 4 32 32 29:10 61 61 29:45 5 5 33 33 44:40 6 6 34 34 62 62 59:00 63 63 59:15 87 59:30 30 7 30 58 35 58 59:59 75 75 --______________________________________
In the first column to the left in this tabulation, there is listed the sequence of hours, giving all 12 hours for which a different number of strikes must be provided on the hour. Thus, the twelve hour sequence will repeat twice a day as is typical of most clocks.
In the next column to the right, there is provided a list of times in minutes and seconds following that hour at each of which, in this chosen format, playing of attack on the compact disc is permitted to begin while satisfying the timing selected for the format. Thus, there are nine total possible starting times for the beginning of playing a track on the compact disc following 12 o'clock prior to one o'clock, these first being two times, 12:14:40 and 12:14:53, which are associated with the first quarter hour time event separating that quarter hour from the second quarter hour. Two further times are permitted for starting play of tracks associated with the half hour, these times being 12:29:10 and 12:29:45. There is but a single time to start a track in association with the three-quarter hour point, that being 12:44:40.
Because of the often more elaborate music selections associated with the hour typical of many clocks, there are four alternative times at which a track could begin to play in association with the coming of the next hour of 1 o'clock. These four times are 12:59:00, 12:59:15, 12:59:30, and 12:59:59. Similar arrangements are provided for each of the other hours, 1 o'clock through 11 o'clock.
The next three columns represent alternatives in the first chime, or musical interlude, series provided on a compact disc, each involving the same basic musical melody selection but with a different amount of usage or with a difference in the strikes noting the hour. Thus, for this first musical melody choice, the selections under column 1 provide corresponding musical melody aspects for the quarter hour event on track 4, for the half hour event on track 5, and for the three-quarter hour event on track 6. The hour time event musical selection also contains the number of strikes appropriate to the particular hour, so that different track is associated each hour point to accommodate the different number of strikes.
Under column 1C, the same tracks are begun for the quarter hour event, the half hour event, and the three-quarter hour event. However, a single track, track 7, is used in connection with each hour event since, in this variant, the strikes are not sounded for the hour. Under column 1H, chimes are sounded only on the hour and carry the strikes with them, and so the associated tracks match the corresponding tracks under column 1.
Columns 2, 2C, and 2H represent the same kind of track and start time arrangement, but for a different chime or musical selection. The chime selection under columns 3, 3C, and 3H are also similar except that they provide for a silent space between the end of the musical interlude for the hour in track 63 and the sounding of the strikes in track 64 when approaching the hour such 1 o'clock. That is, rather than the overlap which possible between the musical melody and the strikes in the first and second chime series, this third chime series clearly separates the strikes from the musical selection, or eliminates them altogether under column 3C, or provides for only the strikes under column 3H. This is an appropriate arrangement for carillons.
The last chime, or musical selection appears under Column 4. In this selection, only a musical melody with, and strikes on, the hour are permitted.
In more detail, the first two chime series accommodate chimes with the following characteristics:
1) these series contain musical selections for up to four different quarter hour time events, and if the clock has no music in some or several of the quarters, then the tracks still exist for those quarters to satisfy the format but would contain only silence data. That is, the compact disc player 18 is directed by system controller 10 to play a track designated for a particular time even if the chimes selected for some discs do not have any music data corresponding thereto in the tracks chosen for those time slots;
2) the first quarter hour music is no longer then seven seconds excluding any decay of the last note;
3) the second quarter hour music is no longer then 15 seconds again excluding any decay of the last note;
4) the three-quarter hour music is no longer then 20 seconds, once again excluding any decay of the last note;
5) the fourth quarter hour music is no longer then 30 seconds excluding the striking of the hours;
6) the sound of the music that precedes the striking of the hour bell has not died out before the hour strikes start (if they exist), and therefore the fourth quarter hour music and striking bells must be on the same track;
7) the length of the hourly strike is unrestricted (if they exist); and
8) musical tones can be substituted for (or added to) the hourly strikes.
Research has indicated that most progressive chimes will be able to fit within these criteria.
The third chime series accommodates chimes with the following characteristics:
1) the chimes contain up to four quarter hours of music, and if the clock has no music in some or several of the quarter hours, then the tracks would still exist for those quarter hours but would contain only silence data;
2) the first quarter hour music is no longer then 15 seconds excluding the decay of the last note;
3) the second quarter hour music is no longer then 1 minute and allows for a strike tone at exactly the half hour;
4) the three-quarter hour music is no longer then 20 seconds excluding any decay of the last note;
5) the fourth quarter hour music is no longer then 50 seconds, not including the striking of the hours (if they exist);
6) the sound of the music that precedes the striking of the hour bell has died out before the hour strikes start (if they exist), and therefore the fourth quarter hour music and striking bells need not be on the same track; and
7) the length of the hourly strikes is unrestricted (if they exist).
Again, research indicates that many carillons will meet these criteria.
Finally, the fourth chime series accommodates chimes that play only on the hour, which is typical of many historical music house clocks. The following characteristics are permitted:
1) the chimes music plays only on the hour;
2) the chimes music can play a different tune each hour;
3) the chimes music tunes are no longer then 50 seconds excluding any decay of the last note; and
4) the chimes music is played before the hour and may finish with a strike tone or bell designating the number of the hour, the first strike of which is played exactly on the hour.
The chimes selection over these four formats taken together, as given in the compact disc format described in the tabulation above, will allow the flexibility for playing the chimes of the vast majority of chime playing clocks ever produced. However, while the above compact disc format provides a flexibility for playing such a variety of chimes, the format does not by itself accommodate the differences between the allowed times for playing under the format and the actual times of playing of any particular chime chosen to be placed on the compact disc within the format criteria. Rather, this accommodation is made by the placement of intentional silence data at the beginning of each track on the disc of such a length that the total time of that track meets the maximum allowed time under the compact disc format set out above.
For instance, in the first series of chimes, the chime passage associated with the first quarter hour event following the hour event is permitted to last for up to 8 seconds, and so the disc player will always be instructed by system controller 10 to start playing 10 seconds before the occurrence of the exact 15 minute time event following the hour, i.e. the first quarter hour following the hour, when the user has selected chime 1. Assume that on the first disc, the chime passage associated with the first quarter hour that is recorded as chime 1 lasts in actual playing time for only 4 seconds, and so the audio information data for that 4 seconds is recorded in that track. Then, in order that the musical melody end exactly on the quarter hour, silence data for 3 seconds must be added at the beginning of the track preceding that audio information, or music, data.
If the chime that is recorded on another compact disc as chime 1 has, for instance, audio information data in the corresponding hour event track which will lead to 6 seconds playing of a musical melody, then 1 seconds of silence data must be added to that track so that the track playing time reaches the format playing time permitted of 10 seconds.
This use of silence data in the tracks is particularly important in the fourth quarter hour so that the hour strike, if present, strikes exactly on the hour. In many instances, musical clocks play a short tune immediately prior to the hour followed by an hour bell that strikes exactly on the hour. In chime series 1 in the above table, the maximum length permitted for the fourth quarter hour musical selection preceding the hour is 30 seconds, and compact disc player 18 will always start playing 30 seconds before the hour. (Of course, the switching on of compact disc player 18 and getting the disc up to speed, and the like, will begin more then 30 seconds before the hour.) Since the fourth quarter hour musical selection and the hourly strikes are on the same track on the compact disc, the timing of the start of the tune must be adjusted such that the hour strike occurs exactly on the hour. This is again accomplished by adding silence data to the beginning of the track of an appropriate duration. If the time from the start of the fourth quarter hour musical melody to the first strike is, as an example, 22 seconds, then 8 seconds of silence data must be added to the beginning of the track for that chime. All of these silences are a critical part of the composition and editing of each track on each compact disc.
The example of the methodology described above for two different chime selections as chime 1 on two different discs is shown diagrammatically in FIG. 4 for the two different chimes, or musical selections, each entered as the same chime number 1 but on two different discs with the pertinent track portion from each being represented in that figure. The example shows the situation on approaching 2 o'clock. Both of the differing musical selections, as stated, are on the same numbered track (track 10) on their respective discs, and compact disc player 18 will be directed by system controller 10 to start playing that track at exactly 1:59:30 for each compact disc in accord one of the permitted start times for the fourth quarter hour following 1 o'clock in the above table.
However, the musical selection prelude to the hour in the case of the chime on the top disc in FIG. 4 is longer then its counterpart in the bottom disc shown there, 20 seconds on the top compared to 14 seconds on the bottom. Therefore, to have the hourly strike tone, or bell, strike exactly on the hour in both chimes, a compensating period of silence data is added to the track prior to the beginning of the musical selection in each of such a duration that the total time between the start of the track (1:59:30) and the first hour strike note is exactly 30 seconds. Thus, there is 10 seconds of silence data added after 1:59:30 in the upper track, and 16 seconds of silence data added after the 1:59:30 point on the lower track.
As can also be seen, the subsequent additional strikes and their duration, including their decays is not restricted by the disc format or the timing methodology, and does not require any coordination between the discs, subject to available disc data space. Thus, this formatting and timing arrangement allows recorded music from a wide variety of quite different clock music arrangements to be played on the one timekeeping system in either of FIGS. 1 or 2.
In the system of FIG. 2, audio storage programmable read-only memory 18' is shown as a subsystem concerning which greater detail is shown in FIG. 5. A random access memory, 40, serves as an address generator to provide a sequence of addresses to an audio storage programmable read-only memory, 41. System controller 10 provides on the address bus extending therefrom to memory 40 a starting address for the audio information data in a chime passage, and a stop address therefor, between which the selected chime audio data is stored in audio storage programmable read-only memory 41. Address generator 40 then provides all of the addresses in between these start and stop addresses to audio storage programmable read-only memory 41, one address being so provided with each cycle of an oscillator, 42, in its oscillatory output signal provided to address generator 40 which signal contains an oscillation frequency of 44.1 kHz.
The chime audio information data in the memory location at each such address supplied to audio storage programmable read only memory 41 by memory 40 is sequentially supplied to its output, and from there this data is in turn supplied to an analog-to-digital converter, 43, to provide the analog audio information output signal AUDIO IN. Thus, system controller 10 can control the timing of initiating the presentation of, and the selection of, audio data from a semiconductor memory as well as from a compact disc player.
System controller is shown in greater detail in the block diagram of FIGS. 6A and 6B for the situation of using a compact disc player for storage of audio information rather than a semiconductor memory. A microprocessor, 50, in FIG. 6A is used to control and manage the operation of the timekeeping system shown in FIGS. 1 and 2. Microprocessor 50 is operated on a time base set by a clock, 51, i.e. a crystal controlled oscillator, which provides an oscillatory output signal to microprocessor containing oscillations at a rate of 4.1952 MHz thereby enabling microprocessor 50 to execute commands at a rate proceeding 1.0 MHz.
Microprocessor 50 is connected to an address bus, 52, and a data bus, 53. Address bus 52 is a 16 bit bus, and data bus 53 is an 8 bit bus. The arithmetic logic unit of the microprocessor 50 is an 8 bit unit.
Keyboard 14 in control panel 12 is connected to a port in microprocessor 50 by an 8 bit bus to allow parallel operation. Audio storage compact disc player 18 is connected to microprocessor 50 by a single line for serial communication to player 18. Finally, microprocessor 50 has a port meeting the RS232 standard for serial communication, this being usable for connection with an external computer for analysis purposes to permit loading the timekeeping system program into that computer and permitting automated circuit analysis.
System controller 10 uses a random-access memory, 54, for temporary storage of variables being calculated or used by microprocessor 50. Such variables include the current time, copies of the contents or registers used in the timekeeping system, and storage of variables for various program needs in the performance by microprocessor 50 of the program operating the timekeeping system. Random-access memory 54 is a static random access memory configured on an 8k ×8 bit basis.
The address port of random-access memory 54 are connected to address bus 52, and the data port of is connected to data bus 53. In addition, power is supplied to random-access memory 54 through a capacitor and diode arrangement such that the absence of power on the power supply lines results in the capacitor supplying electric power to the memory until discharged. Thus, if electrical power is removed from across the timekeeping system circuitry or if a low battery voltage condition has been detected resulting in the reduction by the system of voltage across the system, random-access memory 54 will continue to store the state of the system registers. As a result, microprocessor 50, once full power is restored to the timekeeping system circuitry, can obtain the previous timekeeping system register condition at the time of power loss and restore the timekeeping system circuit to that condition.
Microprocessor 50 is also connected to a further memory in FIG. 6B, this being a programmable read-only memory, 55, which is also configured on an 8k ×8 bit basis. This memory contains all of the program information for microprocessor 50 as well as several control tables. These control tables include the serial commands for audio storage compact disc play 18, the formatting tables involving chime or musical start times and the chime or music selection compact disc tracks, or programmable read-only memory start and stop addresses, for the various chimes. In addition, display 13 is a liquid crystal display and a display table is also stored in memory 55 for properly selecting display segments to form various selected alphanumeric display characters. Programmable read only memory 55 is also connected to address bus 52 at its address port and to data bus 53 at its data port.
Once electrical power is applied to the time keeping system, microprocessor 50 will fetch a starting address from programmable read-only memory 55, this address being the one in which the system operating program stored in memory 55 begins. As soon as microprocessor 50 has this address, that processor will begin to respond to commands listed in that operating program, and will continually manage and monitor the timekeeping system circuitry. Primarily, among these program directives, microprocessor 50 attempts to match the current time (to be supplied thereto by a real time clock as will be described below) with any of the times stored in the format tables contained in memory 55. If one of the stored times matches the current time, microprocessor 50 will then fetch from the format tables the associated audio storage compact disc player 18 track, or audio storage programmable read-only memory 18' start and stop addresses, and transmit this information data to either the player or the memory to begin having it provide the data for the selected chime or musical passage.
As indicated, a real time clock, 56, is used to provide all of the timekeeping duties in the timekeeping system. Real time clock 56 is connected to microprocessor 50 in FIG. 6 by address bus 52 at its address port, to data bus 53 at its data port, and by an interrupt line at an interrupt output thereof. On a provision of electrical power to the circuitry of the timekeeping system, microprocessor 50 will provide data to real time clock 56 indicating that it should begin operating with a time of 12:00:00 a.m. Thereafter, real time clock 56 will maintain the current time through its internal circuitry based on its crystal controlled oscillator establishing its time base. If the user of the timekeeping system should change the times through entries of key pad 14, microprocessor 50 will load this new data into real time clock 56, which will then continue to keep current time from this newly introduced time reference.
Once every second, real time clock 56 generates an interrupt (the "second interrupt") on the single line connecting it to the corresponding interrupt input on microprocessor 50 thereby indicating another time passage increment of one second having occurred. Microprocessor 50 responds on each such occurrence by obtaining the current time from real time clock 56 over data bus 53, and so begins another comparison of this newly obtained current time value with the format table time values stored in programmable read-only memory 55 to determine when the audio storage source used should next begin supplying audio information data.
Real time clock 56 is also supplied electrical power through the same capacitor and diode used in connection with random-access memory 54 to assure its ability to operate until sufficient discharging of the capacitor occurs following a loss of electrical power. Thus, the actual time will also be of available to microprocessor 50 in that discharge period should electrical power be resupplied before too great a discharge of that capacitor to thereby begin again accurate operation of the timekeeping system circuitry.
Microprocessor 50 operates control registers in which it sets logic values to form signals used to direct operation of other system components in the timekeeping system, and a status register in which it keeps track of the status of the timekeeping system. Each of these registers are 8 bit registers. Microprocessor 50 is connected to these control registers and the status register by data bus 53 in FIGS. 6A and 6B.
The first of these control registers, 57, also indicated to be control register 1 in FIG. 6B, supplies a first signal labeled AUDIO OFF which is used to switch on and off electrical power to an audio amplifier used to drive loudspeakers 19 to be described below. Control register 1 provides another signal, LIGHT CONTROL, for switching the backlight of liquid crystal display 13 on or off. A further signal supplied thereby, CD POWER CONTROL, switches electrical power on and off to audio storage compact disc player 18, and to an audio controller to be described below. Finally, four signals on a bus, used to control the supply of electrical power to the various analog clock displays in time display 17 through a clock controller to be described below, are provided by control register 1 to that clock controller.
The second control register, 58, also designated control register 2 in FIG. 6A, has two output buses, one going to the audio controller to be described below and the other going to the liquid crystal display controller also to be described below. Each bus has three lines, one for data, one a clock control line to control loading of the data, and an enable line.
The status register, designated 59 in FIG. 6B, receives several signals indicating the status of various control signals which can then be checked as needed by microprocessor 50. The BATTERY LOW signal over two lines indicates both (a) a loss of primary power with the result that the voltage into the power control to be described below is below 7.2 volts, and (b) a drop in battery voltage below 7.8 volts in situations where primary electrical power to the timekeeping system has not been lost. The next three control signals monitored, CD POWER CONTROL, LIGHT CONTROL, and AUDIO OFF, have been previously described in connection with control register 1. The signal PEAK AUDIO DETECTOR is the output signal of an audio level peak detector which indicates whether an audio output signal is currently being detected or not, which will be referred to below. Finally, the signal ADC CONVERSION DONE contains information as to the completion of a conversion of a value in an analog signal to a corresponding digital value by an analog-to-digital converter to be described below.
A control/decode logic circuit, 60, is connected in FIG. 6A to, and decodes signals on, address bus 52. If an address associated with another subsystem block, to which an output of circuit 60 is connected in FIG. 6 has been decoded, control/decode logic circuit 60 generates an enable signal which is sent to the block so addressed. This permits microprocessor 50 to send or retrieve data from that block.
As directed by microprocessor 50 through register 57, a clock controller, 61, in FIG. 6B supplies electrical power to the four independently controlled clock motors, each configured as shown in FIG. 3, to operate the four analog clock displays in time display 17: the main hour and minute clock, the day of the week clock, the moon position clock, and the moon phase clock. The main clock, as are all the analog clocks in display 17, is set to an initial position manually to match the correct current time at the setting occurrence, which is also kept by real time clock 56 and microprocessor 50 and can be displayed on liquid crystal display 13. The main clock always runs continuously after electrical power has been supplied to the timekeeping system so that the setting of that clock to the proper time (typically matching the current time that can be displayed on the digital clock shown in display 13) will start that clock keeping correct time.
However, as indicated above in connection with the description of the independently controlled clock motor of FIG. 3, such independently controlled clock motors operating the analog display clocks are each operated with a self-contained and independent time base provided by an oscillator in that arrangement. Since the crystal in the crystal controlled oscillator in an independently controlled clock motor will never exactly match the crystal in real time clock 56, and given the passage of sufficient time, the occurrences of rotations of the rotor in an independently controlled clock motor used in display 17 will begin to diverge in time from the appearances of "second interrupts" from real time clock 56, rather than occurring essentially simultaneously, if not resynchronized.
Thus, in FIG. 7A, the one Hertz sequence of pulses representing the "second interrupts" provided by real time clock 56 to microprocessor 50 is shown in solid line form. The one second time duration equivalent angular rotation occurrences of a clock motor rotor in an actuator 23 are shown in dashed lines indicating that the time drift between the crystals of the oscillators in each is such as to cause these motor rotation occurrences to lag behind the real time Clock "second interrupt" pulses. The opposite situation is shown in FIG. 7B where the rotor rotation occurrences lead the "second interrupt" pulses from real time clock 56. In either of FIGS. 7A and 7B, the gap between the dashed line pulses and the solid pulses will grow over time as the crystals (or other oscillator circuit components) in real time clock 56 and the independently controlled clock motors used in display 17 continue to cause the oscillators therein to drift apart in time.
Since the maximum oscillation frequency drift rate for these crystals over time is known and can be specified, the timekeeping system of FIGS. 1 and 2 can resynchronize the main clock independently controlled clock motor rotor rotations with the one Hertz "second interrupts" of real time clock 56 by simply turning power off to the main clock independently controlled clock motor more often than the amount of time required for the drift in oscillator frequency differences to exceed half the period of a cycle in the sequence of real time clock "second interrupt" pulses. The desired resynchronization is thus achieved since, as described above, the application of electrical power to a independently controlled clock motor almost immediately causes a rotation of the rotor in the clock motor therein. Since the termination of electrical power to the main clock independently controlled clock motor can be made to occur essentially in conjunction with a "second interrupt" pulse from real time clock 56, and since such electrical power can be reapplied in just milliseconds while still obtaining the rotation of the clock motor rotor, there is, as a result of such a power termination, an effective resynchronization achieved between the rotor rotations of the main clock independently controlled clock motor and the "second interrupts" provided by real time clock 56.
The same resynchronization procedure can be used with the independently controlled clock motors for the other three analog clocks, but there is no necessity for specially providing such an arrangement for these other three clocks as there is with the main clock. This is true because of the manner in which the other three clocks have their effective rotation rates slowed to the point of keeping them matched to the time relationships they depict, all of which are based on time bases of a much lower frequency then 1 Hertz.
As indicated above, actuator 23, in an independently controlled clock motor of the nature described in connection with FIG. 3, has a rotor which completes a rotation every two seconds, and further has gearing arrangements with concentrically mounted, cylindrical shell shafts one of which rotates fully once a minute, another which completes a rotation once an hour, and a final one completing a rotation once every twelve hours. However, the twelve hour clock motor shaft can be controlled so that it completes a rotation in one week instead of 12 hours to establish the proper drive arrangement for operating the day clock. This is accomplished by stopping the movement of the 12 hour shaft for a total of six and a half days every week through terminating electrical power to the independently controlled clock motor for the day clock for that period of time.
Alternatively, electrical power to the independently controlled clock motor for the day clock can be supplied and withheld in a ratio of power on for one duration and power off for 13 similar durations. The latter method will make the lack of motion in the analog display for the day clock unnoticeable to an observer if the durations chosen are sufficiently brief. Thus, if the independently controlled clock motor for the day clock is supplied electrical power for one minute and no electrical power for the next 13 minutes, and this pattern is repeated continuously, the day clock will appear to move smoothly because 14 minutes is a very small increment of the time in a total week, which then becomes the period of rotation of the 12 hour clock shaft and so of the hand driven thereby over the week based dial face use with the day clock. Microprocessor 50 and programmable read only memory 55 can be easily programmed to provide this on-off pattern of electrical power supply to the day clock independently controlled clock motor.
Another electrical power on-off pattern that can be usefully employed is to have the desired ratio of electrical power on and off times accomplished within every minute or within every hour that the day clock is used. In this situation, the day clock independently controlled clock motor is to be supplied electrical power for one fourteenth of every hour, or 257.14286 seconds. However, typically, an independently controlled clock motor operates only in integer seconds so that a residual error accumulates every hour totalling a fraction of a second (0.14286) if the day clock independently controlled clock motor is supplied electrical power for possible integer 257 seconds each hour.
On the other hand, this accumulation can be easily compensated by having power supplied for an extra period of time to the day clock independently controlled clock motor once a day. Thus, after a day has passed, an accumulative error of 3.42857 seconds (0.14286×24) has accumulated, and 3 seconds of this can be compensated by supplying electrical power to this independently controlled clock motor for an extra 3 seconds once per day. If the result in diminished error (0.42857 seconds per day) needs to be further reduced, additional corrections can be introduced in a similar fashion once a week, or once a month, or even once a year. In most situations, the value of such extra corrections is quickly diminished as accumulative error quickly becomes less than the intrinsic accuracy of the crystal in the day clock independently controlled clock motor itself.
Similar principles apply to creating the movements of the dials which rotate in synchronism with the rotation of the moon about the earth, and with the phases of the moon. In the moon position clock, the rotation of the earth under the moon plus the motion of the moon during its rotation results in a cycle lasting 24 hours, 50 minutes, and 28 seconds. Assuming the dial on the 12 hour clock shaft is used, the moon position independently controlled clock motor would need to be supplied electrical power 28.98421 seconds every minute with no power being supplied for the remainder of the minute. Since, again, most such independently controlled clock motors operate on integer seconds only, the moon position clock motor and control circuit can be supplied electrical power for 29 seconds leaving an accumulating error of 0.01579 seconds every minute. This is the same as 22.73651 seconds every day which can be easily corrected by reducing the time electrical power is supplied by 23 seconds during some point in each day. Of course, further corrections can be made as indicated above if thought desired. Hence, such independently controlled clock motors can be made to keep time on any desired time base by microprocessor 50 and memory 55 through the foregoing methods.
As indicated above, audio storage compact disc player 18 (or audio storage programmable read-only memory 18') is controlled at an output port of microprocessor 50 over a serial communication line. The actual command codes recognized by player 18 for operation are stored in programmable read-only memory 55. The command codes are initially read from the programmable read-only memory by microprocessor 50, and the proper commands for player 18 are then assembled in microprocessor 50 and transmitted serially out of the microprocessor port to player 18. Thus, microprocessor 50 is directly the controller for audio storage compact disc player 18 (or audio storage programmable read-only memory 18'). Storing the command codes appropriate to the choice of a compact disc player to service player 18 permits a wide variety of such players to be used through merely changing the corresponding command table in memory 55. Since the commands stored in memory 55 for audio storage compact disc player 18 are sufficient to control starting, stopping, pausing, and advancing that player, microprocessor 50 can start the player retrieving data from its compact disc at any programmed time, and the data can be selected easily through directing the player to provide data from the selected track.
Electrical power to audio storage compact disc player 18 is controlled by a compact disc player power switch, 62, in FIG. 6A which receives a power input and the control signal CD POWER CONTROL. Of course, this control signal is supplied by microprocessor 50 to register 57 so that it can indeed totally control audio storage compact disc player 18.
A liquid crystal display controller, 63, controls liquid crystal display 13 segment by segment to thereby control which alphanumeric characters are displayed in each segment character provided therein. The system allows the master time kept by real time clock 56 to be displayed in display 13, as indicated above, and the nighttime starting and ending times for turning down the volume of the chimes to be heard through adjusting the audio controller to be described below. These times are set by position of wipers on the pair of potentiometers through manipulating appropriate buttons in control panel 12. Also, chimes can be caused to be played at any set time through controlling a potentiometer in control panel 12 to thereby allow the clock to serve as an alarm. In addition, display 13 can permit track and melody selection information to be displayed thereon, all under the control of microprocessor 50 operating through register 58.
An analog-to-digital converter, 64, is used to convert analog potentiometer settings into corresponding digital signals. The converter used is a 8 bit converter having a linearity of plus or minus the least significant bit, and can complete a conversion time 50 μs. Microprocessor 50 directs converter 64 over address bus 52 to switch its input to the analog signal source to be converted through a multiplexing arrangement in the converter, and to convert the analog value received after such switching. Microprocessor 50 checks register 59 to determine such a conversion is done. Thereafter, microprocessor 50 reads the data related to the conversion on data base 53.
The multiplexing arrangement in converter 64 allows switching between the analog voltages supplied by the day volume and night volume potentiometers 15 and 16 and, in addition, to the settings for the potentiometers used for choosing the bass and treble levels for the audio and for the balance between the midrange speakers, these audio control being set by positioning wipers on potentiometer mounted internally to the timekeeping system but which could be made available in control panel 12. The various data for controlling the audio so obtained by microprocessor 50 is then inserted in register 58 where control signals are transmitted to an audio controller, 65.
Audio controller 65 in FIG. 6B is, as stated, used to adjust the volume, treble, bass and speaker volume balance in the analog audio signals provided by audio storage compact disk player 18 (or audio storage programmable read only memory 18') as the AUDIO IN signals supplied to audio controller 65. These two analog stereophonic signals, as adjusted by audio controller 65, are then transmitted to an audio amplifier, 66. As indicated, audio controller 65 is controlled by microprocessor 50 through register 58 over the bus extending therebetween, and through register 57 which controls the power drawn by audio controller 65 through a switch in that controller with the signal CD POWER CONTROL.
Audio amplifier 66 is a fixed gain (10) audio amplifier. Amplifier 66 receives the analog audio signals from controller 65, amplifies them, and provides them to loudspeakers 19. One of the analog stereophonic signals is supplied to the right midrange speaker, and the remaining one is supplied to both the left midrange speaker and the bass speaker. Microprocessor 50, during times of audio inactivity, can shut off amplifier 66 through register 57 by directing the proper signal AUDIO OFF to amplifier 66. An audio activity detector, 67, or audio level peak detector, is used to detect a signal being transmitted over the wire to the left midrange speaker and the bass speaker to monitor the presence of audio activity. The signal from detector 67, as indicated above, is then provided to status register 59 to indicate the presence or absence of such audio activity. Through monitoring audio activity, microprocessor 50 can switch off portions of the timekeeping circuit not being used in the absence of audio to conserve power including stopping any play of audio storage compact disk player 18. Also, many compact disc players have the capability to be programmed to play a selected track, or a selected series of tracks, and to then stop once such play is completed so as to require no outside commands to be shut off.
Power for various portions of timekeeping circuitry is provided as appropriate to such portions by power controller, 68, receiving the BATTERY IN input from battery power supply 11. Power controller 68 also has the circuitry for monitoring battery voltage, and provides the information resulting from such monitoring to status register 59 as described above.
A general operation flow chart is shown in FIGS. 8A and 8B for system controller 10. Though much detail is omitted, the general flow of operation of the system is presented along the lines described in the foregoing text. The chart is specifically directed toward the use of a compact disk player for the audio information storage rather than a programmable read only memory.
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. | A timekeeping system for providing selected ones of a plurality of audio signal portions, obtained from stored audio information, to be synchronized with selected time events even though the audio signal portions are of durations differing from one another. A rotator, operating with independent rotation timing, can be synchronized to the timing generator output signal by at least temporarily removing power from the rotator before the rotation period thereof drifts by more than a selected fraction of the period of the timing generator output signal. Further, the rotator rotation period for the angular rotation of the output structure can be effectively increased by selectively removing power from the rotator. | 6 |
This application claims the benefit of Korean Applications No. P2003-51511 filed on Jul. 25, 2003, P2003-51512 filed on Jul. 25, 2003, and P2003-72247 filed on Oct. 16, 2003, which are hereby incorporated by reference.
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to a washing machine, and more particularly, to a method of performing a spinning operation for a washing machine.
2. Discussion of the Related Art
Generally, a washing machine performs washing by executing a washing operation, a rinsing operation, and a spinning operation. The spinning operation includes a load pre-balancing cycle, a load weighing cycle, a load balancing cycle, and a main spinning cycle.
According to the principles of the related art, before the main spinning cycle, a microprocessor determines a load weight of wet clothes to measure spinning operation parameters, which helps to balance the load in the tub. However, it is very likely that some wet clothes in the washing machine become tangled one another by a nature of the mechanism of a drum washing machine. Consequently, an unevenly distributed load of the clothes in the washing machine creates an unnecessary moment about the center of a tub, which makes the motor irregularly rotate. For example, when a chunk of the wet clothes spins from a top to a bottom of the tub in the washing machine, the moment created by a gravity of the chunk forcibly rotates the motor over its limit. On the other hand, when the chunk spins from the bottom to the top, it creates an opposite rotational force that prevents the motor from rotating in the right direction. Therefore, the entanglement of the clothes causes a vibration of the tub, a nose, and a walking of the washing machine, all of which resulted in inaccuracy of the load weight of the wet clothes. As a result, the inaccurate load weight causes the inaccurate spinning operation parameters, which influence a performance of the main spinning operation.
According to the principles of the related art, after the load weighing cycle, the rotational speeds up the tub with a constant acceleration regardless of the load weight to perform the load balancing cycle. Speeding with the constant acceleration has caused a problem of the vibration of the tub, the walking of the washing machine, and the poor performance of the main spinning cycle. For example, if 10 kg clothes are not evenly distributed and a relatively low speed is used to redistribute them, it will be very difficult for the relatively low speed to not only balance the 10 kg load evenly but also reach a desired speed quickly. So to speak, the 10 kg unbalanced load creates the moment about the center of the tub. The moment then causes the vibration of the motor, the noise, the walking of the washing machine, and a lagging of the cycle. Thus, the load balancing cycle needs to last longer, meaning that more power is needed and inefficiency of the spinning operation is occurred.
During the load balancing cycle, the microprocessor determines an unbalancing value, which represents how irregularly the load of the wet clothes is distributed in the washing machine. Even though the microprocessor determines whether the main spinning operation can be carried out dependent upon the unbalancing value, the load is not likely to be evenly balanced for the smooth performance of the main spinning cycle because the unbalanced distribution levels are determined below a resonance frequency range. It is realized that the unbalanced distribution levels alter prominently within the resonance frequency range. Therefore, the unbalance load determined below the resonance frequency range is not accurate, which influences the performance of the main spinning cycle.
SUMMARY OF THE INVENTION
Accordingly, the present invention is directed to a washing machine that substantially obviates one or more problems due to limitations and disadvantages of the related art.
An object of the present invention is to provide more accurate washing parameters such as load weight of wet clothes, acceleration rates while balancing a load of the wet clothes, and to minimize the unbalanced distribution level of the wet clothes within a tub so that the performance of the spinning operation can be improved.
Additional advantages, objects, and features of the invention will be set forth in part in the description which follows and in part will become apparent to those having ordinary skill in the art upon examination of the following or may be learned from practice of the invention. The objectives and other advantages of the invention may be realized and attained by the structure particularly pointed out in the written description and claims hereof as well as the appended drawings.
To achieve these objects and other advantages and in accordance with the purpose of the invention, as embodied and broadly described herein, a method of controlling a spinning operation of a washing machine includes the steps of measuring the load weight of the wet clothes contained in the tub to be spun, determining an optimal acceleration rate based upon the measured load weight, and increasing a rotational speed of the tub to a first predetermined speed at the optimal acceleration rate in order to minimize unbalanced distribution of the wet clothes within the tub.
In another aspect of the present invention, a method of controlling a spinning operation of a washing machine includes the steps of measuring a load weight of wet clothes contained in a tub to be spun, selecting at least two distinct optimal acceleration rates if the measured load weight belongs to a particular acceleration range, and increasing the rotational speed of the tub to a first predetermined speed at the selected optimal acceleration rates alternately in order to minimize unbalanced distribution of the wet clothes within the tub.
In another aspect of the present invention, a method of controlling a spinning operation of a washing machine includes the steps of measuring a load weight of wet clothes contained in a tub to be spun, determining an optimal acceleration rate based upon the measured load weight, and increasing a rotational speed of the tub to a first predetermined speed at the optimal acceleration rate in order to minimize unbalanced distribution of the wet clothes within the tub. The method further includes the steps of measuring an unbalanced distribution level of the wet clothes within the tub while rotating the tub at the first predetermined speed, and interrupting the spinning operation of the washing machine when the measured unbalanced distribution level is greater than a predetermined value.
In another aspect of the present invention, a method of controlling a spinning operation of a washing machine includes the steps of measuring a first unbalanced distribution level of wet cloths contained within the tub while rotating the tub at a first speed, and interrupting the spinning operation of the washing machine when the first unbalanced distribution level is greater than a first predetermined value. The method further includes the steps of measuring a second unbalanced distribution level of the wet clothes while rotating the tub at a second speed selected from a resonance frequency range of the washing machine, and interrupting the spinning operation of the washing machine when a difference between the first and second unbalanced distribution levels is greater than a second predetermined value.
In another aspect of the present invention, a method of controlling a spinning operation of a washing machine includes the steps of measuring a load weight of the wet clothes contained in a tub to be spun, determining an optimal acceleration rate based upon the measured load weight, and increasing the rotational speed of the tub to a first speed at the optimal acceleration rate in order to minimize unbalanced distribution of the wet clothes within the tub. The method further includes the steps of measuring a first unbalanced distribution level of the wet clothes while rotating the tub at the first speed, interrupting the spinning operation of the washing machine when the first unbalanced distribution level is greater than a first predetermined value, measuring a second unbalanced distribution level of the wet clothes while rotating the tub at a second speed selected from a resonance frequency range of the washing machine, and interrupting the spinning operation of the washing machine when a difference between the first and second unbalanced distribution levels is greater than a second predetermined value.
It is to be understood that both the foregoing general description and the following detailed description of the present invention are exemplary and explanatory and are intended to provide further explanation of the invention as claimed.
BRIEF DESCRIPTION OF THE DRAWINGS
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this application, illustrate embodiment(s) of the invention and together with the description serve to explain the principle of the invention. In the drawings;
FIG. 1 illustrates a prospective side view of a washing machine in accordance with the present invention;
FIG. 2 is a flowchart illustrating one embodiment of the method of controlling a spinning operation of the washing machine in accordance with the present invention;
FIG. 3 is a graph illustrating a spinning operation of the washing machine including a load balancing cycle;
FIG. 4 is a graph illustrating a spinning operation of the washing machine including a first load balancing cycle and a second load balancing cycle;
FIG. 5 is a flowchart illustrating another embodiment of the method of controlling a spinning operation of the washing machine in accordance with the present invention; and
FIG. 6 is a graph illustrating a spinning operation of the washing machine, in which the unbalanced distribution level of the wet clothes is measured more than once.
DETAILED DESCRIPTION OF THE INVENTION
Reference will now be made in detail to the preferred embodiments of the present invention, examples of which are illustrated in the accompanying drawings. Wherever possible, the same reference numbers will be used throughout the drawings to refer to the same or like parts.
FIG. 1 illustrates a prospective side view of a washing machine in accordance with the present invention. According to FIG. 1 , the washing machine includes a cabinet 5 , a tub 3 , and a drum 9 . The drum 9 includes a drum axle 13 , which transmits a driving force of a DC motor 6 to the drum 9 . For smooth operation of the motor 6 , the drum axle 13 is equipped with bearings 12 at its both ends, which are placed in a bearing housing (not illustrated). The motor 6 itself contains a stator 7 and a rotor 8 which is directly connected to the drum 9 and rotates it. The washing machine also includes a hanging spring 4 which functions as a support between an inner top of the cabinet 5 and an outer top of the tub 3 . In order to reduce vibration of the tub 3 , the washing machine includes a friction damper 10 provided between an inner bottom of the cabinet 5 and the outer bottom of the tub 3 . In addition, the washing machine includes a motor sensor 11 which measures a number of the rotor 8 rotation, which represents the speed of the motor 6 .
FIG. 2 is a flow chart illustrating a method of controlling a spinning operation of the washing machine shown in FIG. 1 according to one embodiment of the present invention. According to FIG. 2 , a microprocessor (not illustrated) of the washing machine initially increases the rotational speed of the tub 3 from zero to a second predetermined speed. It then measures an acceleration time that it takes for the rotational speed to reach the second predetermined speed from zero.
Finally, it determines the load weight of the wet clothes based upon the measured acceleration (S 201 ). Measuring the load weight of the wet clothes improves the performance of the washing machine by obtaining more accurate washing parameters. An example of the washing parameters is the acceleration rate at which the microprocessor increases the rotational speed. The microprocessor determines the optimal acceleration rate based on the measured load weight and increases the rotational speed at the determined optimal acceleration rate (S 202 ).
According to the present invention, the corresponding acceleration rate now helps rebalance the load of the clothes so efficiently that it saves time and neither vibrates the tub 3 nor creates a noise. Thus, the load balancing cycle is shortened. Now, the motor 6 rotates at the corresponding acceleration rate to balance the load and the microprocessor determines the unbalanced distribution level, which represents how irregularly the load is distributed in the tub 3 (S 203 ). If the unbalanced distribution level is less than the reference value (S 204 ), then it moves onto the main spinning cycle to perform. (S 205 ). Otherwise, the microprocessor interrupts the spinning operation and shuts off a power supply to the motor 6 that rotates the tub 3 for a predetermined time (S 206 ) and goes back to the step of increasing the rotational speed at the determined optimal acceleration rate upon the measured load weight (S 202 ).
FIG. 3 is a graph illustrating a spinning operation including a determined optimal acceleration rate during a load balancing cycle in accordance with the present invention. During the load balancing cycle, the motor 6 rotates up to 108 RPM at the determined acceleration rate based upon the load measured weight. According to the present invention, table 1 below shows how the acceleration rate differentiates upon the load weight.
TABLE 1
Acceleration rate varies dependent upon load weight.
Load Weight
Acceleration Rate (RPM/ms)
Light
1/160, 1/190 (alternate rotation)
Medium Light
1/150
Medium Heavy
1/180
Heavy
1/200
As tabulated in the table 1, the microprocessor determines the acceleration rate which corresponds to the load weight. A plurality of the acceleration rates is predetermined for a plurality of the load weight ranges. Each load weight range is assigned to a certain acceleration rate. Exceptionally, for the light load, the microprocessor alternately increases the rotational speed of the tub 3 to a predetermined speed by selecting the two determined optimal acceleration rates one by one in order to minimize the unbalanced distribution of the wet clothes within the tub 3 . The acceleration rate noticeably varies as the load weight changes in order to optimize efficiency of the load balancing cycle. To be more specific, the acceleration rate is inversely proportional to the load weight. The acceleration rate helps to quickly lower the unbalanced distribution level. Then, it will proceed to the main spinning cycle if the unbalanced distribution level is less than the reference value. As a note, the unit of the acceleration rate is RPM/ms, meaning that the speed of the motor increases by 1 revolution per minute (RPM) in 1 millisecond.
In addition to the load balancing cycle specified above, it may include an additional step of a load balancing cycle prior to the load weighing cycle. The additional step helps to measure the load weight more accurately by reducing other side effects such as the vibration of the motor and the walking of the washing machine. For example, FIG. 4 is a graph illustrating a spinning operation including the additional step of a first load balancing cycle prior to the load weighing cycle, and a step of a second load balancing cycle with the determined acceleration rate. It is realized that the rotational speed needs to be approximately as low as 46 RPM due to the fact that below 50 RPM a gravity of the load prevails over a centrifugal force of the motor so that the load moves freely and gets balanced easily. During the first load balancing cycle, the motor alternately rotates with the load at the predetermined speed at least one cycle in each direction, a first direction and a second direction.
It is likely that at the predetermined speed the load reaches a top of the tub 3 , it falls down to a bottom of the tub 3 due to the gravity, instead of sticking to a wall of the tub 3 and spinning with it by the centrifugal force. Fallen by the gravity, the unbalanced load is evenly spread out in the tub 3 . For example, a heavy chunk of the tangled load is spinning around in the tub 3 causing the vibration of the motor. The microprocessor can spread out the heavy chunk of the tangled load by free-falling from the top and being hit on the bottom of the tub 3 , continuously.
FIG. 5 is a flowchart illustrating a spinning operation including a plurality of unbalanced distribution levels in accordance with the present invention. The microprocessor measures a first unbalanced distribution level at a first speed below a resonance frequency range of the motor (S 501 ). The resonance frequency range of the washing machine is usually from 170 rpm to 250 rpm and the main spinning cycle is frequently performed above 300 rpm. The first unbalanced distribution level is determined by measuring a speed variation of a motor that rotates the tub 3 . For example, if the motor rotates at 100 rpm, the microprocessor measures how much the speed fluctuates at 100 rpm. It then determines if the first unbalanced distribution level is less than a first reference value (S 502 ). It interrupts the spinning operation of the washing machine and shuts off the power supply to the motor 6 that rotates the tub 3 for a predetermined time when the first unbalance value is greater than a first reference value (S 505 ). If the first unbalanced distribution level is less than the first reference value, the microprocessor measures a second unbalanced distribution level (S 503 ). The important is that it measures the second unbalanced distribution level at a second speed selected from the resonance frequency of the washing machine.
Now, the microprocessor determines difference between the first unbalanced distribution level and the second unbalanced distribution level. It may calculate the difference by dividing the first unbalanced distribution level by the second unbalanced distribution level, as a ratio. Or, it may simply subtract one from the other. It then compares the difference to a second reference value to determine if the difference is less than the second reference value. (S 504 ). It interrupts the spinning operation of the washing machine and shuts off the power supply to the motor 6 for the predetermined time when the difference is greater than the second reference value (S 505 ). If the difference is less than the second reference value, then it proceeds to the main spinning cycle (S 506 ).
FIG. 6 is a graph illustrating a spinning operation including a plurality of unbalanced distribution levels in accordance with the present invention. The present invention measures the plurality of unbalanced distribution levels. For example, as shown in FIG. 6 , a first unbalanced distribution level is measured at 108 rpm below the resonance frequency range. “A” denotes a last minute drain-out stage during which the microprocessor speeds up the motor to 170 rpm for a predetermined time in order to drain out leftover water in the tub 3 . If the first unbalanced distribution level is less than the first reference value, the microprocessor stores the first unbalance distribution level and determines a second unbalance distribution level at 170 rpm selected from the resonance frequency range.
As experimentally proved, the first unbalanced distribution level determined below the resonance frequency range is prominently different from the second one within the resonance frequency range. If proceeding to the main spinning cycle is determined based on the only first unbalanced distribution level, the washing machine will be unstably performed causing the vibration, walking of the washing machine, and noises from it. Determining a difference between the first and the second determined unbalanced distribution levels and considering it as the unbalanced distribution level, the present invention obtains smoother and improved performance of the washing machine. The microprocessor performs the last minute drain-out stage at 300 rpm.
Therefore, according to the present invention, the spinning operation includes the optional load first balancing cycle which untangles the load, the load weighing cycle which measures the load weight, the load balancing cycle which balances the load, and the main spinning cycle.
It will be apparent to those skilled in the art that various modifications and variations can be made in the present invention without departing from the spirit or scope of the inventions. Thus, it is intended that the present invention covers the modifications and variations of this invention provided they come within the scope of the appended claims and their equivalents. | A method of performing a spinning operation of a washing machine is disclosed. First, a load weight of wet clothes contained in a tub is measured, and an optimal acceleration rate is calculated based upon the measured load weight. Finally, a rotational speed of the tub is gradually increased up to a predetermined speed at the calculated optimal acceleration rate such that the unbalanced distribution of the wet clothes within the tub is minimized. | 3 |
BACKGROUND OF THE INVENTION
Novelty siding has long been available to the public in the form of elongated boards having an upper edge with an integral upstanding tongue and a lower edge with a tongue recess, rabbett or groove, the front face of each board usually having a groove to simulate clapboarding.
Such siding, panelling or sheathing is shown in many forms in, for example, a publication entitled "Standard Patterns", Western Wood Products Co. of Western Wood Products Association, Yeon Building, Portland, Oregon 97204.
Prior patents exemplary of such siding, decking, flooring, roofing or panelling are the following:
U.S. Pat. No. 2,400,357 May 14, 1946 to Krajci
U.S. Pat. No. 3,262,239 July 26, 1966 to Mills
U.S. Pat. No. 4,065,899 Jan. 3, 1978 to Kirkhuff
in all of which the siding unit has an upper tongue and lower tongue groove but requires attachment to a substrate of boards or plyscore.
In the following U.S. Patents, however, all of which also disclose an upper tongue and a lower tongue recess, no backer board is used and the units are attached directly to the studs:
U.S. Pat. No. 2,231,007 Feb. 11, 1941 to Vane
U.S. Pat. No. 2,390,087 Dec. 4, 1945 to Fink
U.S. Pat. No. 2,693,621 Nov. 9, 1954 to Errion
U.S. Pat. No. 2,831,218 Apr. 22, 1958 to Stark
U.S. Pat. No. 3,626,439 Dec. 7, 1971 to Knessel
U.S. Pat. No. 4,034,439 July 12, 1977 to Sanders
Most of the above mentioned patents disclose an outer, lower, integral depending rib on the lower edge of the board for covering the joint with the next lower most board.
The above mentioned Mills U.S. Pat. No. 3,262,239, Fink U.S. Pat. No. 2,390,087 and Stark U.S. Pat. No. 2,831,218 all disclose laminated board units, and the Errion U.S. Pat. No. 2,693,621 discloses one piece units, which are of sufficient thickness, strength and insulative properties to be directly applied to frame studding thereby eliminating the cost and expense of an intervening substrate of shiplapped boards, plyscore or composition board.
SUMMARY OF THE INVENTION
The combined backer board and siding of this invention is characterized by being sufficiently thick at the top and bottom to serve as a rigid connection between upright studs without other support. The upper edge is preferably at least one and one quarter inches in thickness as is the lower edge, the lower edge being at least about one and one half inches in thickness when the outer or front face is tapered. Unlike the above prior patents, in this invention the upper edge contains a front, upstanding tongue and a rear, downward sloping surface to shed rainwater, there being no pockets, or grooves, in the upper edge to permit water to accumulate. The lower edge includes a rear depending tongue and a front depending tongue separated by a tongue groove which receives the tongue of the next lower board. Standard boards of uniform thickness are used and preferably a compressible gasket between upstanding tongue and tongue groove is provided to seal the joint between boards.
To avoid leakage of air or water at the joints, when the upstanding tongue is integral the tongue groove in the lower edge is made of slightly greater dimensions then the corresponding dimensions of the tongue to provide a predetermined clearance space for caulking or sealing compound. No caulking is necessary when the seal is a separate gasket of compressible material.
To enable nailing of each unit directly onto the studs of a building a nailing surface, or plane, at an angle of about 45° to the vertical may be provided on the front upper edge. A corresponding surface, or plane, at a different angle is formed on the rear face of the rib depending from the front of the lower edge to create an air space for ventilating the joint.
In one form of the invention the rear face of the unit is flatwise against the studs while a front face is inclined to present a clapboard appearance. In another form of the unit both front and rear face are parallel but the tongue and tongue recess position the boards with the upper edge touching the studs and the lower edge spaced away from the studs to permit air circulation. In still another form of the invention, the front and rear surfaces taper away from each other from top to bottom with plural tongues and tongue recesses which position the units with lower edges flatwise against the studs and the upper edges spaced away from the studs for air circulation. In this form the boards are reversible.
BRIEF DESCRIPTION OF THE DRAWING
FIG. 1 is an end elevation, in section, of the combined backer board and siding units of the invention
FIG. 2 is a view similar to FIG. 1 showing the nailing surface of the invention
FIG. 3 is a view similar to FIG. 1 showing a modification in which the front and rear surfaces are parallel
FIG. 4 is a view similar to FIG. 1 showing the tongue and tongue recess so located as to permit the use of boards of rectangular cross section.
FIG. 5 is a view similar to FIG. 1 of a modification in which there are plural tongues and tongue recesses and the front and rear surfaces are both tapered
FIG. 6 is a view similar to FIG. 5 of a reversible board, the sealing tongue being formed by an elongated flexible, resilient member and
FIG. 7 is a view similar to FIG. 3 of the preferred form of the invention in which standard width boards are provided with the tongue, groove, rib and air spaces of the invention.
DESCRIPTION OF THE PREFERRED EMBODIMENT
The one piece combined backer and siding board 20 of the invention includes the elongated body 21 of solid, heat insulative material such as wood 22 having a front face 23, a rear face 24, an upper edge 25 and a lower edge 26. In the embodiment of FIGS. 1 and 2, the rear face 24 is normal to the plane of the upper edge 25 and, when applied to stud 27, lies flatwise against the front face 28 of the stud in the conventional manner. The front face 23 of the board 20 is inclined from the vertical to taper outwardly and downwardly from upper edge 25 to lower edge 26.
Unlike relatively thin shingles, clapboards and novelty siding which must be nailed to backer boards, or plywood panels which in turn are nailed to studs, the boards 20 of this invention are about one and one quarter inches thick at the upper edge 25 and about one and one half inches thick at the lower edge 26 to provide sufficient rigidity and insulation between the conventionally sixteen inch spaced studs 27 to require no reinforcement.
The relatively thick upper edge 25 includes a sealing groove 29 of curved cross section and predetermined dimensions which extends longitudinally along the central portion thereof and which is flanked on each opposite side by the rear, integral upstanding rib 31 and the front, integral upstanding rib 32. As shown in FIG. 1 the front rib 32 preferably includes an under cut longitudinally extending groove 33, which serves as a water check and toe nail groove. The angular cross section of groove 33 permits the upper angular surface 34 to block admission of water into the joint between boards while the lower angular surface 35, preferably at 45° to the vertical, provides a nailing surface which guides nails, driven normal thereto, below sealing groove 29, without entering the groove, and into a stud 27.
The relatively thick lower edge 26 of body 21 includes a downwardly depending, integral sealing tongue 36 of predetermined dimensions and curved cross section which extends longitudinally along the intermediate portion of the lower edge. The dimensions of each tongue 36 and tongue groove 29 are such that when a lower board 20 is nailed by a nail 37 to a stud 27 and the tongue of a next higher board 20 is inserted in the tongue groove there is sufficient clearance, or space, 38 at the rear of the groove 29 to receive a substantial amount of caulking compound 39, thereby filling the groove 29 and tightening the seal of the joint 41 between boards.
Each board 20 includes an integral, downward depending front rib 42, which extends longitudinally along lower edge 26, parallel to the tongue 36 and which preferably is of curved cross section as shown. If the rib 42 is considered to form a rabbett groove at the lower edge 26, then the sealing tongue 36 is central of the rabbett groove as shown. It will be seen that if, as proposed in the prior art, an upper tongue is seated in a lower tongue groove, and a lower outer rib is also provided, there is substantial waste of lumber whereas in this invention by tongue grooving the upper edge and forming the depending integral, sealing tongue alongside the depending integral front rib there is much less waste of material.
As shown in FIG. 1, in the lowermost board 20, nailed to stud 27, the upper edge 43 of a vinyl plastic covering 44 may be inserted in the space 45 behind the rib 42 and the lower portion 46 thereof may be pre-curved to fit around the curved surface 47 of rib 42 for nailing through holes 48 by nails 49.
In FIG. 2 another embodiment is illustrated in which the front rib 32 of each board 20 includes a beveled surface 51, corresponding to surface 35 and the rib 42 of each board 20 includes a rear face 52, uniformly spaced from the front face 23 to create a substantial air space 45.
In FIG. 3 still another embodiment is illustrated in which the board 54, corresponding to board 20, has the front face 55 parallel to the rear face 56 and the front face 55 is still inclined in the manner of shingles or clapboards by the positioning and structure of the tongue 57 and tongue groove 58. As shown, the tongue 57 extends along the lower edge 59 of the board parallel to the cover rib 61 but the rib 61 is of greater depth than tongue 57. This construction not only enables boards of rectangular cross section to be used but also spaces the lower edges 59 away from the studs 27 to give air access all around the board to prolong the useful life of certain wood.
In the embodiment of FIG. 4 a board 62 of rectangular cross section is also used, the tongue 63 in the lower edge 64 being equal in depth to the depth of the rib 65 and the rib 65 and front upper rib 66 having beveled nailing surfaces 67 and 68 respectively which form an air space 45.
In the embodiment of FIG. 5 the board 69 has a front face 71 and a rear face 72 which are both inclined and taper away from each other from upper edge 73 to lower edge 74. The cross section of board 69 is thus symetrical so that the board is reversible. A central tongue groove 75 is flanked by rear rib 76 and front rib 77 all of curved cross section in the upper edge 73. A central tongue 78 in the lower edge 74, seats in the tongue groove 75 of the next lowermost board, and is flanked by a lower rib 79 and a lower rear rib 81. A caulking space 38 for caulking compound 39 is provided in groove 75 and an air space 45 is provided under cover rib 77.
As shown in FIG. 6 a reversible board 82, corresponding to reversible board 69 of FIG. 5, is provided with a front, lower, cover rib 83, a central, lower groove 84, a rear, lower rib 85 and an upper edge tongue 86 which fits in the tongue groove 84 of the next higher board. An air space 87, corresponding to air space 45 is provided under cover rib 83 to ventilate the joint. In this embodiment, instead of an integral, depending, sealing tongue in the lower edge of each board, a resilient, compressible, element 88, which may be of O ring material and configuration, such as of rubber, is seated in a groove 89, to depend downwardly for also seating in a corresponding tongue groove 91 in the upper edge, or tongue 86, of the next lower board. The reversible boards 82 are affixed from bottom to top of vertical studs 92, by means of the shims 93 shown in dotted lines, for positioning the bottom board at the correct angle by screws or nails 94. The shims 93 are then removed and successive, upper boards are self-positioned, without shims, an elongated member 88 being placed in the grooves 89 and 91 for slight compression, to seal each joint.
In the preferred embodiment of FIG. 7, the combined backer board and siding 95 is formed from standard boarding of uniform thickness so that no special knives are required to taper one or both faces thereof. Each board 95 corresponds to board 54 of FIG. 3 except that the rear lower tongue 96, corresponding to rear lower tongue 57, is seated on a downward sloping surface 97 to permit run-off of any accumulation of moisture in the joint. Instead of a caulking space, caulking compound and integral depending sealing tongue in a tongue groove, the board 95 includes a sealing gasket 98, similar to element 88 of FIG. 6, the sealing gasket 98 being of resilient, flexible, compressible rubber or the like seated in a suitable gasket groove 99 in the tongue groove 84 in the board 95, and in a corresponding gasket groove 101 in the upper tongue 86 in the next lower board and being compressed for a firm, tight seal when one board 95 is affixed above another as illustrated in FIG. 7. An air space 102, similar to air space 45, is provided under cover tongue, or rib, 103 to ventilate the joint. The shim 104 forms the starter for the boards 95, nailed by nails or screws 94. The air space 105 is advantageous from an insulation point of view in the finished wall of a building. | A unitary combined backer and siding board is sufficiently thick and strong to eliminate the need for backer boards or plyscore as a substrate on the studs of the walls of a building. The board is standard, commercially available stock with parallel front and rear faces and of uniform thickness of about one and one quarter inches. The upper edge has a front, upstanding tongue of curved cross section which fits in a tongue groove of curved cross section in the lower edge. The upper edge is free of grooving and has a downward sloping surface between the upstanding tongue and the rear face to shed rainwater. A compressible sealing gasket is located between tongue and tongue groove. | 4 |
BACKGROUND OF THE INVENTION
The invention relates to an actuator, having a housing, a coil, an armature which interacts with a tappet and a spring, and of which the armature plate is arranged opposite an armature counterpiece, and wherein the actuator has at least one magnetostrictively acting component. The invention further relates to a method for operating an actuator of this kind.
An actuator of this kind is known from DE 198 43 534 A1. This actuator is installed on a fuel injector for an internal combustion engine. In this case, the magnetostrictive actuator is screwed to the side of the fuel injector and, by means of a hydraulic fluid, transmits a movement which is executed by the actuator to the valve needle of the fuel injector. To this end, a transmitter plunger is additionally arranged between the actuator and the space which accommodates the hydraulic liquid. Overall, the actuator, which is formed in this way and has the fuel injection valve, is of complicated construction, wherein the possible movement distance of the valve needle is furthermore small.
SUMMARY OF THE INVENTION
The object of the invention is to specify an actuator and a method for operating an actuator, with which actuator and method large actuating travel distances can be realized at high actuating forces.
This object is achieved in that the actuator is additionally designed as a solenoid. The method according to the invention is distinguished in that, when current is applied to the coil, a magnetic flux forms across the armature, the tappet, a sliding piece and the housing, the magnetostrictive tappet being extended by said magnetic flux, and, after a limit extension is reached, the attraction force between the armature plate and the armature counterpiece is large enough to move the armature, together with the tappet and the sliding piece, to bear against the armature counterpiece. In this case, the actuator additionally acts as a solenoid. The particular advantage of the invention therefore lies in the combination of a magnetostrictive actuator or magnetostrictively acting actuator with a solenoid, wherein the two actuator concepts share a magnetic circuit. Several advantages are achieved as a result. Only one coil is required, as a result of which the installation space requirement for the actuator is low overall. The number of components is likewise low. The magnetostrictive actuator has to cover only a small actuating travel distance, and therefore said magnetostrictive actuator can be of small design overall. Finally, the force profile of the actuator combination which is designed in this way can be better matched to corresponding requirements. Therefore, in summary, an actuator is provided which is able to realize large actuating travel distances at high actuating forces together with a clear structure and low costs.
In one development of the invention, the tappet is of magnetostrictive design. Magnetostriction is the deformation of magnetic (in particular ferromagnetic) substances as a result of a magnetic field being applied. In the process, the body, in the present case the tappet, experiences an elastic change in length at a constant volume. Suitable materials for the tappet include materials with a high degree of magnetostriction, for example Terfenol or iron/nickel alloys.
In a further refinement of the invention, the tappet is arranged between the armature and, on the opposite side, a sliding piece. When current is applied to the coil, the tappet extends and displaces the armature ultimately as far as a limit extension amount in relation to the sliding piece which is supported in a manner fixed to the housing.
In one development of the invention, the armature and the sliding piece are connected to one another by means of a spring which surrounds the tappet. The spring applies the necessary pretension to the tappet. In a further refinement, the spring is in this case designed as a sleeve spring which is additionally a tension spring. The sleeve spring is fixedly connected to the armature and to the sliding piece and clamps the tappet between said components with a defined force.
In one development of the invention, the sliding piece is of cylindrical design and is guided in a recess in the housing. Firstly, this results in the assembly, comprising the sliding piece, the tappet, the armature and the sleeve spring, being guided, and secondly, a low-loss magnetic flux is ensured by the guidance.
In one development of the invention, the coil is arranged in the housing so as to surround at least the tappet and the spring. In the process, the coil can further also surround a subregion in each case of the armature and of the sliding piece in order to exert a force, which is as constant as possible, on the components even during the intended movements of the components.
In one development of the invention, the armature interacts with a coupler rod opposite the tappet. In the process, the coupler rod is preferably connected to the armature plate and guided through an opening in the armature counterpiece. In the process, the coupler rod transmits the corresponding movement to the components which are to be moved, and, furthermore, the movable components are guided on the opposite side to the sliding piece. In one development of the invention, the component which is to be operated is a fuel injector of an injection system for an internal combustion engine. In this case, the actuator which is designed in this way is advantageously to be integrated into the housing of a fuel injector of this kind.
BRIEF DESCRIPTION OF THE DRAWINGS
Further advantageous refinements of the invention can be found in the description of the drawings in which one exemplary embodiment of the invention which is illustrated in the drawing is described in greater detail.
In the drawings:
FIG. 1 shows a force/distance graph of various force profiles of actuators and a force profile which is necessary for moving a valve needle, and
FIG. 2 shows an actuator which is designed according to the invention and is installed on a fuel injection valve.
DETAILED DESCRIPTION
FIG. 1 shows a force/distance graph with various force profiles or stroke profiles of different actuators and a typical hydraulic force profile which has to be exerted on a valve needle of a fuel injector in order to move said valve needle.
In the graph, the needle stroke Nh (or actuating travel distance) of a valve needle, which needle stroke corresponds to an air gap, which is to be overcome, in a (magnetic) actuator, is plotted on the abscissa, and the force K is plotted on the ordinate. The characteristic curve a indicates the typical force profile of a magnetostrictive actuator which, starting from a high initial force and a then linearly decreasing force, covers only a small overall actuating travel distance. The characteristic curve b indicates the typical force profile of a magnetic lifting actuator (solenoid) which, starting from a low initial force, exhibits an increasing increase in force with a large overall actuating travel distance. The characteristic curve c identifies a typical hydraulic force profile which has to be exerted on the valve needle 6 , illustrated in FIG. 2 , of a fuel injector 5 in order to move said valve needle. In the event of a combination of the two actuators having the characteristic curves a and b, a changeover point d from a magnetostrictive actuator to a solenoid is produced at the point at which the characteristic curves c and b intersect. It is further clear that the combination according to the invention of a magnetostrictive actuator and a solenoid always generates a force which is considerably higher than the force which is necessary for moving the valve needle 6 .
In the illustrated exemplary embodiment, the actuator 1 , illustrated in FIG. 2 , is connected to a fuel injector 5 , but, in principle, can also be connected to any other desired devices or components in which an associated component is intended to be moved. The fuel injector 5 is part of a common rail injection system with which fuel, in particular diesel fuel, is intended to be injected into an associated combustion space of a preferably self-igniting internal combustion engine under high pressure.
To this end, fuel is supplied to the fuel injector 5 via a high-pressure line which is arranged by way of a high-pressure line connection 7 on a common housing 8 of the actuator 1 and of the fuel injector 5 . The high-pressure line connection 7 is connected to a valve needle space 10 and a control space 11 via connecting channels 9 , 9 a , 9 b . In the illustrated position of the valve needle 6 , injection openings 12 through which the fuel, which is located in the valve needle space 10 , can be injected into the combustion space are closed by a valve needle tip of the valve needle 6 . The injection openings 12 are arranged in a valve needle body 13 which interacts with a valve body 14 . For its part, the valve body 14 interacts with an intermediate piece 15 which adjoins an armature counterpiece 16 . The intermediate piece 15 and the armature counterpiece 16 are inserted into the housing 8 and the armature counterpiece 16 is supported on a projection 17 in the housing 8 . Said components are braced to one another by a union nut 18 , wherein the union nut 18 is supported by way of a ring projection 19 on the valve needle body 13 and is screwed onto the housing 8 by way of the opposite end region.
The valve needle 6 is pushed into the position in which it closes the injection openings 12 by a valve needle spring 20 which is arranged in the region of the control space 11 and is supported on the valve needle 6 and the intermediate piece 15 . At the same time, an additional closing force to that provided by the valve needle spring 20 is exerted on the valve needle 6 by the high fuel pressure prevailing in the control space 11 and the valve needle space 10 , supported by a step projection 25 on the valve needle 6 .
The injection openings 12 which are controlled by the valve needle 6 are opened when the valve needle 6 is moved in the direction of the intermediate piece 15 . A movement of this kind is executed when a coupler rod 22 which is guided through an opening in the armature counterpiece 16 is moved by the actuator 1 in the direction of the control space 11 and fluid, in particular fuel, which is located in an actuator space 22 is conveyed to a valve needle control space 24 by a connection 23 . The valve needle control space 24 is arranged opposite the control space 11 on the step projection 25 of the valve needle 6 and, when the pressure in the valve needle control space 24 is high enough, the valve needle 6 is pushed in the direction of the intermediate piece 15 against the force of the valve needle spring 20 and the fuel pressure prevailing in the control space 11 . The injection operation which is initiated in this way is terminated by the fluid pressure in the valve needle control space 24 being lowered and the force which is exerted by the valve needle spring 20 and the fuel pressure in the control space 11 being greater than the forces prevailing in the valve needle control space 24 and the valve needle space 10 . This state is produced by corresponding driving and, respectively, disconnection of the actuator 1 .
The coupler rod 21 is pushed against the armature plate 3 by a coupler rod spring 26 and can be guided, for example, in a recess in the armature plate 3 in order to fix the armature plate 3 in position.
The actuator 1 has a space 28 which is made in the housing 8 and which accommodates the components of the actuator 1 . In particular, a coil 29 is arranged and secured in a suitable manner in the space 28 . The coil 29 is connected in a switchable manner to a voltage source via connection lines. Within the coil 29 , a tappet 30 which is produced from a magnetostrictive material is arranged between the armature 2 and an opposite sliding piece 31 . The armature 2 is connected to a sleeve spring 32 by way of the sliding piece 31 with the inclusion of the tappet 30 , said sleeve spring exerting a required pretension on the tappet 30 . The sliding piece 31 is guided in a movable manner in a recess 33 in the housing 8 . This guidance of the sliding piece 31 in the recess 33 produces an at least low-loss magnetic circuit, comprising the armature counterpiece 16 , the armature 2 , the magnetostrictive tappet 30 , the sliding piece 31 and the housing 8 , when current is applied to the coil 29 . At the same time, the guidance of the sliding piece 31 in the recess 33 causes guidance of the tappet 30 together with the armature 2 .
If current is applied to the coil 29 , a magnetic flux initially forms across the tappet 30 , the armature 2 , the housing 8 and the sliding piece 31 . This flux generates an attraction force between the armature 2 and the armature counterpiece 16 , but this attraction force is not large enough to ultimately lift the valve needle 6 from the seat in order to open the injection openings 12 . The magnetostrictive tappet 30 wants to extend owing to the generated magnetic field. This extension is impeded by the force which acts on the valve needle 6 by means of the valve needle control space 24 and the actuator control space 22 and the coupler rod 21 on the armature 2 . This leads to a pressure force in the magnetostrictive tappet 30 . The tappet 30 will be extended until an equilibrium is established between the pressure force in the tappet 30 and the force on the coupler rod 21 . This results in a reduction in volume in the actuator control space 22 , wherein the displaced fluid is pushed into the valve needle control space 24 through the connection 23 . As a result, the valve needle 6 is lifted out of the seat. When the valve needle 6 has completed a sufficient stroke, the attraction force between the armature 2 and the armature counterpiece 16 is large enough to move the components armature 2 , tappet 30 , sliding piece 31 and sleeve spring 32 . In this state, the actuator 1 (additionally) acts as a solenoid. This movement is converted by the actuator control space 22 and the valve needle control space 24 into a further movement of the valve needle 6 . Force can be decreased or increased by means of the area ratios in the actuator control space 22 and the valve needle control space 24 . The injection operation which is initiated in this way is terminated by current not being applied to the coil 29 , and accordingly the armature 2 together with the tappet 30 and the sliding piece 31 being moved back to the illustrated starting position. As a result, the pressure in the valve needle control space 24 is reduced and the valve needle 6 is moved back to the position in which it closes the injection openings 12 . | The invention relates to an actuator ( 1 ) comprising a housing ( 8 ), a coil ( 29 ) and an armature ( 2 ) which interacts with a tappet ( 30 ) and a spring, the armature plate ( 3 ) thereof being arranged to lie opposite an armature counterpiece ( 16 ), and said actuator ( 1 ) comprising at least one magnetostrictively-active component. According to the invention, an actuator ( 1 ) is provided with which large actuating paths can be travelled at high actuating forces. This is achieved by the actuator ( 1 ) additionally being designed to act as a solenoid. | 5 |
GOVERNMENT RIGHTS
[0001] This invention was made with Government support under Contract No. F49620-92-J-05 24 (Princeton University), awarded by the U.S. Air Force OSR (Office of Scientific Research). The Government has certain rights in this invention.
FIELD OF THE INVENTION
[0002] The present invention relates to the fabrication of optical quality thin films, and more particularly to the low pressure fabrication of such thin films for application in non-linear optical devices and organic light emitting devices.
BACKGROUND OF THE INVENTION
[0003] The field of organic electroluminescence is a rapidly growing technology. Spurred by potential application to displays, organic light emitting devices (OLEDs) are capable of achieving external quantum efficiencies of over 3%, and operational lifetimes on the order of 10,000 hours at video brightness. Both small molecule and polymer-based OLEDs are known, but polymer-based devices have a general advantage of simple and inexpensive fabrication by spin-on deposition techniques. In contrast, small molecule devices are usually fabricated by thermal evaporation in vacuum, which is usually a more expensive process than spin-on deposition. Examples of OLED structures and processing techniques are provided in published PCT application WO 96/19792, incorporated herein by reference.
[0004] The use of organic vapor phase deposition (OVPD) has made progress towards the low cost, large scale deposition of small molecular weight organic layers with numerous potential photonic device applications such as displays. The OVPD process is described in U.S. Pat. No. 5,554,220 to Forrest et al.; S. R. Forrest et al., “Intense Second Harmonic Generation and Long-Range Structural Ordering in Thin Films of an Organic Salt Grown by Organic Vapor Phase Deposition,” 68 Appl. Phys. Lett. 1326 (1996); and P. E. Burrows et al., “Organic Vapor Phase Deposition: a New Method for the Growth of Organic Thin Films with Large Optical Non-linearities,” 156 J. of Crystal Growth 91 (1995), each of which is incorporated herein by reference.
[0005] The OVPD process uses carrier gases to transport source materials to a substrate, where the gases condense to form a desired thin film. The OVPD technique has been used, for example, to deposit films of the optically non-linear organic (NLO) salt, 4′-dimethylamino-N-methyl-4-stilbazolium tosylate (DAST), from volatile precursors 4′-dimethylamino-N-methyl-4-stilbazolium iodide (DASI) and methyl p-toluensulfonate (methyltosylate, MT), which are transported by carrier gases to a heated substrate. In this process, DASI thermally decomposes to form 4-dimethylamino-4-stilbazole (DAS), which subsequently reacts with MT to form DAST on the substrate.
[0006] Because of its capability for controlled co-deposition of materials with radically different vapor pressures, OVPD is believed to be the only method for the precise stoichiometric growth of multi-component thin films. However, the OPVD process is conducted at atmospheric pressure, and films grown at or near atmospheric pressure are often rough and have non-uniform surface morphologies due to gas phase nucleation and a diffusion-limited growth process.
SUMMARY OF THE INVENTION
[0007] The present invention makes use of low pressure deposition techniques to produce organic thin films having superior surface properties. In one aspect, the present invention comprises a method for preparing an organic thin film on a substrate, the method comprising the steps of providing a plurality of organic precursors, the organic precursors being in the vapor phase; and reacting the plurality of organic precursors at a sub-atmospheric pressure in the presence of the substrate to form a thin film on the substrate. In another aspect, the present invention includes organic films made by such a method. In yet another aspect, the present invention includes an apparatus designed to facilitate the reaction of organic precursors at sub-atmospheric pressures to form an organic film on a substrate.
[0008] One advantage of the present invention is that it provides multi-component organic thin films wherein the amount of each component in such films can be controlled accurately and precisely.
[0009] Another advantage of the present invention is that it provides uniform organic thin films having smooth surfaces.
[0010] Another advantage of the invention is that it provides a low pressure organic vapor phase deposition method and apparatus for the growth of thin films of organic light emitting materials and optically non-linear organic salts.
[0011] Another advantage of the invention is that it provides a low pressure organic molecular beam deposition method and apparatus for the formation of thin films of organic light emitting materials and optically non-linear organic salts.
[0012] Yet another advantage of the invention is that it provides a method and apparatus for the uniform deposition of organic materials over large substrate areas.
BRIEF DESCRIPTION OF THE DRAWINGS
[0013] [0013]FIG. 1 shows a LPOVPD reactor, in accordance with an embodiment of the present invention.
[0014] [0014]FIG. 2 shows an OMVD reactor, in accordance with an embodiment of the present invention.
[0015] [0015]FIG. 3 shows an apparatus for the continuous low pressure deposition of organic materials onto substrates, in accordance with an embodiment of the present invention.
[0016] [0016]FIGS. 4A and 4B are planar and cross-sectional views, respectively, of a reactant gas distributor, in accordance with an embodiment of the present invention.
[0017] [0017]FIG. 5 is a side view of a roll-to-roll substrate delivery mechanism, in accordance with an embodiment of the present invention.
DETAILED DESCRIPTION
[0018] The present invention provides a method and apparatus for the growth of organic thin films on substrates while under sub-atmospheric pressures. The method of the invention is herein identified as low pressure organic vapor deposition (LPOVPD). The LPOVPD method of the present invention allows for the accurate and precise control of the deposition of multi-component organic thin films. In addition, the thin films of the present invention are characterized by superior surface properties such as low surface roughnesses.
[0019] A LPOVPD reactor 10 in accordance with an embodiment of the present invention is schematically shown in FIG. 1. Reactor 10 includes a reaction chamber, such as a reactor tube 12 , and tubing extending into the reaction chamber. Reactor tube 12 is a cylinder having a suitable dimension such as, for example, a diameter of 10 cm and an approximate length of 45 cm in an experimental apparatus. Reactor tube 12 is made of any suitable material such as glass or quartz. An open container such as crucible 14 contains a first organic precursor material and is placed within tube 36 near one end 20 of the reactor tube 12 . Alternatively, crucible 14 is placed directly on the reactor tube 12 or on shelves or tubes therein. Crucible 14 is heated or cooled by means of a multi-zone heater/cooler 18 , which substantially surrounds reactor tube 12 . The temperature control of crucible 14 results in the thermal decomposition or volatilization of the first organic precursor material within crucible 14 . A regulated stream 30 of inert carrier gas is passed through tube 36 and into the reaction chamber, thus causing vapor of the first organic precursor to flow along the reactor tube 12 toward its exhaust end 22 . The inert carrier gas is an inert gas such as nitrogen, helium, argon, krypton, xenon, neon and the like. Gases with a reducing character, such as hydrogen, ammonia and methane, are also inert for many organic materials. Use of these reducing gases often has the additional benefit of assisting in the burning of undesired excess reactants.
[0020] Inert gas is delivered from tank 24 through a regulator valve 26 and into tubing 28 for delivery through at least two flow paths, 30 and 38 , and into reactor tube 12 . One flow path 30 includes a series connected pressure regulator 32 , flow meter 34 and quick switching valve 35 from which the carrier gas is delivered into end 20 of reactor tube 12 . The second flow path 38 includes a series connected pressure regulator 40 , flow meter 42 and quick switching valve 39 from which the carrier gas flows into a bubbler 46 , which contains a second organic precursor material 48 . To facilitate the temperature control of second organic precursor material 48 , bubbler 46 is partially immersed in bath 50 within container 52 . Inert gas from tank 24 bubbles through the second organic precursor 48 and through tubing 54 to carry vapor of the second organic precursor 48 into reactor tube 12 . During this process, tube 54 must be maintained at a sufficiently high temperature to avoid recondensation of the volatilized second organic precursor 48 as it travels from the bubbler to the reactor.
[0021] The amount of any precursor entering reactor tube 12 is controlled by processing parameters such as the temperature and flow rate of the carrier gas and the temperature of the reactants. The LPOVPD method provides precise metering of the precursors or reactants independently of their vapor pressure or chemical nature using pressure mass flow controllers. The present method thus permits the combination of materials with widely different characteristics in ratios necessary for the production of desired films.
[0022] The precursor streams are capable of being turned on and off almost instantly by employing quick switching valves 35 and 39 . These valves direct the precursor streams into reactor 12 or into a by-pass line (not shown) so that at any given time, different precursor streams may be entering the reactor 12 for the deposition of films of different compositions and characteristics. Valve 39 also regulates the admittance of carrier gas into bubbler 46 . Valves 35 and 39 thus allow the rapid change of reactant streams entering the reactor 12 , for changing the nature and the composition of the grown films. It is thus possible, for example, to grow ABAB, ABCABC, ABABCAB, and ABCDABCD-type films, where each letter denotes a different molecular layer or composition.
[0023] A vacuum pump 66 and control throttle valve 68 are attached to reactor 10 at the exhaust 62 . Most of the organic vapors not deposited onto substrate 58 are condensed in a trap 64 placed upstream from pump 66 . Trap 64 contains liquid nitrogen or a neutral, fluorocarbon oil, for example. Throttle valve 68 regulates the pressure in reactor 10 . An appropriate pressure gauge is connected to the reactor (not shown) with electronic feedback to the control throttle valve 68 to maintain a desired pressure in the reactor.
[0024] Vacuum pump 66 provides a pressure of about 0.001-100 Torr in reactor tube 12 . The actual pressure for any combination of acceptor, donor, and single component layers is experimentally determined with reference to the temperatures required to volatilize the precursor materials, the wall temperature to prevent condensation of the precursor materials, and the reaction zone temperature gradient. The optimal choice of pressure is unique to the requirements of each deposited organic layer. For example, optimal pressures for the deposition of single component layers such as tris-(8-hydroxyquinoline) aluminum (Alq 3 ) or N-N′-diphenyl-N,N-bis(3-methylphenyl) 1,1′-biphenyl-4,4′diamine (TPD) are about 0.1-10 Torr.
[0025] The substrates on which the thin films of the present invention are deposited are typically selected from those materials that are commonly encountered in semiconductor and optics manufacturing. Such materials include, for example, glass, quartz, silicon, gallium arsenide and other III-V semiconductors, aluminum, gold and other precious and non-precious metals, polymer films, silicon dioxide and silicon nitride, indium-tin-oxide and the like. For high quality optical thin films, it is preferable to use substrates that provide crystalline interactions with the deposited organic film to induce epitaxial growth. To achieve such epitaxial growth, it is often necessary to coat substrates with non-polar organics having crystalline structures similar to the film to be deposited.
[0026] In addition, as an organic thin film is deposited onto substrate 58 , it is often desirable to control the temperature of the substrate. Independent control of substrate temperature is accomplished, for example, by contacting substrate 58 with temperature-control block 60 , which has channels therein for the circulation of materials such as water, gas, freon glycerin, liquid nitrogen, and the like. It can also be heated by the use of resistance or radiant heaters positioned on or near the block 60 .
[0027] Reactor 20 of FIG. 1 is expandable to include multiple bubblers 46 N to feed additional precursors into reactor 20 . Similarly, multiple carrier gas flow paths 30 N are used to deliver yet additional precursors from crucibles 14 N. As an alternative, crucibles 14 , 14 N are vertically stackable on shelves or in tubes within reactor tube 12 for processing the additional precursors. Depending on the organic film to be deposited, one or more flow paths 30 , 38 are used alone or in any combination to provide the necessary precursor materials.
[0028] The method of the present invention is used to deposit a wide variety of organic thin films from the reaction of vapor precursors. As used herein, “reaction” refers to a chemical reaction in which precursor reactants form a distinct reaction product, or alternatively, it merely refers to a combination or mixture of precursor materials, or where precursor materials form a donor-acceptor or quest-host relationship. For example, in accordance with the present invention, the following NLO materials are formed as thin films by the reaction of the listed precursors:
Film Material First Precursor Second Precursor 4′-dimethylamino-N- 4′-dimethylamino-4- methyl tosylate (MT) methyl-4-stilbazolium stilbazole (DAS) tosylate (DAST) 4′-dimethylamino-4- methyl 4′-dimethylamino-4- methylstilbazolium methanesulfonate stilbazole (DAS) methanesulfonate (MM) (DASM) 4′-dimethylamino-4- methyl 4′-dimethylamino-4- methyistilbazolium trifluoromethane- stilbazole (DAS) trifluoromethanesulfonate sulfonate (M f M) (DASM f ) 4′-dimethylamino-N- methyl tosylate 4′-dimethylamino-4- methyl-4-stilbazolium (MT) methylstilbazolium tosylate (DAST) thiophenoxide (DASTh) 4′-methoxy-4- methyl tosylate 4′-methoxy-4- methylstilbazolium (MT) methylstilbazole tosylate (MeOST) (MeOS) 4′-dimethylamino-N- methyl tosylate 4′-dimethylamino-4- methyl-4-stilbazolium (MT) ethylstilbazolium tosylate (DAST) iodide (DAS(Et)I) 4′-dimethylamino-N- methyl tosylate 4′-dimethylamino-4- methyl-4-stilbazolium (MT) ethylstilbazolium tosylate (DAST) hydroxide (DAS(Et)OH) 4′-dimethylamino-4- acetyl 4′-dimethylamino-4- acetylstilbazolium toluenesulfonate stilbazole (DAS) tosylate (DAAST) (AT) 4′dimethylamino-4- methyl 4′-dimethylamino-4- methylstilbazolium trifluoroacetate stilbazole (DAS) trifluoroacetate (MA f ) (DASA f )
[0029] In another example relating more specifically to light emitting materials used to make OLEDs, the precursors consist of, for example, tetrathisferlvalene (TFF) and 7,7,8,8-tetracyanoquinodimethane (TCNQ). The mixing step results in the charge transfer complex TTF-TCNQ which deposits onto a substrate. In another example relating to OLEDs, 4-(dicyanomethylene)-2-methyl-6-(p-dimethylaminostyryl)-4H-pyran (DCM) is added into a high flow rate carrier gas stream while Alq 3 is added into a lower flow rate carrier gas stream. These streams are then mixed in a central reactor tube, thus providing the desired dilution of the guest molecule in the host matrix film to form a single luminescent layer. Other guest molecule examples in Alq 3 hosts are 5,10,15,20-tetraphenyl-21H,23H-porphine (TPP), Rubrene, DCM2, Coumarin, etc. As a variation, multiple dopants can be added into a single host to achieve efficient broad color conversion.
[0030] In another example, a bilayer light emitting device consisting of a hole transporting layer (“HTL”) such as TPD; α-4,4′-bis[N-(1-naphthyl)-N-Phenyl-amino]biphenyl (α-NPD); or MTDATA, layered onto the surface of a light emitting layer (“EL”) such as Alq 3 , bis- (8-hydroxyquinoline)aluminum oxyphenyl ((Alq 2 )′-OPh) or doped combinations of these layers, is grown by sequentially growing the HTL and EL to desired thicknesses. This is followed by growing additional layers onto the organics, or by growth on metallic contact layers using organometallic sources such as trimethyl-indium, trimethyl-gallium, and the like.
[0031] In addition to the apparatus and method described with reference to FIG. 1, the present invention includes a low pressure reactor 70 and method as shown in FIG. 2. Reactor 70 includes a modified ultra-high vacuum chamber 71 and a vacuum pump such as a turbomolecular pump (not shown) connected to valve 72 . Typical chamber base pressures in chamber 71 are 10 −8 -10 −11 Torr. The process of depositing organic layers with the use of reactor 70 is called organic molecular beam vapor deposition (OMVD). Although both LPOVPD and OMVD make use of sub-atmospheric pressures for the deposition of organic layers, the principle difference between these processes is that in the latter, the molecular mean free path is comparable to or larger than the dimensions of the chamber 70 . In comparison, the mean free path in LPOVPD is significantly shorter than the gas reactor dimensions. OMVD thus allows for the formation of highly directed molecular “beams” from the injectors to the substrate, allowing for precise kinetic control of the grown film thickness, purity and morphology.
[0032] Bubbler 74 is included for containing a first precursor material 75 . The bubbler 74 is placed into container 76 and immersed in a temperature controlled bath 80 . A high purity inert carrier gas 78 bubbles through first precursor 75 , and carries respective vapors through heated tubing 79 and into vacuum chamber 71 by way of injector 82 . Once inside chamber 71 , the precursor vapors form a molecular beam 83 that impinges on substrate 85 . Substrate 85 is provided with a means for providing temperature control such as coolant port 81 , for example.
[0033] Vacuum chamber 71 optionally is provided with at least one Knudsen or K-cell 86 , which contains a second precursor material 88 . K-cell 86 is a uniformly heated and controlled oven for the effusion of evaporants under vacuum. For example, K-cell 86 is heated to crack DASI or other precursor and sublime the resulting DAS, such that it is injected into reactor 70 as a molecular beam 89 . Alternatively, K-cell 86 simply sublimes a single component substance such as Alq 3 . Alternatively, K-cell 86 is fitted with a carrier gas inlet used to dilute the concentration of the molecular species being sublimed or evaporated into the gas stream by thermalization. This dilution process is particularly useful in achieving precise doping levels of guest-host systems such as DCM-Alq 3 by controlling the temperatures of bath 80 and Knudsen cell 86 as well as the flow of carrier gas 78 to bubbler 74 .
[0034] Molecular beams 83 and 89 impinge on substrate 85 to deposit an organic thin film, the thickness of which is monitored by quartz crystal 93 . Sample holder 90 rotates to ensure a uniform deposition and reaction of precursor materials. The deposition of precursor materials is further controlled by shutters 87 , which are used to interrupt molecular beams 83 and 89 .
[0035] Reactor 70 also optionally includes a cooled shroud 91 to help keep the pressure of vacuum chamber 71 to a minimum for re-evaporated precursor materials. Also preferably included is a partition 92 to keep precursor materials from migrating and thus contaminating each other.
[0036] Reactor 70 is embellished with many of the same attributes of the LPOVPD reactor shown in FIG. 1, such as quick switching valves, bypass lines and the like. Reactor 70 is able to be fitted with multiple Knudsen cells and bubblers for the deposition of multiple precursor materials onto substrate 85 . Reactor 70 also preferably includes a “load-lock” 94 for sample introduction. Load-lock 94 includes door 95 and vacuum pump 96 , and provides for the exchange of samples without compromising the pressure of chamber 71 .
[0037] The apparatus of FIG. 1 is optionally modified for the continuous deposition of organic layers on large area substrates, as shown by the example illustrated in FIG. 3. The apparatus of FIG. 3 includes a plurality of vacuum chambers such as loading chamber 146 , organic layer deposition chambers 150 and 152 , contact deposition chamber 154 , and unload chamber 156 . As an example, each deposition chamber is a LPOVPD reactor 10 of FIG. 1. The substrates 137 are transported on a conveyor belt 148 through each of chambers 150 , 152 , 154 and 156 . In the embodiment shown in FIG. 3, chambers 150 , 152 and 154 include sources 158 , 160 and 162 , respectively, of radiant heat to prevent the condensation of organic vapors. Although only two organic layer deposition chambers 150 and 152 are shown in FIG. 3, additional chambers are included as desired. In passing from the loading chamber 146 to the organic layer deposition chambers 150 and 152 , and from the contact deposition chamber 154 to the unload chamber 156 , the substrate 137 passes through air locks (not shown) so as not to compromise the vacuum in the chambers 150 , 152 , and 154 . As an example relating to OLEDs, chambers 150 and 152 are used for the deposition of TPD and Alq 3 , respectively, and chamber 154 is used for the deposition of an Mg:Ag contact layer.
[0038] Each of the chambers 150 , 152 , and 154 in the example of FIG. 3 includes a reactant gas distributor (RGD) 108 for the deposition of organic precursor materials, as shown in detail in FIGS. 4A and 4B. RGD's 108 are used as an alternative to the organic precursor delivery mechanisms of FIGS. 1 and 2, and are used to provide gas curtains, 120 , 120 ′, 120 ″ and 120 ″′. RGD 108 ensures that where multiple organic precursors are deposited, the precursors remain separated until deposited on a substrate, whereupon reaction of the precursors is permitted to take place. RGD 108 includes heater 122 , second carrier gas inlet 112 and gas manifold 132 . Heater 122 prevents the premature condensation of organic precursor materials. Over RGD 108 is a first carrier gas inlet 114 and distributor plate 110 . First carrier gas inlet 114 supplies gas which usually carries a first organic precursor of generally low volatility such as, for example, MT. The first carrier gas enters a reaction chamber though distributor plate 110 , which is a wire mesh, a glass filter material, or a porous stainless steel plate, for example. The column of carrier gas flowing through distributor plate 110 is shadowed by the RGD 108 . RGD 108 provides a planar gas curtain 120 of a second organic precursor of generally low vapor pressure such as, for example, DAS. A second carrier gas containing a second organic precursor enters at inlet 112 and is directed into gas manifold 132 . Manifold 132 is a hollow tube having a line of holes 134 for feeding the second carrier has into an annular cavity 126 , which surrounds manifold 132 . Second carrier gas exits RGD 108 through slit 136 , thus giving it the shape of a planar curtain.
[0039] As an example, curtain 120 is comprised of TPD vapors, curtain 120 ′ is comprised of Alq 3 vapors and curtain 120 ″ is comprised of vapors such as a polypyrole or metallorganic compounds that produce a conductive surface. If desired, control or tuning of the color of light emitted by an OLED can be effected by suitable doping of the Alq 3 layer with an additional RGD device 108 in the chamber 152 that produces a curtain 120 ″′ of dopant vapor.
[0040] The apparatus of FIG. 1, FIG. 2 or FIG. 3 is optionally modified by using a “roll-to-roll” substrate delivery system, as shown in FIG. 5. The delivery system shown in FIG. 5 is suitable for the deposition of organic thin films onto large area, flexible substrates. Substrate 180 is made of a polymer sheet or metal foil, for example, and is delivered from roll 181 to roll 182 . The deposition of organic precursors onto substrate 180 occurs when substrate 180 is unrolled from roll 181 and is therefore exposed to the reaction chamber of FIG. 1, or when exposed to the molecular beam or curtains of FIGS. 2 and 3, respectively. Rolls 181 and 182 are driven by any suitable means, such as a variable speed motor. The speed at which substrate 180 is passed from roll 181 to roll 182 dictates the thickness of the organic film that forms on substrate 180 .
[0041] The present invention is further described with reference to the following non-limiting examples.
EXAMPLE 1
[0042] Using the apparatus of FIG. 1, layers of organic light emitting materials were grown using glass and flexible polyester substrates precoated with transparent layers of indium tin oxide (ITO). The ITO forms the anode of the device with a thickness of 1700 Å and 1200 Å for the glass and polyester substrates, respectively, yielding anode resistances of 10 Ω and 60 Ω, respectively. Glass substrates were cleaned by rinsing in a solution of detergent and deionized water in an ultrasonic bath, and then boiling in 1,1,1-trichloroethane, rinsing in acetone and finally rinsing in 2-propanol. To avoid damage due to exposure to organic solvents, the flexible substrates were cleaned by rinsing only in the detergent and 2-propanol solutions.
[0043] Glass substrates were placed within the reactor tube 12 at a location where the temperature was approximately 220° C. The first layer deposited on the ITO surface was TPD, a hole transporting material. Specifically, TPD vapor was carried from crucible 14 to substrate 28 via nitrogen carrier gas. The TPD growth conditions included a source temperature of 200±5° C., a nitrogen carrier gas flow rate of 100 sccm, a reactor pressure of 0.50 Torr and a growth time of 20 minutes. At a nitrogen flow rate of 100 sccm, the Reynolds number of the system was ˜500, indicating operation well within the laminar flow regime. The TPD layer was grown to a thickness of between 100-300 Å.
[0044] After deposition, the temperature near the TPD crucible was reduced, and the corresponding nitrogen flow was shut off. Next, an electron transporting layer of Alq 3 was grown by turning on a separate nitrogen line to carry Alq 3 vapor from crucible 14 N into chamber 12 . The Alq 3 growth conditions included a source temperature of 247±8° C., a nitrogen flow rate of 50 sccm, a pressure of 0.65 Torr and a growth time of 10 minutes. During the deposition of both the TDP and Alq 3 , the substrate was maintained at 15° C. using a water cooled stainless steel substrate holder. The TPD layer was grown to a thickness of between 700-1100 Å.
[0045] After deposition of the Alq 3 layer, the substrate was removed from the reactor and a Mg:Ag top contact was applied by thermal evaporation. The contact was completed with the evaporation of a 1000 Å thick protective Ag layer.
[0046] The use of low pressures during deposition resulted in organic layers having smooth and uniform surfaces. For example, the TPD and Alq 3 layers were measured via atomic force microscopy to have RMS roughnesses of 6-8 Å and 9-11 Å, respectively. The resulting OLED devices exhibited current-voltage characteristics wherein IαV at low voltages and IαV 9 at higher voltages. The turn-on voltage, V T , at which the power law dependence of I on V changed, was about 6V.
EXAMPLE 2
[0047] An NLO film was prepared using the apparatus shown in FIG. 1. MT 48 was loaded into a 30 cm 3 bubbler 46 , the temperature of which was maintained at approximately 80°-100° C. by silicone oil bath 50 . Nitrogen gas was used to bubble through the MT 48 , thereby carrying MT vapor through glass tube 54 and into reactor tube 12 at a location approximately 5 cm beyond crucible 14 , which contained was placed on the floor of reactor tube 12 and DASI. The pressure within reactor tube 12 was maintained at about 10 −2 torr. DAS vapor reacted with the MT vapor to form a solid film of DAST on substrates 58 , which were supported on substrate block 60 . Excess unreacted MT vapor and any volatile side-reaction products were exhausted from exhaust tube 62 . DAST films thus formed are useful as optical switches, for example.
[0048] The present invention makes use of low pressure deposition techniques to produce organic thin films having superior surface properties and accurate and precise compositions. Although various embodiments of the invention are shown and described herein, they are not meant to be limiting. For example, those of skill in the art may recognize certain modifications to these embodiments, which modifications are meant to be covered by the spirit and scope of the appended claims.
[0049] The subject invention as disclosed herein may be used in conjunction with co-pending applications: “High Reliability, High Efficiency, Integratable Organic Light Emitting Devices and Methods of Producing Same”, Ser. No. 08/774,119 (filed Dec. 23, 1996); “Novel Materials for Multicolor LED's”, Ser. No. 08/850,264 (filed May 2, 1997); “Electron Transporting and Light Emitting Layers Based on Organic Free Radicals”, Ser. No. 08/774,120 (filed Dec. 23, 1996); “Multicolor Display Devices”, Ser. No. 08/772,333 (filed Dec. 23, 1996); “Red-Emitting Organic Light Emitting Devices (LED's)”, Ser. No. 08/774,087 (filed Dec. 23, 1996); “Driving Circuit For Stacked Organic Light Emitting Devices”, Ser. No. 08/792,050 (filed Feb. 3, 1997); “High Efficiency Organic Light Emitting Device Structures”, Ser. No. 08/772,332 (filed Dec. 23, 1996); “Vacuum Deposited, Non-Polymeric Flexible Organic Light Emitting Devices”, Ser. No. 08/789,319 (filed Jan. 23, 1997); “Displays Having Mesa Pixel Configuration”, Ser. No. 08/794,595 (filed Feb. 3, 1997); “Stacked Organic Light Emitting Devices”, Ser. No. 08/792,046 (filed Feb. 3, 1997); “High Contrast Transparent Organic Light Emitting Device Display”, Ser. No. 08/821,380 (filed Mar. 20, 1997); “Organic Light Emitting Devices Containing A Metal Complex of 5-Hydroxy-Quinoxaline as A Host Material”, Ser. No. 08/838,099 (filed Apr. 15, 1997); “Light Emitting Devices Having High Brightness”, Ser. No. 08/844,353 (filed Apr. 18, 1997); “Organic Semiconductor Laser”, Ser. No. 60/046,061 (filed May 9, 1997); “Organic Semiconductor Laser”, Ser. No. 08/859,468 (filed May 19, 1997); “Saturated Full Color Stacked Organic Light Emitting Devices”, Ser. No. 08/858,994 (filed May 20, 1997); “An Organic Light Emitting Device Containing a Hole Injection Enhancement Layer”, Ser. No. 08/865,491 (filed May 29, 1997); “Plasma Treatment of Conductive Layers”, Ser. No. PCT/US97/10252; (filed Jun. 12, 1997; Patterning of Thin Films for the Fabrication of Organic Multi-Color Displays”, Ser. No. PCT/US97/10289 (filed Jun. 12, 1997); “Double Heterostructure Infrared and Vertical Cavity Surface Emitting Organic Lasers”, Ser. No. 60/053,176 (filed July 18, 1997); “Oleds Containing Thermally Stable Asymmetric Charge Carrier Materials”, Ser. No. 08/929,029 filed (Sep. 8, 1997), “Light Emitting Device with Stack of Oleds and Phosphor Downconverter”, Ser. No. 08/925,403 (filed Sep. 9, 1997), “An Improved Method for Depositing Indium Tin Oxide Layers in Organic Light Emitting Devices”, Ser. No. 08/928,800 (filed Sep. 12, 1997), “Azlactone-Related Dopants in the Emissive Layer of an Oled” (filed Oct. 9, 1997), Ser. No. 08/948,130, “A Highly Transparent Organic Light Emitting Device Employing A Non-Metallic Cathode”, (filed Nov. 3, 1997), Attorney Docket No. 10020/40 (Provisional), and “A Highly Transparent Organic Light Emitting Device Employing a Non-Metallic Cathode”, (filed Nov. 5, 1997), Attorney Docket No. 10020/44, each co-pending application being incorporated herein by reference in its entirety. The subject invention may also be used in conjunction with the subject matter of each of co-pending U.S. patent application Ser. Nos. 08/354,674, 08/613,207, 08/632,322 and 08/693,359 and provisional patent application Ser. Nos. 60/010,013, 60/024,001 and 60/025,501, each of which is also incorporated herein by reference in its entirety. | Methods for preparing organic thin films on substrates, the method comprising the steps of providing a plurality of organic precursors in the vapor phase, and reacting the plurality or organic precursors at a sub-atmospheric pressure. Also included are thin films made by such a method and apparatuses used to conduct such a method. The method is well-suited to the formation of organic light emitting devices and other display-related technologies. | 7 |
[0001] This application claims priority to Taiwan Patent Application No. 101208199 filed on May 2, 2012.
BACKGROUND OF THE INVENTION
[0002] The present invention generally relates to a lock and the application thereof and, more particularly, to a lock capable of converting a horizontal axial rotation into a vertical displacement and the application thereof.
[0003] Electronic apparatus and storage devices in market are provided with a lock on the housing thereof to prevent access of components resided in the housing from people without authorization for security purpose. However, such lock currently available in market has disadvantages such as a large number of movable elements, a complex structure and a high cost.
[0004] It may therefore be desirable by one skilled in the art to provide a lock that allows a user to easily lock and unlock an object such as a cover plate of a housing with a simple, compact structure and low cost of. CL BRIEF SUMMARY OF THE INVENTION
[0005] To achieve the aforesaid objective, examples of the present invention may provide a lock mounted to a base. The base has an inner surface and an outer surface. The lock comprises a lock plate and a motion module. The motion module has a curved surface facing the lock plate. The curved surface comprises a first surface and a second surface. A main feature of the present invention is that the lock has a close status and a far status. The lock plate abuts against the first surface and has a first distance from the base when the lock is in the close status, and abuts against the second surface and has a second distance, which is greater than the first distance, from the base when the lock is in the far status.
[0006] For example, the lock disclosed above comprises a fixed portion, a movable portion and an abutting portion in practical applications. The fixed portion is fixed to the inner surface of the base. The movable portion extends outwards from the fixed portion and can be elastically deformed under the action of an external force. The through-hole portion is formed in the movable portion and through the lock plate, and has a sidewall. The abutting portion extends in a normal direction from the sidewall and abuts against the curved surface of the lock to adjust a relative distance between the lock plate and the base. Furthermore, the fixed portion, the movable portion, the through-hole portion and the abutting portion are all selectively formed integrally with the lock plate (ONE PIECE FORMED).
[0007] The motion module further has an extending portion that extends vertically towards the base and extends through the through-hole portion to be pivotally connected with the through-hole portion. The base comprises a through-hole, and the motion module comprises an interfacing part having a head portion and a tail portion. The tail portion is fixed to an end of the extending portion and penetrates through the base to be pivotally connected with the base, and the head portion abuts against the outer surface of the base. Both the head portion and the extending portion have a cross-sectional area greater than that of the tail portion. Meanwhile, the motion module has two blocking surfaces, and the two blocking surfaces are disposed on the first surface and the second surface respectively and extend in a normal direction from the first surface and the second surface respectively to limit a rotation angle of the abutting portion.
[0008] Besides, an angle of smaller than 6° is included between the base and an extending direction of the movable portion of the lock plate. The motion module has a back surface facing away from the lock plate, and a vertical distance between the back surface and the base in the close status is the same as that in the far status. It is worth noting that, the lock of the present invention can be used in an electronic device or a computer housing.
[0009] According to the above descriptions, some examples of the present invention may provide a novel lock that allows the user to easily lock and unlock an object such as a cover plate of a housing effectively in a limited space. As compared to the prior art, the lock of the present invention has a simple structure, a low manufacturing cost and a small volume. Thereby, the long-lasting problem with the prior art is solved.
[0010] Some examples of the present invention may provide a lock applied to a base of an electronic device, the base has an inner surface and an outer surface, the lock comprises a lock plate comprising: a fixed portion; and a movable portion; and a motion module having a curved surface facing the lock plate, the curved surface comprising a first surface and a second surface.
[0011] Some examples of the present invention may provide a lock applied to a base of a computer housing, the base having an inner surface and an outer surface, the lock comprises a lock plate comprising: a fixed portion fixed to the inner surface of the base; a movable portion extending outwards from the fixed portion; a through-hole portion formed in the movable portion and through the lock plate, and the through-hole portion having a sidewall; and an abutting portion extending in an normal direction from the sidewall and abutting against the curved surface of the lock to adjust a relative distance between the lock plate and the base; and a motion module having a curved surface facing the lock plate, the curved surface comprising a first surface and a second surface, the motion module comprising: an extending portion extending vertically towards the base and extending through the through-hole portion; an interfacing part having a head portion and a tail portion, the tail portion is fixed to an end of the extending portion and penetrates through the base to be pivotally connected with the base, and the head portion abuts against the outer surface of the base, wherein both the head portion and the extending portion have a cross-sectional area greater than that of the tail portion; two blocking surfaces disposed on the first surface and the second surface respectively and extending in a normal direction from the first surface and the second surface respectively to limit a rotation angle of the abutting portion; and a back surface facing away from the lock plate.
[0012] Additional features and advantages of the present invention will be set forth in part in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention. The features and advantages of the invention will be realized and attained by means of the elements and combinations particularly pointed out in the appended claims.
[0013] It is to be understood that both the foregoing general description and the following detailed description are exemplary and explanatory only and are not restrictive of the invention, as claimed.
BRIEF DESCRIPTION OF THE DRAWINGS
[0014] The foregoing summary, as well as the following detailed description of the invention, will be better understood when read in conjunction with the appended drawings. For the purpose of illustrating the invention, there are shown in the drawings examples which are presently preferred. It should be understood, however, that the invention is not limited to the precise arrangements and instrumentalities shown.
[0015] In the drawings:
[0016] FIG. 1A is an assembly diagram of elements of a lock in accordance with an embodiment of the present invention;
[0017] FIG. 1B is a partially cross-sectional front view of the lock in a close status in accordance with an embodiment of the present invention;
[0018] FIG. 1C is a partially cross-sectional back view of the lock in a far status in accordance with an embodiment of the present invention;
[0019] FIG. 2 is a schematic perspective view of a lock plate in accordance with an embodiment of the present invention;
[0020] FIG. 3 is a schematic perspective view of a motion module in accordance with an embodiment of the present invention;
[0021] FIG. 4A is a partially cross-sectional front view of a lock in a close status in accordance with another embodiment of the present invention; and
[0022] FIG. 4B is a partially cross-sectional back view of the lock in a close status in accordance with another embodiment of the present invention.
DETAILED DESCRIPTION OF THE INVENTION
[0023] Reference will now be made in detail to the present examples of the invention, examples of which are illustrated in the accompanying drawings. Wherever possible, the same reference numbers will be used throughout the drawings to refer to the same or like parts.
[0024] Hereinbelow, the aforesaid subject matter will be further described. The present invention relates to a lock that allows for locking and unlocking in a limited space. However, it shall be appreciated that, unless otherwise defined, all scientific and technical terms used in this specification shall have the same meanings as generally known by those skilled in the art. Additionally, what described in this specification is only some of various embodiments of the present invention, and any methods or devices similar to or equivalent to what described herein may be used in practical implementations of the present invention.
[0025] The wording “above or below” a numeric value as set forth herein shall be interpreted to include the numeric value itself. It shall be appreciated that, the wording “the present invention” and similar wordings used in this specification are all intended to mean the lock of the present invention. Furthermore, the sequence of steps of methods or flow processes used to execute disclosed functions in this specification shall not be limited to what described in this specification, but may be adjusted freely depending on the user's needs unless otherwise specified. Moreover, unless otherwise specified, the scale, sizes, relative positions and shapes of individual elements shown in the figures are all similar to what shall be in practical applications and this shall also be a basis for subsequent supplement or amendment of the specification. Considering that elements described in different embodiments of this specification have similar properties, like designations and reference numerals represent like elements throughout the attached drawings. Further, it shall be noted that, structural parts such as devices, modules and units set forth in this specification shall not be limited to hardware implementations independent of each other, but may also be integrated into a single unit.
[0026] Now, the lock of the present invention will be described. Referring to FIG. 1A through FIG. 1C together, FIG. 1A is an assembly diagram of a lock in accordance with an embodiment of the present invention, FIG. 1B is a partially cross-sectional front view of the lock in a close status S 1 in accordance with an embodiment of the present invention, and FIG. 1C is a partially cross-sectional back view of the lock in a far status S 2 in accordance with an embodiment of the present invention. Additionally, FIG. 1C has been turned over horizontally in order to distinguish FIG. 1B and FIG. 1C from each other. As can be seen, the lock 1 of the present invention is disposed on a base B to lock the base B to an external latching element L so that a relative position of the base B is maintained. The aforesaid base B generally refers to any object or a surface thereof on which the lock 1 of the present invention can be disposed. In this embodiment, the base B is a cover plate of a computer housing, but it is not limited thereto. The term “base B” may also refer to an electronic device, a door sheet, or any other object or a surface thereof that conforms to the aforesaid definition. The base B has an inner surface B 1 and an outer surface B 2 . The inner surface B 1 is defined as a surface of the base B that faces a lock plate 10 , and the outer surface B 2 is defined as the other surface of the base B that is opposite to the inner surface. Further, as can be known from the figures, the lock 1 of the present invention generally comprises the lock plate 10 and a motion module 20 . Taking FIG. 1A and FIG. 1B as an example, in the present invention, the lock plate 10 is sandwiched between the motion module 20 and the base B and, through axial rotation of the motion module 20 , the lock plate 10 is driven to abut against a surface of the motion module 20 so that the lock plate 10 is elastically deformed correspondingly in compliance with thickness variations of the surface of the motion module 20 . The lock 1 of the present invention has a close status S 1 and a far status S 2 depending on different relative positions of the lock plate 10 with respect to the base B. Simply speaking, the lock plate 10 is closer to the base B when the lock 1 is in the close status S 1 , and is farther from the base B when the lock 1 is in the far status S 2 . Thereby, the lock 1 of the present invention allows for locking and unlocking.
[0027] After having generally described the operation mode of the present invention, structures of the lock plate 10 and the motion module 20 will be described respectively now. Referring to FIG. 2 , there is shown a schematic perspective view of a lock plate of a lock in accordance with an embodiment of the present invention. The lock plate 10 refers to an element of the lock 1 that is used to mate with or abut against an external latching element L so that the base B and the lock 1 can be locked to each other. Furthermore, the lock plate 10 of the present invention generally has a fixed portion 11 , a movable portion 12 and a lock opening 13 .
[0028] The fixed portion 11 is disposed at an end of the lock plate 10 to fix the lock plate 10 to the surface of the base B. Taking FIG. 2 as an example, the fixed portion 11 is disposed on the lock plate 10 and comprises a large protrusion, a recess and a small protrusion so that the fixed portion 11 can be embedded into a corresponding structure of the base B. It shall be noted that, the large protrusion, the recess and the small protrusion illustrated herein are only provided as an example and are used to prevent wrong assembly by the user.
[0029] However, the fixed portion 11 of the present invention is not limited to what described above, and any part or structure that is located on the surface of the lock plate 10 and used to connect the lock plate 10 to the surface of the base B can be considered as the fixed portion 11 of the lock plate 10 . Furthermore, the means for connection between the fixed portion 11 and the base B is not limited to the protrusions and the recess disclosed above, and the fixed portion 11 and the base B may also be fixed to each other through adhesion, soldering, snap-fitting and so on.
[0030] The movable portion 12 of the lock plate 10 is adjacent to the fixed portion 11 of the lock plate 10 , and extends outwards from the fixed portion 11 . The movable portion 12 can be elastically deformed under the action of a force to adjust a vertical position of the locking opening 13 . Furthermore, as depicted, an angle A is included between an extending direction of the movable portion 12 and a surface on which the fixed portion 11 is disposed. Taking the design of FIG. 2 as an example, the angle is approximately 6°, but it is not merely limited thereto. Rather, the angle may be changed or adjusted correspondingly depending on such factors as the size of the lock plate 10 , the position of the fixed portion 11 and the shape of the motion module 20 , and is preferably smaller than 20°. On the other hand, the surface of the movable portion 12 is formed with a through-hole portion 14 which has a sidewall 15 , and the through-hole portion 14 is used for inserting the motion module 20 therethrough. The sidewall 15 further has a protrusion for use as an abutting portion 16 . The abutting portion 16 extends from the sidewall 15 in a normal direction T of the sidewall 15 . The abutting portion 16 is used to abut against the curved surface 23 of the lock 1 so as to adjust a relative distance between the movable portion 12 of the lock plate 10 and the base B according to the shape of the curved surface 23 .
[0031] The lock opening 13 extends outwards from the movable portion 12 , and is used to interlock with or abut with an external latching element L for purpose of locking the base B.
[0032] Generally speaking, the fixed portion 11 of the lock plate 10 is fixed to the base, and the lock opening 13 can be elastically deformed correspondingly in compliance with the varying height of the movable portion 12 so that the lock 1 is switched between a locking status and an unlocking status. Incidentally, the fixed portion 11 , the movable portion 12 , the through-hole portion 14 and the abutting portion 16 may be (but not limited to) integrally formed with the lock plate 10 (ONE PIECE FORMED).
[0033] Referring next to FIG. 3 , there is shown a schematic perspective view of the motion module 20 of the lock 1 in accordance with an embodiment of the present invention.
[0034] In the present invention, the motion module 20 generally refers to any object capable of controlling a vertical distance between the lock plate 10 and the base B so that the lock 1 can be switched between the locking status and the unlocking status by controlling the position of the lock plate 10 , or a combination of such objects. For example, in the design depicted in
[0035] FIG. 3 , the motion module 20 has a main body 21 and an interfacing part 22 . The motion module 20 is disposed on the surface of the lock plate 10 and is adapted to apply a force to the lock plate 10 in a direction towards the base B. The motion module 20 has a curved surface 23 facing the lock plate 10 , and the curved surface 23 comprises a first surface 23 A and a second surface 23 B. As can be seen, the first surface 23 A and the second surface 23 B are disposed at two ends of the curved surface 23 respectively and have a different height or thickness from each other. Additionally, the motion module 20 has two blocking surfaces 24 , which are disposed on the first surface 23 A and the second surface 23 B respectively and extend outwards in a normal direction from the first surface 23 A and the second surface 23 B respectively to limit a rotation angle of the abutting portion 16 . Besides, the motion module 20 has an extending portion 25 , which extends vertically towards the base B and is formed with a hollow hole portion 26 for another element to be inserted therein. Meanwhile, the motion module 20 further comprises an interfacing part 22 corresponding to the hollow hole portion 26 . The interfacing part 22 has a head portion 221 and a tail portion 222 . The tail portion 222 is fixed to an end of the extending portion 25 and extends through the hole of the base B to be pivotally connected with the base B, and the head portion 221 abuts against the outer surface of the base B. To achieve the aforesaid effect, the hole of the base B must have a horizontal cross-section area smaller than that of the head portion 221 and the extending portion 25 . Meanwhile, the tail portion 222 is connected into the hollow hole portion 26 through a conventional means so as to move along with the motion module 20 . For example, as shown in this figure, the hollow hole portion 26 and the interfacing portion are fixed with respect to each other by an adhesive or a thread structure. Furthermore, the outer surface of the head portion 221 is formed with a recess so that an unlocking tool can be inserted therein to rotate the interfacing part 22 . However, the present invention is not limited to the form of a recess, and the recess may also be replaced by a manually operated screw or other tool-free designs depending on the design requirements. Additionally, the reference plane of the aforesaid horizontal cross-sectional area is parallel to the base B.
[0036] Next, how the lock of the present invention is used and relationships among individual elements will be further described. Referring back to FIG. 1B and FIG. 1C , the motion module 20 is disposed on the other surface of the lock plate 10 opposite to the base B and is connected to the base B via an extending portion 25 that extends through the base B. After being fixed to the base B, the motion module 20 can only rotate axially and the position thereof or the maximum distance between the motion module 20 and the base B becomes invariable. Meanwhile, the abutting portion 16 of the lock plate 10 will abut against any position of the curved surface 23 of the motion module 20 .
[0037] Furthermore, the lock 1 has a close status S 1 and a far status S 2 in use. When the lock 1 is in the close status S 1 , the abutting portion 16 of the lock plate 10 abuts against the first surface 23 A and has a first distance D 1 from the base B; and when the lock 1 is in the far status S 2 , the abutting portion 16 of the locking plate 10 abuts against the second surface 23 B and has a second distance D 2 from the base B. It shall be appreciated that, switching between the first surface 23 A and the second surface 23 B of the motion module 20 has no influence on the position of the motion module 20 relative to the base B. It shall be emphasized again that, the motion module 20 can only rotate axially with respect to the base B but cannot perform other axial movements, so the distance between a back surface 27 of the motion module 20 and the base is invariable. Incidentally, the first distance D 1 and the second distance D 2 are defined as respective minimum vertical distances between the abutting portion 16 of the lock plate 10 and the base B. Simply speaking, the close status S 1 refers to a status in which the lock plate 10 is closer to the base B, while the far status S 2 refers to a status in which the lock plate 10 is farther from the base B.
[0038] Referring to FIG. 1A again, as can be seen, the motion module 20 has a back surface 27 , which is defined as a surface of the motion module 20 opposite to the curved surface 23 . When the lock 1 is disposed in the close status S 1 and the far status S 2 , the vertical distance between the back surface 27 and the base B remains unchanged and is not affected by variations of the distance between the lock plate 10 and the base B.
[0039] More specifically, when the first surface 23 A at a higher level abuts against the abutting portion 16 of the lock plate 10 , the lock plate 10 is pressed to be elastically deformed towards the base B to move closer to the base B, as shown in FIG. 1B . On the other hand, when the second surface 23 B at a lower level abuts against the abutting portion 16 of the lock plate 10 , the lock plate 10 is elastically deformed, with the fixed portion 11 being as a fulcrum, in a direction opposite to the base B to move away from the base B, as shown in FIG. 1C . Through the aforesaid operations and through use of an external latching element L, the lock 1 of the present invention can be switched between the locking status and the unlocking status. It shall be appreciated that, switching between the first surface 23 A and the second surface 23 B of the motion module 20 is accomplished through the horizontal axial rotation of the motion module 20 itself, and the vertical distance between the back surface 27 of the motion module 20 and the base B is not affected by variations of the distance between the lock plate 10 and the base B.
[0040] It shall also be emphasized that, any module that has a curved surface 23 for the abutting portion 16 to abut against and that can utilize the curved surface 23 to adjust the relative vertical position between the lock plate 10 and the base B can be considered as the motion module 20 of the present invention. For example, besides the design depicted in FIG. 1A , the motion module 20 may also be disposed between the lock plate 10 and the base B with the curved surface 23 thereof facing the lock plate 20 to accomplish the aforesaid movements as shown in FIG. 4A and FIG. 4B . In the latter case, the motion module 20 may selectively comprise a reset element 28 (e.g., a spring or a reed) for applying a force to the lock plate 10 in a direction towards or opposite to the base B. However, the motion module 20 is not limited to having the aforesaid reset element 28 , but may also be reset by virtue of elasticity of the lock plate 10 itself. Furthermore, because FIG. 4A and FIG. 4B correspond to FIG. 1B and FIG. 1C respectively, reference may be made to the above descriptions for design of individual elements and no further description will be made herein again. This design is different from the design depicted in FIG. 1A in that, the blocking surfaces 24 are omitted, so a user may lock and unlock the lock in a clockwise or counterclockwise direction and the rotation direction of the motion module during the locking and unlocking operations is not limited. Moreover, the lock of the present invention may also be adjusted to operate reversely, i.e., the locking and unlocking operations are accomplished by having motion module move together with the external latching element and sandwiching the lock plate therebetween.
[0041] According to the above descriptions, the present invention provides a novel lock that allows the user to easily lock and unlock an object such as a cover plate of a housing effectively in a limited space. As compared to the prior art, the lock of the present invention has a simple structure, a low manufacturing cost and a small volume. Thereby, the long-lasting problem with the prior art is solved.
[0042] The detailed descriptions of the preferred embodiments of the present invention are provided to disclose the features and spirits of the present invention more clearly but not to limit the scope of the present invention thereto. Rather, it is intended to cover various modifications and equivalent arrangements into the scope claimed in the present invention. Accordingly, the scope claimed in the present invention shall be interpreted in the broadest sense to cover all possible modifications and equivalent arrangements. | The present invention discloses a lock and the application thereof. The lock is applied on a base having an inner surface and an outer surface. The lock comprises a locking plate and a motion module. The motion module has a curved surface facing the locking plate. The curved surface has a first surface and a second surface. A main feature of the present invention is that the lock has a close status and a far status. The locking plate contacts with the first surface and has a first distance from the base in the close status, and contacts with the second surface of the base and has a second distance, which is greater than the first distance, from the base in the far status. The invention has the advantages of low cost and simplicity, and solves the long lasting problem of the prior arts. | 8 |
This invention relates to concrete pavers of the slipform variety. More particularly, a concrete paver is disclosed in which telescoping frame members extending across the paver are provided with extension members. These extension members enable the paver to expand to paving widths beyond that presently achieved by conventional telescoping members. Further, the present disclosure does away with the necessity of the installation of a fixed frame extension members. As a result, this invention also substantially reduces machine preparation time for paving at differing machine widths.
BACKGROUND OF THE INVENTION
Concrete slipform pavers are known. Specifically, such pavers include a "tractor" and a "paving kit".
Regarding the tractor, most concrete slipform pavers include a tractor which is comprised of a rectilinear frame which straddles the concrete roadway or runway while it is paved. This frame is propelled and supported on either end by side bolsters and crawler track(s). The frame supports a diesel engine driven hydraulic power unit which supplies power to the tractor and paving kit.
The paving kit is typically suspended below the tractor frame by mechanical means. The paving kit takes its hydraulic power from the power unit on the tractor. The tractor and paving kit comprising the slipform pass over the concrete placed in its path in a relatively even and level mass that can be conveniently paved. During this slipform process the tractor attached paving kit spreads the concrete dumped in the path of the paver, levels and vibrates it into a semi-liquid state, then confines and finishes the concrete into a slab with an upwardly exposed and finished surface. Sideforms mounted to the side of the slipform kit confine the sides of the slab during the paving process.
The tractor typically has either two or four crawler tracks supporting and propelling the frame and attached paving kit. Other kits can be attached to these tractors such as kits for conveying and spreading concrete and trimming and spreading base materials. For the purposes of this description, we will focus on the paving kit used for slipform paving.
With respect to both two and four track pavers, the tractor frame is known to telescope itself normal to the direction of the paving movement. This telescoping normal to the direction of the paving movement enables the tractor frame to span different widths of pavements within the limits of the telescopic extensions. Once these telescopic extensions limits are reached, a fixed frame extension can be added to one or both sides of the telescopic frame for further extension. Despite the telescopic ability of the frame, the process is still a relatively complex and time consuming operation. Adding a fixed frame extension(s) significantly increases the complexity and difficulty of the frame width change.
Regarding the addition of the fixed frame extension, this addition requires that the side bolster and crawler(s) on at least one side of the machine be removed, the fixed frame extension inserted, and the side bolster and crawlers reattached. Hydraulic and electrical lines must also be disconnected then reconnected. This is not a trivial operation. The frame section and side bolster/-crawlers are heavy members. They must be separately manipulated into place--usually by cranes and their attendant crews. Cranes have scheduling problems, are big, heavy, dangerous, and slow.
SUMMARY OF THE INVENTION
A conventional telescoping frame on a paving tractor is provided with fixed frame extension members for insertion to and attachment with a telescoping frame member. The conventional telescoping frame includes paired forward and paired rear side-by-side female tube members. Each forward and rear tube member conventionally acts for the telescoping support of male extension members which attach directly to the side bolster, which in turn attaches to the hydraulic jacking columns and crawlers. Within the limits of expansion, the male extension members co-acting with clamps acting through the female tube members provide for both movement of the point of crawler support and expansion of the paving width of the tractor frame. Into this combination, extenders are added for attachment to the supported end of the male extension members interior of the female telescoping members. During frame width expansion, the male telescoping members are expanded to register their ends interior of the female telescoping members to attachment access ports in the female telescoping member. The extenders are inserted, supported, and registered at complimentary attachment apertures with attachment to the male telescoping members taking place. Once attachment has occurred, further extension of the male telescoping members occurs. A simple system of pinned cross-bracing reinforces the extended frame with relatively light bracing members. When the telescoping members at both sides of the frame are provided with the extenders to extend the telescoping span of the paver, a tractor of greater expansion and range of expansion capability is provided which obviates the need for fixed frame extensions, and permit frame expansion without heavy lifting equipment.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1A is a perspective view of a concrete paver of this invention in conventional operation;
FIG. 1B is a perspective view of a concrete paver illustrating the crawler tracks turned 90° from the paving disposition illustrated in FIG. 1A and with the telescoping members in an orientation where the extending members may be inserted into the paver female telescoping tractor frame to increase the paving width;
FIG. 1C is a detail of the insertion of the extending members--it being understood that light lifting equipment (not shown) causes the required insert of the extender;
FIG. 2 is a perspective view that illustrates one side of the paver extended to the increased width for paving a wider slab, the other side of the paver not being shown and shows the light bracing members in position;
FIG. 3 is a plan schematic of the frame illustrating the principle of extension insertion for expanding the frame, the paver side bolsters not being shown;
FIG. 4A is a side elevation of the female telescoping member and a plan and elevation of the extender member illustrating apertures for the installation of pins to enable connection interior of the female telescoping tube of the extenders to the male member;
FIG. 4B is an elevation of the forward box beam of the paver frame illustrating apertures for insertion of pins to effect fastening of the extenders with the hidden lines showing apertures located on the inner female telescoping tube;
FIG. 5 is a plan schematic of the frame illustrating offset of the paver frame in expansion for positioning a reinforcing bar inserter at a position where interference with the frame member does not occur;
FIG. 6 is a detail illustrating the connecting end of the extender to the male telescoping member;
FIG. 7 is a detail of the male telescoping member connected to an extender, and applicable pins inserted through the female telescoping member, it being noted that line up pin holes may be required in the male telescopic member and extender connection for ease of pin hole line up; and
FIG. 8 is a partial plan view of the frame illustrating the case where the extenders are attached and the frame is contacted to minimum dimension.
DESCRIPTION OF THE PREFERRED EMBODIMENT
FIG. 1A illustrates paver P proceeding in paving direction 15 for paving roadway or runway R. Paver P includes tractor frame F and paving kit K. Since the invention herein relates to the configuration of tractor frame F, paving kit K will be briefly discussed. In the description here, it will be assumed that conventional paving kit may be removed or attached from tractor frame F for the purposes of transport or to add other attachments without further discussion.
Paving kit K is conventional and includes spreader plow 18. Spreader plow 18 functions to spread concrete placed in paving direction 15 on what is to become roadway or runway R. There follows metering gate, vibrators, slipform pan 22 and trailing pan 24. It will be understood that paving kit K can be augmented with all sorts of accessories. Reinforcing bar inserters, tamper bars, side bar inserters and the like are typically added or taken off the machine as the job requires.
It will be understood that the width of the paving kit K is varied with extensions like the tractor frame F as the particular width of the job specifies. Such paving kit extensions come in all matter of widths. It is common to have one foot, two foot, three foot, five foot, and six foot extensions. In the conventional placement of these sections, the telescopic tractor frame is first expanded, and the requisite number and length of paving kit extensions installed. Since this process is conventional, it will not be further discussed herein.
The operation of a paver can be simply stated for purposes of this description. Typically, a system of grade level reference wires W are strung adjacent and parallel to the roadway or runway grade being constructed. Sensors 26 with wire feelers, one located at each corner of the machine attached to the frame, follow grade level reference wires W. Leveling sensors (not shown) on the frame independently adjusts the height of the frame relative to each of crawlers T 1 -T 4 through hydraulic cylinder C 1 -C 4 at each corner of the frame. The paving kit suspended from the frame thus is continually adjusted to maintain a preset elevation disposition relative to the wires as paving occurs.
Frame F can be best understood with a first reference to FIG. 1A. Frame F includes side relatively telescoping members S. These respective side relatively telescoping members S are fully set forth and described in Guntert et al U.S. patent application Ser. No. 08/450,242, filed May 25, 1995 entitled FOUR TRACK PAVING MACHINE WITH TELESCOPING TRANSPORT COMPRESSION IN DIRECTION 0F PAVING MACHINE TRAVEL. An abbreviated description of the function of these side relatively telescoping members S will suffice.
Four track paver P is disclosed having a frame with side relatively telescoping members S or side bolsters which contract for transport to reduce the dimension of the machine in the direction of paving machine travel 15. The rectilinear frame includes four crawlers T 1 -T 4 , one at each corner of the frame. Each crawlers T 1 -T 4 is directly supported on its own hydraulic cylinder C 1 C 4 and mounted for pivotal movement about the axis of the hydraulic cylinder. The frame telescopes at side relatively telescoping side bolster members S between the leading and trailing crawlers at the sides of the machine. When expanded, the paving machine has the full forward and rear dimension required for paving. When contracted, the paving machine has a profile allowing convenient transport with the crawlers rotated 90° or normal to the direction of travel to power the frame widening. Full details of this function of the machine can be realized by consulting the above reference patent application which is incorporated by reference into this patent application. Conventional four track paver side bolsters with pivoting arms can also be used with the present application. It is envisioned that the present application can also be used with two track paver provided external hydraulic cylinders are utilized to provide the power to telescope in the absence of four crawler tracks and the ability of turning the four crawlers 90° or normal to the direction of paving to power the frame widening.
The present application relates to the side to side paving expansion of paver P. This being the case, attention will now be directed to FIG. 3. This figure is advantageous because it focuses on the paving width extension of the paver telescopic tractor frame and does not show the appurtenant apparatus.
Rectilinear tractor frame F includes forward box beam B F and rear box beam B R . Each forward box beam B F and each rear box beam B R defines leading interior female compartment 28 and trailing interior female compartment 30. Thus, side relatively telescoping members S and forward box beam B F and rear box beam B R define a rectilinear tractor frame F.
It is conventional with some pavers P to include telescoping expansion across the paving width. Accordingly, forward box beam B F and rear box beam B R each define forward female telescoping member F F at leading interior female compartment 28 and rear female telescoping member F R at trailing interior female compartment 30.
It is required that male telescoping members be received into the respective female telescoping members. This being the case, right forward male telescoping member 32 is received in forward female telescoping member F F of forward box beam B F . Similarly, left forward male telescoping member 34 is received in rear female telescoping member F R of forward box beam B F .
The trailing section of the frame is identically constructed. Right trailing male telescoping member 36 is supported in forward female telescoping member F F of rear box beam B R . Similarly, left trailing male telescoping member 38 is supported in rear female telescoping member F R of rear box beam B R .
Dimensions are important. Therefore, reference will be made to the dimensions important here utilized in the United States. It is envisioned that this invention will be adaptable to dimensions important to other parts of the world that incorporate Metric Dimensions.
Forward box beam B F and rear box beam B R are typically a nominal 12 feet in length. Respective right forward male telescoping member 32, left forward male telescoping member 34, right trailing male telescoping member 36, and left trailing male telescoping member 38 are also 12 feet in length. This enables the leading and trailing male telescoping members to be entirely received within forward box beam B F and rear box beam B R . It can therefore be quickly understood by the reader that the present machine has a capability of paving over a 12 foot span to match the minimum paving width generally paved in the United States. Even though the tractor frame might be limited to a minimum width of 12', when the telescopic frame is fully contracted, the paving kit may be arranged in a paving width less than 12'.
Expansion of paver P at any width between 12 and 25 feet can be readily understood. It is known that during telescoping movement or expansion of paver P, connection and disconnection of hydraulic jacking columns (hereinafter called cylinders) C 1 C 4 is not desired. Accordingly, the respective cylinders C 1 C 4 are all attached at the distal ends of respective right forward male telescoping member 32, left forward male telescoping member 34, right trailing male telescoping member 36, and left trailing male telescoping member 38. Crawlers T 1 -T 4 conventionally attach to hydraulic cylinders C 1 -C 4 . For the purposes of this illustration, FIG. 3 does not show the side bolsters and only shows the cylinders C 1 -C 4 and crawler tracks T 1 -T 4 attached to their respective corner. Presuming that crawlers T 1 -T 4 are rotated 90° by respective turning cylinders 40, it can be seen that powering of crawlers T 1 -T 4 can move to extend the respective male telescoping members 32, 34, 36, and 38. In a normal extension process, the respective male telescoping members 32, 34, 36, and 38 would all be extended in the range of six to six and one half feet. This would extend the paver tractor frame from 12 foot to a maximum range of a 25 foot span. In the prior art, this is the maximum paving width extension that such a paver would allow.
The reason for this maximum extension can be easily understood. It will be understood that male telescoping members 32, 34, 36, and 38 are in cantilever support when extended from the respective forward box beam B F and rear box beam B R . Further, the paver is heavy, weighing in the order of 75,000 pounds or more. It is therefore to be understood that extension of male telescoping members 32, 34, 36, and 38 substantially beyond a six foot extension is not prudent. Thus a certain minimum length of male telescoping member must remain engaged in the female box beam frame section to maintain the structural integrity of the tractor frame. Moreover, in the prior art and in most cases, power for the extension of the telescopic tractor frame was provided by hydraulic cylinders or screw jacks located either inside or outside the telescopic members and which were connected between the male and female telescopic tube. These hydraulic cylinders or screw jacks had the ability to extend the male telescoping members away from the female telescopic tube to its entire extended length or a portion of it, where in such cases, an extension to the extending cylinder or screw jack was required.
In the prior art, the only way the paver telescopic tractor frame could be extended beyond the maximum telescopic ability of 25' was to unbolt and hydraulically disconnect the cylinders C1-C4 and crawler tracks T1-T4 from each corner of the machine and add a fixed frame extension to the ends of the male telescopic members 32, 34, 36, and 38 and the cylinders C1-C4.
Having set forth this limitation, extenders E 1 -E 4 can now be discussed. This may be most conveniently done by considering the disposition of tractor frame F as illustrated in FIG. 3 and thereafter discussing the extension of the frame as illustrated in FIG. 5.
Before insertion of extenders E 1 -E 4 , it is required that tractor frame F be expanded to the approximately 25 foot span illustrated in FIG. 3. This defines clearance required for receipt of extenders E 1 -E 4 in two discrete aspects.
First, the respective forward female telescoping member F F and rear female telescoping member F R of forward box beam B F and rear box beam B R are open on the ends for receipt of extenders E 1 -E 4 . Second, hydraulic cylinders C 1 -C 4 and crawlers T 1 -T 4 , are sufficiently moved away from forward box beam B F and rear box beam B R so as to define clearance for insertion of extenders E 1 -E 4 .
It should be noted that insertion of extenders E 1 -E 4 is a relatively simple matter that can be handled by the onsite operating crew of the paver. Specifically, by utilizing a fork lift, boom truck or similar lifting apparatus, each of extenders E 1 -E 4 can be individually inserted. At the same time, detachment of heavy hydraulic cylinders C 1 -C 4 and crawlers T 1 -T 4 is not required.
Referring to FIG. 4A, right forward male telescoping member 32 is illustrated without attachment of either hydraulic cylinder or crawler. It defines single male connector plate 42 at its end opposite from where the hydraulic cylinder and crawler is attached. Single male connector plate 42 is bored by upper pin aperture 44 and lower pin aperture 46.
The construction of extender E 1 is analogous. It includes paired female connector plate members 52 which are in turn bored by upper pin aperture 54 and lower pin aperture 56.
Fastening of the member together is conventional. Referring to the details of FIGS. 6 and 7, such attached can be readily understood. Specifically, by placing pins N across the respective apertures 44, 54 and 46, 56, extenders E 1 -E 4 can be rigidly attached to their respective male telescoping members 32, 34, 36, and 38.
There remains to be understood how such pinning can occur within forward box beam B F and rear box beam B R . The detail of forward box beam B F in FIG. 4B provides elongate upper aperture 64 and elongate lower aperture 66 in forward box beam B F . By registering the respective ends of extenders E 1 -E 4 to the respective male telescoping members 32, 34, 36, and 38, ready access for the required insertion of pins N can occur.
It is necessary that the respective forward box beam B F and rear box beam B R have clamps for firm attachment to the respective male telescoping members 32, 34, 36, and 38. To this end, clamps L 1 -L 4 are illustrated only at forward box beam B F in FIG. 4B. To avoid confusing detail, these respective clamps are not set forth elsewhere in the drawings.
Further, a word about the practical aspects of inserting pins N. In a heavily loaded paver P, it will be understood that some gross manipulation of the paver will be required for precise pin placement. This being the case, clamps L 1 -L 4 can be manipulated, paver P and kit K can be raised and lowered and a portion of the tractor weight taken by four stanchions located at the four corners of the female telescopic tractor member, and both the male telescoping member and the particular crawler moved to effect pin placement. The use of separate line up holes in the male and female connector plates is envisioned to effect pin placement.
It will further be understood, that expansion and contraction of paver P can occur through crawlers T 1 -T 4 . The paver P is designed so the crawler tracks on each side of the machine can be controlled together as a pair. This provides the power for driving the telescoping movement. In the case where this tractor frame is used in conjunction with two track machines, where four crawlers are not available for driving the telescoping movement, conventional external hydraulic cylinders as used in the prior art, connected between the male and female telescopic members, can be used to power the telescopic movement.
There remains to be considered the expanded disposition of tractor frame F as illustrated in FIG. 5. As shown in FIG. 5, paver P is expanded to a maximum design paving width of 34 feet. Normally, such expansion will be symmetrical; each of the male telescoping members 32, 34, 36, and 38 will extend the same distance. Since this is easily comprehended, we illustrate the case where eccentric expansion has occurred. A word of explanation of the need for eccentric expansion can be helpful.
As has been previously emphasized, paver P frequently includes installed accessories such as bar inserters, side bar inserters, and other accessories as the vagaries of any job may require. At the same time, the transverse spacing of such accessories may interfere with placement of the major structural members of tractor frame F such as side relatively telescoping members S. This being the case, eccentric expansion such as that illustrated in FIG. 5 can act to register attached accessories to their required location.
Referring to FIG. 5, it can be seen that extenders E 2 and E 4 protrude partially from forward box beam B F and rear box beam B R , respectively. On the other side, extenders E 1 and E 3 do not protrude at all from rear box beam B F and rear box beam B R , respectively. This gives the disclosed apparatus a flexibility of dimension that is highly practicable.
It is apparent, that when male telescoping members 32, 34, 36, and 38 are fully extended, cross bracing of paver P will be desired--if not required. Referring to FIG. 2, such cross bracing is illustrated. Specifically, with extenders E 1 -E 4 installed and male telescoping members 32, 34, 36, and 38 extended, two types of cross bracing can be utilized. Diagonal cross brace 68 and normal cross brace 70 can be used with conventional fastening as by bolts or pins occurring at the distal ends of the braces 68, 70 to male telescoping members 32, 34, 36, and 38. It is envisioned that one or both of the distal ends of the cross bracing may include a screw adjustable attachment bracket so that the length of the brace does not have to be exact.
There also needs to be considered the minimum contracted disposition of the tractor frame F as illustrated in FIG. 8 with the extenders attached. As shown in FIG. 8, paver P (not completely shown) is contracted to its minimum design paving width of 17'6" with the extenders E 1 -E 4 still attached. Because the female telescoping members B R , B F , F F , F R are all open on the end to receive extenders, the male telescoping members 32, 34, 36 and 38 can be contracted until they interfere with the side bolsters. In prior art, as stated above, the maximum range of telescopic ability of the tractor frame was six to six and one-half feet per side, or a telescopic range of 12' to 25'. Because of the opening on the ends of the female telescoping members, the male telescopic members may be contracted beyond the ends of the female tubes by approximately three feet on a side. Thus the resulting range of telescopic ability is 17'6"to 34', or eight and one quarter feet side.
The reader will understand that detail of attachment of paving kit K has been in the large part omitted. This omission is intentional as this attachment is standard and well understood by the prior art. It is further understood that this paving kit can be substituted with a concrete spreading/placing kit or a base spreading/finegrading kit.
It will be further understood that this invention is equally applicable to both two track and four track pavers. This being the case, it is understood that the tractor of this invention includes at least two crawler tracks with one crawler on either side of the paver. A tractor having four crawler tracks is included in this definition.
In the above specification, we have illustrated the preferred embodiment to include male and female telescoping members. The reader is to understand that these respective terms are used in the broadest possible sense. What is required is that the two members move relative to one another with cantilever support being taken by one member from an adjacent member. Thus, all types relatively sliding support and extension schemes are intended to be covered. These include conventional telescoping connection, and side-by-side members which slide relative to one another and provide in the extended position relative support to one another. | A conventional telescoping frame on a paving tractor is provided with fixed male extension members for insertion to and attachment with a telescoping frame member. The conventional telescoping frame includes paired forward and paired rear side-by-side female tube members. Each forward and rear tube member conventionally acts for the telescoping support of male extension members which attach directly to the cylinder and crawler via a side bolster. Within the limits of expansion, the male extension members co-acting with clamps acting through the female tube members provide for both movement of the point of crawler support and expansion of the paving width of the tractor frame. Into this combination, extenders are added for attachment to the supported end of the male extension members interior of the female telescoping members. During frame width expansion, the male telescoping members are expanded to register their ends interior of the female telescoping members to attachment access ports in the female telescoping member. The extenders are inserted, supported, and registered at complimentary attachment apertures with attachment to the males telescoping members taking place. Once attachment has occurred, further extension of the male telescoping members occurs. A simple system of pinned cross-bracing reinforces the extended frame with relatively light bracing members. | 4 |
CROSS REFERENCE TO RELATED APPLICATIONS
[0001] This application claims the benefit of U.S. Provisional Application No. 61/619,880 filed on Apr. 3, 2012, the contents of which are incorporated by reference herein in their entirety.
BACKGROUND OF THE INVENTION
[0002] 1. Field of the Invention
[0003] The present invention generally relates to embodiments of a method, system and apparatus for optimized management of medicine administration.
[0004] 2. Description of the Related Art
[0005] Modern medicine relies heavily on the prescription of medications that are to be taken by the patient in an appropriate treatment regimen. A single prescription might involve a regimen such as: “Take 2 tablets, twice per day, morning and evening, after a meal.” Patients who have complex medical problems commonly receive multiple prescriptions, which can lead to patient confusion and frustration. Many patients fail to faithfully follow the treatments that have been prescribed, especially when they face chronic “polypharmacy” regimens: the need to follow multiple prescription regimens at once. Poor compliance can lead to poor patient outcomes and increased healthcare costs in the form of expensive interventions and a higher incidence of hospitalization.
[0006] Poor adherence to prescription regimens can sometimes be partially addressed by the assistance of a nurse caregiver, to place medicines into organizing containers and then provide reminders and instructions to the patient in an ongoing manner. The problems with this approach are: (a) it is labor intensive and hence relatively expensive, (b) it works only when patients are in proximity to a nurse caregiver, (c) there's no easy or efficient way for medical professionals to monitor the patient's actual usage pattern unless they are continuously in proximity, and (d) any medications left unused are wasted.
[0007] Embodiments of the invention described herein address these concerns by providing a novel automated method, system and apparatus for organizing medications for the patient, capable of reminding them to take the medication, tracking their usage pattern, and enabling reclamation of any unused medications in a manner that meets FDA requirements for reuse.
SUMMARY
[0008] One embodiment of the invention includes a comprehensive, technology-enhanced pharmacy system for patients following a complex medication regimen. The system is capable of addressing multi-faceted factors which undermine treatment adherence in the target population. The system comprises: (1) a Computer Assisted Telephone Interview (CATI) platform capable of use by pharmacy personnel in structuring and guiding patient interactions; (2) a Multi-Source Integrated Treatment Database (MSITD) System including prescription information, drug information, real-time treatment status variables, and provider/patient preferences; (3) a set of Treatment Optimization Algorithms (TOA) configured to optimize patient medication regimens with respect to factors such as cost, safety, and lifestyle; (4) Personal Medication Cartridges (PMC) including customized medication packets and barcode or RFID technology for tracking; (5) a portable, mobile-technology enabled Drug Dispensing Device (DDD) capable of supporting polypharmacy medication regimens and the Personal Medication Cartridges; (6) a Treatment Incentive Program (TIP) for motivating patients to maintain treatment adherence; and (7) Treatment Portals for use by physicians, pharmacy personnel, and patients for monitoring treatment status as appropriate with respect to medication adherence, clinical symptoms, and overall treatment progress.
[0009] Embodiments of the invention include a portable medication dispenser (DDD) that may provide for tracking of dispensing activity and automating selection of medications to dispense. The DDD is configured to remind patients to take medications at the proper time, and then provide the correct medications. The apparatus includes a processing unit and sufficient information technology such that it can determine which medications should be dispensed at any particular time. The apparatus can also trigger reminders to the patient when medication administration is appropriate. For example, when a patient presses a “dispense” button on the DDD, the DDD can determine the appropriate medications to dispense at that time.
[0010] One embodiment of the DDD accomplishes the dispensing of medications by loading a Personal Medication Cartridge (PMC) which includes medication packets for any or all of the types of medication that the patient may need. Each packet may hold one or more pills, and each packet may be labeled with an identifying mark, such as, for example, a barcode. The PMC may include sealed and labeled blister packets with medication, where the labels include information specific to the prescription. In this case, the printed information may include a barcode, RFID, or similar that can be read by a barcode reader, RFID, or similar, that will be located within the DDD and a mechanism is provided such that the barcode reader can read and identify each of the packets loaded into the DDD via the PMC.
[0011] An embodiment of the apparatus may also comprise a dispensing mechanism such that when the barcode reader identifies the correct medication packet for dispensing, the dispensing mechanism can push the packet out of the device for use by the patient. After dispensing one medication packet, the DDD can repeat the process of using the bar code reader to identify the next packet that needs to be dispensed, and can employ its dispensing mechanism again to dispense that packet. The DDD may repeat this process until all needed packets are dispensed.
[0012] To supplement that patient's knowledge, the DDD may contain a screen that displays information about each packet as it is dispensed. This can include information such as “take this medication with food.”
[0013] The DDD may also contain a system to transfer data to/from a remote system, such as a wireless modem. As packets are dispensed to the patient, the patient's usage pattern is recorded and eventually relayed to remote medical systems, such as the Master System included in embodiments of this invention.
[0014] Loading the DDD within the pharmacy is fairly straightforward. The DDD can perform automatic error checking routines to assure that the medications loaded are those expected for the patient. Specifically, when the PMC is loaded into the DDD, each packet contained in the PMC may be read by the barcode reader. This information can be corroborated with data in the MSTID system, and therefore pharmacy or caregiver errors can be caught. For example, if the wrong medications are provided to the patient, they will not be dispensed.
BRIEF DESCRIPTION OF THE DRAWING FIGURES
[0015] Certain embodiments in the present invention will be better understood when read in conjunction with the appended drawings wherein like reference numerals refer to like components. For the purposes of illustrating the device of the present application, there is shown in the drawings preferred embodiments. It should be understood, however, that the application is not limited to the precise arrangement, structures, features, embodiments, aspects, and devices shown, and the arrangements, structures, features, embodiments, aspects and devices shown may be used singularly or in combination with other arrangements, structures, features, embodiments, aspects and devices. The drawings are not necessarily drawn to scale and are not in any way intended to limit the scope of this invention, but merely to clarify a single illustrated embodiment of the invention. In the drawings:
[0016] FIG. 1 is an exemplary diagram of the relationship between components of an embodiment of the invention;
[0017] FIG. 2 is an exemplary diagram illustrating components of a drug dispensing device;
[0018] FIG. 3 is an exemplary flow diagram illustrating a dispensing process from an exemplary drug dispensing device;
[0019] FIG. 4 is a perspective view of an exemplary embodiment of the DDD component and accompanying features;
[0020] FIG. 5 is a top view of an exemplary embodiment of the DDD component featuring additional accompanying features;
[0021] FIG. 6 is a perspective view of an exemplary embodiment of specific features of the DDD component;
[0022] FIG. 7 is a top view of an exemplary embodiment of the DDD component featuring accompanying features;
[0023] FIG. 8 is a perspective view of an exemplary embodiment of the DDD component;
[0024] FIG. 9 is an exemplary engineering drawing of multiple perspectives of the DDD component and accompanying features according to an embodiment of the invention;
[0025] FIG. 10 is an exemplary exploded engineering drawing of the DDD component and accompanying features according to an embodiment of the invention; and
[0026] FIGS. 11 a and 11 b are top views of exemplary engineering drawings of the DDD component and accompanying features according to an embodiment of the invention.
DETAILED DESCRIPTION OF THE INVENTION
[0027] As shown in FIG. 1 , components of one embodiment of a medication therapy management system (called DialogRX) include: A Master System 100 ; a Computer Assisted Telephone Interview (CATI) platform 101 for use by pharmacy personnel in structuring and guiding patient interactions; a Multi-Source Integrated Treatment Database (MSITD) System 102 comprising prescription information, drug information, real-time treatment status variables, and provider/patient preferences; and a set of Treatment Optimization Algorithms (TOA) 103 for optimizing patient medication regimens with respect to cost, safety, and lifestyle. The embodiment's components may interact synergistically to track and guide patient use of Personal Medication Cartridges (PMC) 104 which may contain individual medication dose packets labeled with barcodes or similar. The embodiment also comprises a portable mobile-technology enabled Drug Dispensing Device (DDD) 105 designed for holding and dispensing dose packets from the Personal Medication Cartridges at appropriate times and thus guiding patients through polypharmacy treatment regimens. A Treatment Incentive Program (TIP) 106 may be included, designed to motivate the patient and maintain treatment adherence. Communication with physicians, pharmacy personnel, and patients may be facilitated by Treatment Portals 107 for monitoring treatment status as appropriate with respect to medication adherence, clinical symptoms, and overall treatment progress. The Treatment Portals 107 and CATI platform 101 may connect with the Master System 100 via communication channels 108 that can be a secure internet connection (HTTP over TCP) or any other appropriate communication channel.
[0028] In some embodiments, the CATI platform 101 may be configured for use by pharmacy personnel or treatment management assistants to provide treatment assessments and interventions surrounding patients' medication regimens. The system may also include a series of “smart” CATI modules 109 that are part of the Master System 100 . Modules 109 can be driven by real-time data for responding to key treatment-related events, such as the start of treatment, medication regimen changes, missed doses, refills, adverse reactions, poor adherence, or other medication-related problems. When an event occurs, a corresponding module may activate, detailing appropriate responses to pharmacy personnel or other users on a screen-by-screen basis. The activation may also include scripts for collecting additional information, administering assessments, educating patients, or teaching new skills and coping strategies. Pharmacy interviewers may read the script and/or questions posed on the computer screen and record any relevant answers or information directly into the computer. This information may then be entered into the MSITD 102 as described below and used as part of real-time branching logic sequences to continually guide the treatment process.
[0029] In some embodiments of the invention, the CATI platform 101 may also include CATI-Modules 109 . CATI Modules 109 may include modules for providing Comprehensive Medication Reviews (CMR), Disease State Management, Patient Education, and Treatment-Related Problem Solving. One purpose of the CMR module is to comprehensively assess and optimize patients' medication regimen and related routines. A list of any or all of the patients' medications, including prescription and over-the-counter (OTC) medications, herbal therapies, and dietary supplements, along with related dosing parameters and guidelines (such as, for example, strength, frequency, missed dose rules, take with/without food, etc.) are reviewed and entered into the patient record and MSITD 102 described below. For use in the treatment optimizer algorithms, patients may also be asked to provide a “dosing convenience rating” for recurring daily and/or weekly activities, such as eating breakfast, coming home from work, going to bed, or other parts of patients' typical routines. Disease State Management modules may focus on assessing the clinical symptoms associated with patients' medical and psychiatric conditions, as well providing coping strategies for the common side-effects of the related medication treatment. Patient Education modules may focus on proactively enhancing patients' general disease and treatment knowledge, while TRPS modules may help providers respond to treatment-related problems as they occur in real-time, such as poor adherence rates, untimely cartridge swapping or refill requests, or other adverse events or treatment lapses.
[0030] In some embodiments of the invention, the MSITD System 102 is a master database, control, and reporting system for the apparatus, method or system. It may comprise prescription (Rx) information, drug information and patient-specific data. The drug data may include established dosing guidelines, restrictions, and warnings of commonly used prescription and OTC medications. The patient-specific data may include treatment-related data collected during enrollment in the DialogRX, including results of CATI-assessments, adherence rates, scheduling information, TIP points, and patient/provider preferences.
[0031] In some embodiments of the invention, Treatment Optimization Algorithms (TOA) 103 may be configured to utilizing MSITD data. The TOA 103 may comprise a series of treatment optimization algorithms which can be configured to optimize treatment outcomes, treatment cost, safety, and overall lifestyle. The TOA's cost optimizer may review the medications included in patients' regimen and identify potentially less expensive alternatives, such as generics. The TOA's safety optimizer may provide adverse reaction information and contraindication data for drugs included in the regimen. The TOA's lifestyle optimizer may use drug-information and patient scheduling/lifestyle preferences to devise a medication schedule that minimizes the total number of weekly dosing episodes, while simultaneously adhering to individual drug dosing guidelines and maximizing the convenience of individual dosing episodes from the patient point of view.
[0032] In some embodiments of the invention, a Patient Medication Cartridge 104 holds individual dose packets 203 , which contain medications for the patient's regimen. FIGS. 2 , and 4 - 11 illustrate exemplary designs and embodiments of the Drug Dispensing Device (DDD) 201 as discussed above. In this exemplary embodiment, the DDD is loaded with a PMC 202 made of a pre-formed, ring-shaped plastic carrier with “slots” arrayed on the ring in a circular pattern. It is envisioned, however, that other shapes and patterns may be utilized. The dose of a given prescription (typically 1 or 2 pills/capsules) is loaded into individual dose packets 203 , and each packet is set into a slot on the PMC 201 . Dose packets can be formed, for example, by loading pills into perforated plastic blister sheets that have indents for pills, sealing that blister sheet with a label, and then breaking the blister tray into individual packets along perforated lines. Labels may be printed such that dose packets display both printed information and a computer-readable mark, for example, a barcode, that identifies the medication contained within the dose packet. Dose packets would be configured to meet the most recent FDA standards of tamper-evident unit packaging, meaning that unused medication would be returnable in their original PMC packaging. Commercial providers of pharmaceutical packaging such as Medi-Dose have provided blister packaging with similar functionality.
[0033] The DDD 201 is designed to be easily loaded with a Patient Medication Cartridge (PMC) and can then read the identity of each dose packet contained in the PMC. The DDD 201 may resemble a portable CD player in shape, with a fold-open top and an open space inside for inserting a PMC 202 , which in turn holds dose packets 203 . In other embodiments, the DDD 201 may be configured in other shapes suitable for the invention. The DDD 201 further comprises a barcode reader (or RFID, or similar) 204 and an electronic system 217 with components known to one skilled in the art for logical control, user interface creation and control, and communication with the master system, including a CPU 205 , ROM 206 , read/write memory 207 , and optional components such as a wireless modem 208 , LCD screen 209 , keypad 210 , and speakers 211 . Prescription and drug information may be stored locally or accessed at the MSITD System 102 via a modem device. The exemplary PMC can the rotated by a rotating mechanism 212 that is under the control of the CPU 205 . This mechanism, which may contain a motor 219 and engage the PMC via gears 218 , can rotate the exemplary PMC ring through at least 360 degrees so that all dose packets 203 can pass in front of the bar code reader (or RFID, or similar) 204 and be identified by the computing system. In some embodiments, the dose packets 203 may be oriented on the PMC such that a barcode label (or similar) 213 on the back of each packet can be seen by the barcode reader 204 that is mounted within the DDD 201 . The DDD 201 may also comprise an ejection mechanism 214 which can eject the dose packets 203 via an exit slot 215 . The ejection mechanism may be comprised of a geared motor 221 driving an ejection arm 222 that can push a packet out of the exit slot 215 . The exit slot 215 may be monitored by a sensor 216 connected to the CPU 205 , enabling the CPU 205 to determine when dose packets 203 have been both pushed outwards and then taken away by the patient. The rotating mechanism 212 may optionally contain a Geneva output gear interfacing with a Geneva planetary ring 220 , such that the rotating mechanism 212 can induce step-by-step rotation of the Medication Cartridge 202 . Thus each packet 203 will stop in front of the base code reader 204 and remain steady so that the barcode can be read reliably.
[0034] The information on the barcodes (or similar), combined with information local to the DDD computing system, or available via a remote connection to the Master System 100 , can enable the DDD computing system to be aware of the exact nature of the medications loaded into the device. This information can be correlated with information available to the DDD (either locally resident or available remotely) about the patient's prescriptions and dispensing instructions for patient medications. Thus, the local computing system may have access to the information needed to dispense correct medications at the proper time. When the CPU determines that is it the proper time to dispense a particular dose packet, it instructs the rotating mechanism to advance the PMC to the correct position for dispensing of that dose packet. The correct position can be calculated by the CPU subsequent to initialization and reading of all packets in the PMC, and it can be further corroborated by using the bar code reader to confirm that the expected dose packet is in the exit position. The CPU can then initiate dispensing by activating the ejection mechanism. Various possible ejection mechanisms can be devised by one familiar with the art.
[0035] FIG. 3 illustrates an exemplary process followed by the DDD 201 . The CPU triggers an initialization procedure 301 once the device is loaded with a PMC 202 whereby the ring-shaped PMC may rotate (for example, by 360 degrees or more) by the rotating mechanism 212 . This enables the CPU 205 to sense the dose packets 203 loaded into the device and its location within the device, information which can be stored and used when the CPU needs to dispense a particular dose packet.
[0036] In step 303 , the CPU correlates information about each packet found with drug information, prescription information, and patient information (whether retrieved from the Master System 100 or stored locally). The CPU can note discrepancies from the expected dose packets, and can initiate alerts via the display and/or via communication with the Master System. When a dosing episode 304 is scheduled, the device reminds users, for example, via visible message on the LCD, beeping, and/or vibrating, initiating a phone call via the Master System, etc. There embodiment may include reminder mechanisms known to one skilled in the art. The patient is asked to acknowledge this reminder by signaling a “Dispense” event, for example, by pressing a button on the DDD for “Dispense.”
[0037] If, in step 305 , the patient does not signal “Dispense,” the device may wait a period of time and then return via path 306 to wait for another dosing episode. Along this path the device will recalculate, prior to the next dosing episode, the medications that need to be dispensed at the next reminder event. Some medications may need to be increased due to a missed dose, while others might not be increased, and hence a different set of dose packets may be selected for the next dispense event. The DDD's CPU, potentially in conjunction with instructions from the Master System 100 , handles this recalculation.
[0038] When the patient does signal “Dispense,” the system moves on to step 307 to index the PMC such that it is in position for dispensing of an appropriate dose packet. In the exemplary embodiment, the PMC 202 is rotated within the DDD by the rotating mechanism, under the control of the computing system, until a packet to be dispensed by the DDD comes into an exit position. This can be confirmed by the barcode reader (or similar) 204 . This will be a position adjacent to an exit slot 215 .
[0039] In step 308 , the ejection mechanism 214 is initiated, which in the exemplary embodiment consists of a mechanical arm that pushes the packet partially out of an exit slot 215 . A sensor 216 near the exit slot notes when the patient has grasped the packet and pulled into completely out, as the patient is instructed to do via the Display 209 . After a dose packet 203 is partially ejected in step 308 , written and/or audio prompts may guide the patient to proper usage (e.g. “take with water”) for that medication in step 309 . The DDD computing system may determine in step 310 if there is another dose packet 203 to dispense at this time, and if so via path 311 it calculates the next packet and returns to step 305 to find and dispense the next dose packet 203 . If the CPU 205 determines that all required dose packets 203 have been dispensed at this time, it follows path 312 to calculate actions for the next dosing episode and waits for the appropriate time to initiate that dosing episode via step 304 .
[0040] In this embodiment, the DDD and its computing resources can track and report the times at which the patient has take manual action to remove medication packets. Reporting to the Master System 100 can occur via modem 208 , or can occur via other communication means as known in the art. Additionally, if the patient fails to take medication at an advised time, the DDD (and its associated computing resources, for example, the Master System 100 networked to the DDD) can recalculate the appropriate treatment path for the patient. For example, if the patient misses a Monday morning dose, the DDD may dispense different medications on Monday afternoon than it otherwise might have. Some medications, when doses are missed, need to be double-dispensed the next time, whereas others do not. This embodiment is configured to accommodate that complexity. Medications from the PMC that are ultimately not dispensed can be reclaimed and reused in future regimens.
[0041] In some embodiments, a Treatment Incentive Program (TIP) may comprise an incentive system incorporated into the DialogRX program to encourage proper system usage and ongoing treatment adherence. TIP points will be awarded to patients for completing assessment and/or intervention interviews with pharmacy personnel, completing educational materials, inserting the expected cartridges into the device in a timely manner, and for achieving specified levels of adherence as measured by the DDD system. Points can then be redeemed for discounts on various DialogRX products and services, including reduced drug costs, copayments, and/or subscription fees. Use of the TIP provides an important motivational impetus for maximizing patient adherence to all treatment-related protocols.
[0042] Treatment reports and treatment management features may be accessible to pharmacists, physicians, and patients as appropriate through secure, password-protected HIPPA compliant portals. Treatment reports may comprise a comprehensive list of patients' current medications and related dosing guidelines, current weekly dosing schedule, adherence records for all drugs across specified timeframes and/or particular dosing episodes, results of all assessments, completed CATI-interviews and/or other educational materials, and TIP totals. By themselves or with the assistance of pharmacy personnel, patients can view their own treatment reports, update scheduling preferences, change the planned time of future dosing episodes, reapply the optimizer algorithms, and set personal dosing prompt preferences. Portals may also be used for integrating physicians into the treatment process, whereby physician preferences for receiving treatment reports and/or alerts can be set (i.e., via phone call, mail, email, or, when available, automatic integration into EMRs).
[0043] Immediately after enrollment in the program, in some embodiments, patients may be administered a set of start-up CATI-modules, which may comprise a CMR interview as described above. As part of the CMR, TOAs can be used initially to optimize patients' medication regimen with respect to cost, safety, and convenience, resulting in a patient medication list and weekly dosing schedule. This information may then be used in the custom packaging process which involves packaging an initial supply of PMCs for a specified time period. A “starter” package is sent to patients consisting of the DDD, initial supply of PMCs, quick-start guide, and patient instructional DVD. The patient quick start guide may contain simple instructions and graphical illustrations of how to set-up/use the system and begin earning TIP points, while the DVD has a short video showing the different parts of the system in real world usage. A “starter” CATI-module is also available to pharmacy personnel for helping patients through the initial setup process as needed.
[0044] Once a patient account has been activated and the initial PMC loaded, the DDD is ready for use. When a dosing episode is scheduled, the device alerts patients and walks them through the dosing process as previously described. If dosing episodes are missed, the dispensing rules for upcoming episodes are adjusted accordingly based on the missed dose rules of all drugs included in the regimen, thereby making it possible to dispense double doses of individual drugs in subsequent dosing episodes as appropriate. To help facilitate advanced planning on the part of patients, LCD screen displays key information about the medication regimen on a regular basis, including time of next dosing episode, the number of remaining episodes available with the current PMC, and current TIP points. As patients use the device, adherence rates at the level of individual medications are calculated as described previously. When it is time for a PMC change, text/audio prompts guide patients through the process of swapping out the cartridges, with the barcode technology (or RFID, or similar) ultimately ensuring use of the correct cartridge and dispensing of only appropriate medication packets. PMCs with unused medication packets can be returned in supplied mailers for additional TIP points, while new PMCs are sent automatically to patients for refill purposes on a timely basis in accordance with their current prescriptions. Throughout the treatment, pharmacists administer CATI-modules as appropriate and update physicians and patients with treatment reports accordingly. Patients are also able to review their treatment reports and make changes to their regimen through access to their personal portal.
[0045] As such, those skilled in the art will appreciate that the conception, upon which this disclosure is based, may readily be utilized as a basis for the designing of other structures, methods and systems for carrying out the several purposes of the present invention. It is important, therefore, that the invention be regarded as including equivalent constructions to those described herein insofar as they do not depart from the spirit and scope of the present invention.
[0046] For example, the specific sequence of the described process may be altered so that certain processes are conducted in parallel or independent, with other processes, to the extent that the processes are not dependent upon each other. Thus, the specific order of steps and/or functions described herein is not to be considered implying a specific sequence of steps to perform the process. Other alterations or modifications of the above processes are also contemplated.
[0047] In addition, features illustrated or described as part of one embodiment can be used on other embodiments to yield a still further embodiment. Additionally, certain features may be interchanged with similar devices or features not mentioned yet which perform the same or similar functions. It is therefore intended that such modifications and variations are included within the totality of the present invention.
[0048] Although the present invention has been described and illustrated in the foregoing exemplary embodiments, it is understood that the present disclosure has been made only by way of example, and that numerous changes in the details of implementation of the invention may be made without departing from the spirit and scope of the invention. | A method, system and apparatus for medication therapy management programs. One embodiment of the invention includes a comprehensive, technology-enhanced pharmacy system for patients following a complex medication to regimen comprising a treatment database, communications interface, and a personal medication cartridge configured to store medication and configured based on a treatment optimization algorithm. Another embodiment of the invention includes a medication administration apparatus comprising computer processing hardware, a user interface, an interface for receiving a personal medication cartridge including medication dose packets labeled with computer-readable identification or an RFID mechanism, a medication ejection mechanism, and a medication dispensing sensor. The medication administration apparatus utilizes medication dose packets and prescription information and identifies individual dose packets using computer-readable information or an RFID mechanism. The medication administration apparatus determines the location and prescription schedule for each dose packet within the medication administration apparatus and provides an indication when a dosing event is scheduled. | 6 |
CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] The present application is a Continuation application under 35 U.S.C. 120 of commonly owned prior application Ser. No. 11/736,065, filed Dec. 15, 2003 in the name of Thomas Michael Guyette, now allowed.
FIELD OF THE INVENTION
[0002] The present invention relates generally to software development systems, and more specifically to increasing decision-making efficiency in large-scale software development projects.
BACKGROUND OF THE INVENTION
[0003] In software development communities made up of large numbers of software developers, it is frequently difficult to communicate relevant architectural decisions to developers at times when such information is needed. Specifically, when a developer is ready to develop or significantly modify a program code component, he or she needs immediate assistance in making myriad design decisions according to standards established for the project. Such assistance must either be sought by searching through a potentially large, unwieldy, and potentially out-of-date body of project documents, or from team leadership, who can be bottlenecks to getting an answer quickly. Existing systems for code management in the development process have not addressed this problem adequately.
[0004] A common example is the developer faced with choosing where to store persistent settings for “points of variability” (“POV data”), such as configuration values, application assembly values, and the like, for a component s/he is developing. Guidance on where and how to store POV data (and the “where-and-how” of other project standards) can be difficult to find, and when the system under development is relatively complex, there are often many different places to store such POV data. Although the design and development process gradually reveals what the POV for a component should be, making the right decision about where to store POV data is not always obvious.
[0005] Several undesirable consequences may result from this situation. First, different developers may each independently make their own determinations as to where POV data should be stored. This likely leads to a proliferation of disparate, disconnected data stores (e.g., separate text files, relational data stores, etc.) across the system. Second, developers may choose to use existing data stores that have inappropriate characteristics for the specific data to be stored. For example, a poorly chosen store might not be available to the component in certain use cases, or may not be translatable to all supported languages, etc. Developers could spend large amounts of development time learning the characteristics of all data stores just so they can make an informed decision about where to store the POV data for the components they develop.
[0006] None of these consequences are desirable, and each may result in bad design decisions that must be fixed and re-written, and, in the case where the product has already been shipped and installed in live production, migrated from one POV data store to another as storage decisions are re-made in newer versions of the product.
[0007] For the above reasons and others, it would be desirable to have a new system for software system development that provides a convenient way for developers to access “development guide” information reflecting architectural decisions about a system under development in a just-in-time fashion—that is, when they need such information to make specific design decisions about their component. Such a system would be applicable to providing convenient, clear, on-demand guidance in determining storage locations for storing POV data, and to making other component design decisions not related to POV data value storage.
SUMMARY OF THE INVENTION
[0008] To address the problems described above and others, a system and method are disclosed that provide an automated software process for acquiring, representing, and distributing information to software developers regarding software system architectural decisions. Using the disclosed system, a development team follows a series of well-defined steps to establish standards for implementation of components in the system. Information about project standards flows from the architects, who determine overall system characteristics and general component needs, into a profiling system that can later be used by developers to assist in making implementation decisions.
[0009] The disclosed system can be used to facilitate developer decisions regarding storage of operational characteristics, such as POV data, by a component under development, using consistent, deterministic project guidelines. During operation of the disclosed system, the POV needs of the component under development are “profiled” by obtaining answers to a series of questions relevant to the high level system design. For example, the flowchart of questions for a given POV data value may be presented to a developer within a graphical user interface (GUI) presented by the disclosed system. The collected answers to the questions lead the developer to a “node” that can be represented as an element in a category array having dimensions equal in number to the number of questions. For example, a decision tree with two questions, each having two possible answers, translates into a two-dimensional category array with four array elements; a decision tree with three questions, each having two possible answers, translates into a three-dimensional category array with eight array elements, etc. Each element of the category array represents a category of POV data, and contains one or more associated design guidelines. During operation of the disclosed system, a developer obtains the design guidelines appropriate for a given piece of POV data when the answers entered by the developer with regard to that POV data value are used to identify one of the elements in the category array. For example, a design guideline for one of the array elements in the category array may indicate that POV data with that element's characteristics should be stored in a text file on the local hard drive, while another array element may indicate the POV data should be stored using a reusable user preference storage component developed by the system team.
[0010] In order to set up and use the disclosed system in the context of developing a specific software system, a series of steps is followed. First, the technical leadership team for the project establishes high-level system design requirements. Next, based on these requirements, the technical leadership determines questions leading to design guidelines for categories of POV data of the system. The design guidelines may then be accessed by the developer, or automatically associated with a program component under development as indicated by the answers provided by a developer.
[0011] Thus there is disclosed a new system for software system development that provides a convenient way for developers to access information reflecting architectural decisions about a program. The disclosed system enables a developer to obtain design guidelines based on the system design when such information is needed during the development process. The disclosed system would further be applicable to providing convenient developer access to information relevant to determining storage locations for POV data of the system under development, such as configuration values.
BRIEF DESCRIPTION OF THE DRAWINGS
[0012] In order to facilitate a fuller understanding of the present invention, reference is now made to the appended drawings. These drawings should not be construed as limiting the present invention, but are intended to be exemplary only.
[0013] FIG. 1 is a block diagram illustrating a topology for a software system under development, shown as a distributed software application;
[0014] FIG. 2 is a flow chart diagram illustrating questions provided during operation of an embodiment of the disclosed system to obtain a profile for a POV of a system under development;
[0015] FIG. 3 is an illustration of a category array in an embodiment of the disclosed system; and
[0016] FIG. 4 is a flow chart diagram illustrating steps performed during operation of an embodiment of the disclosed system to determine an appropriate data store for a POV data value; and
[0017] FIG. 5 is a flow chart illustrating steps performed to use an embodiment of the disclosed system during the software system development process.
DETAILED DESCRIPTION OF EXEMPLARY EMBODIMENTS
[0018] Many software programs are designed for coordinated operation across multiple computer systems, and are sometimes described as “distributed” or “enterprise” programs or applications. FIG. 1 illustrates the execution environment of a client-server enterprise application program, for the purpose of describing how the disclosed system can be used to facilitate good software developer design decisions, in particular during development of such distributed software systems.
[0019] As shown in FIG. 1 , a software program under development may, for example, consist of an enterprise application program that can be accessed from, or executed on, multiple computer systems in a networked computer environment. As shown in FIG. 1 , an enterprise 10 includes a site A 50 having a server system 30 and associated client systems 32 , 34 , 36 , 38 and 40 , some of which may be shared among multiple users. A site B 52 is shown having a server system 12 and associated client systems 14 , 16 , 18 and 20 , and a server system 22 and associated client systems 24 , 26 and 28 . The server and client systems in FIG. 1 are connected through a communications network. The server and client systems of FIG. 1 may each, for example, include one or more processors and associated program code storage, such as program memory, as well as various input/output (I/O) devices or interfaces. A distributed software program may include components distributed among and executing on some or all of the server and client systems shown in the enterprise 10 . Accordingly, operational characteristics, such as, for example, POV data of a software program distributed across the server and client systems of the enterprise 10 , might similarly be distributed across such multiple, separate computer systems.
[0020] During development of a distributed software application operable across the systems shown in the enterprise 10 of FIG. 1 , software developers are faced with a variety of decisions regarding POV data of the software components they develop. For example, a developer may be faced with deciding where and/or how certain POV data, such as configuration values, application assembly values, and the like should be stored. Examples of configuration values in distributed programs include user buddy lists for chat applications, various user settings for word processing applications, individual user and shared lists or groups for electronic mail systems, and system configuration values defining security policies, resource allocation, and/or many other system configuration parameters.
[0021] As will be evident to those skilled in the art, individual POV data values may be user-related values relevant to some or all users, or system-related values relevant to some or all systems. For example, a given user POV data value may be relevant to all users, only users associated with one or more designated server or client systems, or relevant only to an individual user. Similarly, a system configuration value may be relevant to all server and client systems, only certain designated server or client systems, or only an to an individual client or server system. Accordingly, the data store for a POV should be selected in a way that is consistent with the attributes of that piece of POV data. When the software system under development is a distributed software application capable of having components executing on distributed server and client systems, such as those client and server systems shown in the enterprise 10 of FIG. 1 , multiple data stores may be defined for storage of configuration values. Such configuration value data stores may each be designed for storage of certain types or categories of configuration values within the system under development. The number of different data stores used for storing configuration values in a distributed software program operating across multiple client and server systems may be relatively large. Accordingly, a developer of a software component for a complex, distributed software program often faces a difficult task when determining the appropriate data store to be used for storing a given configuration value.
[0022] The disclosed system may be embodied to determine a data store in which a given POV data value should be stored for use by a distributed software component under development. The disclosed system issues a number of questions to a software developer regarding a specific piece of POV data that the developer is interested in determining a data store for. The answers provided by the developer to these questions result in a profile for the piece of POV data. The profile is used by the disclosed system to determine one or more design guidelines for the profiled piece of POV data. For example, in the case of a POV data value consisting of a configuration value, an embodiment of the disclosed system may be used to determine a design guideline consisting of an appropriate data store for the configuration value. In such an embodiment, the data store determined for the configuration value may include any specific type of data storage or data storage location for the configuration value, including but not limited to, any specific type or location of one or more data structures, such as files, databases, text documents, etc. Moreover, an embodiment of the disclosed system may operate to provide design guidelines for storing configuration values in different categories within a shared data store by associating meta-data tags with the configuration values. In this context, the term “meta-data” is used to refer to any specific type of data used to describe the properties of other data. In this case, the meta-data is used to describe and distinguish one or more categories of configuration values sharing a common data store.
[0023] FIG. 2 illustrates a flow of questions provided by an embodiment of the disclosed system to determine a profile for an POV data value consisting of a configuration value. The questions described by the FIG. 2 flow may be provided through any appropriate graphical user interface (GUI) on a user computer system. Similarly, the answers to the questions described by the FIG. 2 flow may be obtained through any appropriate graphical user interface. Those skilled in the art will recognize that the order of the questions in FIG. 2 is for purposes of explanation only, and that any question order may used. Similarly, the specific questions in FIG. 2 are also given only for purposes of explanation, and the specific questions provided in different embodiments may vary, depending on the overall requirements and system design of the system under development.
[0024] At step 70 of the embodiment shown in FIG. 2 , the disclosed system displays a question to the user as to whether the configuration value is to be maintained as the same value for all users of the system under development, or as a different value for each user. The disclosed system captures the answer provided by the user to the question of step 70 , and at step 72 displays a question to the user as to whether the configuration value is to be maintained as the same value for all locations over which the system under development is deployed, or is to be maintained separately in each location. After capturing the answer to the question of step 72 , the disclosed system displays a question at step 73 to determine who is to be allowed to read the configuration value. The answer to the question of step 73 is then captured, and the disclosed system displays a question at step 74 to determine who is to be permitted to read the configuration value, and captures the answer to that question. The disclosed system then operates to display a question to determine whether the configuration value is to be editable at step 75 , and captures the answer to that question. Thus, as shown for purposes of explanation in FIG. 2 , the disclosed system may be embodied to determine whether a given POV data value is the same for all users or different for each user, whether the POV data value is the same in all locations or different for different locations, which users are permitted to read and/or edit the POV data value, and whether the POV data value should be modifiable at development time, installation time, and/or runtime. Questions provided by the disclosed system, such as those shown for purposes of explanation in FIG. 2 , are system-specific, and determined by technical leadership.
[0025] After capturing the user's answers to a set of profiling questions relating to a POV data value of the system under development, such as the questions shown in the flow of FIG. 2 , the disclosed system accesses an entry in a category array determined by those answers. The category array has a number of dimensions dependent on the number of possible answers to the set of profiling questions. For example, the number of entries in the category array may equal the set of possible answer combinations to the profiling questions. In a case where the set of profiling questions for an implementation includes two questions, each of which may be answered by “True” or “False,” the number of entries in the category array would be four. Such a category array 80 is shown for purposes of explanation in FIG. 3 . The two questions in the set of profiling questions for the category array 80 of FIG. 3 are the questions associated with steps 70 and 72 of FIG. 2 .
[0026] The category array 80 includes a first entry 82 associated with a category of configuration values that are the same for all users, and the same for all locations in the system under development. A second entry 84 is associated with a category of configuration values that are different for each user, but are the same for each location. The entry 86 is associated with a category of configuration values that are the same for each user, but are different for each location, and the entry 88 is associated with a category of configuration values that are the different for each user and different for each location. Each of the entries in the category array 80 of FIG. 3 are associated with one or more design guidelines to be provided to a user with regard to a POV data value that maps to that entry. For example, in the case where the POV data value is a configuration value, each of the entries in the category array 80 may be associated with a separate data store for storing configuration values, or with meta-data to identify different categories of configuration values stored within a shared data store. The four entry category array 80 of FIG. 3 is shown for purposes of illustration only, and an embodiment of the disclosed system may have a category array having any appropriate number of entries to reflect the specific set of profiling questions for that embodiment. In any event, after the user has answered the set of profiling questions, the POV data value in question is associated by the disclosed system with one and only one of the entries in the category array.
[0027] FIG. 4 is a flow chart illustrating steps performed by an embodiment of the disclosed system to process the answers to profiling questions. The flow of FIG. 4 is responsive to answers input to the disclosed system for the profiling questions 70 and 72 of FIG. 2 . After starting at step 90 , the disclosed system operates at step 92 to determine whether the POV data value is the same for all users of the system under development. If not, step 92 is followed by step 96 , in which the disclosed system operates to determine whether the POV data value is the same for all locations at which the system is deployed. If not, then a branch of the flow terminates with a display of design guideline 104 , consisting of an indication of a Data Store D: User-specific local store. If at step 96 the disclosed system determines that the POV data value is the same at all locations, then the branch of the flow terminates with a display of design guideline 102 , consisting of an indication of Data Store C: User-specific replicated store.
[0028] If the disclosed system determines at step 92 that the POV data value is the same for all users, then step 92 is followed by step 94 , in which the disclosed system operates to determine whether the POV data value is the same for all locations in which the system under development may be deployed. If not, then the flow terminates with a display of the design guideline 100 , shown as an indication of the Data Store B: Shared local store. If at step 94 the disclosed system determines that the POV data value is the same for all locations, then the flow terminates with a display of the design guideline 98 , shown as an indication of the Data Store A: Shared replicated store.
[0029] Thus the flow chart of FIG. 4 represents a flow of answers to the profiling questions of an embodiment of the disclosed system, and the terminating nodes of the flow chart in FIG. 4 represent respective entries within the category array. The disclosed system may operate to display the design guideline associated with the appropriate entry for an POV data value, or may operate to automatically associate the POV data value with the selected design guideline. Accordingly, in the illustrative embodiment, each design guideline associated with one of the terminating nodes of the flow chart in FIG. 4 may include either: 1) meta-data that is used to tag the POV data value, such as, for example an access control list, 2) an indication or name for a separate data store, and/or 3 ) code that may be output for use by the programmer.
[0030] FIG. 5 is a flow chart showing steps of a method for using an embodiment of the disclosed system in the process of developing a distributed software system. The process shown in FIG. 5 illustrates a preferred order of steps to be performed, and requires the users of the disclosed system to give explicit thought to the profiling questions, category array, and profiling flow, in order to insure maximum efficiency of designing and developing a configurable distributed system.
[0031] As shown in FIG. 5 , at step 120 , a technical leadership team for a software development project establishes high-level system design requirements for security, location distributivity, etc. At step 122 , the technical leadership team uses the system design determined at step 120 to determine needs for different types of configuration data storage. At step 124 , the technical leadership team defines the list of dimensions for the category array, and at step 126 , re-tools the category array into a code flow representation. Next, at step 128 , the technical leadership team “caps” the end of each code flow branch in the flow determined at step 126 with a node containing a design guideline, such as a description of where and how a configuration value matching the profile question answers represented by that flow branch should be stored. A configuration system development team then creates components at step 130 representing the data store indications in the design guidelines defined at step 128 . These components created at step 130 are then usable by other developers to store configuration data in an appropriate place.
[0032] At step 132 developers develop their software components using temporary data storage locations for the necessary POV data values, in this case configuration values, such as text files, as “rough drafts” of such components, until the configuration system team finishes developing the configuration subsystem having the data stores associated with the design guidelines in the entries of the category array. When the developers are ready to integrate their components into the overall system being developed, they use the disclosed system to traverse the flow for each temporarily stored POV data value at step 134 , and the displayed results of using the disclosed system for such a traversal informs them where and how to store the configuration value of interest at step 136 .
[0033] Developers may also have a need for further division of configuration value storage, (i.e., for adding another dimension to the category array). In these cases, the developer approaches the configuration subsystem team to re-work the configuration design to meet their needs. Developers use the configuration systems provided to store their configuration data, and remove their “rough draft” storage code. The disclosed system, as illustrated in FIG. 5 , thus assists developers in making important design decisions.
[0034] FIGS. 2 , 4 and 5 are flowchart illustrations of methods, apparatus (systems) and computer program products according to an embodiment of the invention. It will be understood that each block of the flowchart illustrations, and combinations of blocks in the flowchart illustrations, can be implemented by computer program instructions. These computer program instructions may be loaded onto a computer or other programmable data processing apparatus to produce a machine, such that the instructions which execute on the computer or other programmable data processing apparatus create means for implementing the functions specified in the flowchart block or blocks. These computer program instructions may also be stored in a computer-readable memory that can direct a computer or other programmable data processing apparatus to function in a particular manner, such that the instructions stored in the computer-readable memory produce an article of manufacture including instruction means which implement the function specified in the flowchart block or blocks. The computer program instructions may also be loaded onto a computer or other programmable data processing apparatus to cause a series of operational steps to be performed on the computer or other programmable apparatus to produce a computer implemented process such that the instructions which execute on the computer or other programmable apparatus provide steps for implementing the functions specified in the flowchart block or blocks.
[0035] Those skilled in the art should readily appreciate that programs defining the functions of the present invention can be delivered to a computer in many forms; including, but not limited to: (a) information permanently stored on non-writable storage media (e.g. read only memory devices within a computer such as ROM or CD-ROM disks readable by a computer I/O attachment); (b) information alterably stored on writable storage media (e.g. floppy disks and hard drives); or (c) information conveyed to a computer through communication media for example using baseband signaling or broadband signaling techniques, including carrier wave signaling techniques, such as over computer or telephone networks via a modem.
[0036] While the invention is described through the above exemplary embodiments, it will be understood by those of ordinary skill in the art that modification to and variation of the illustrated embodiments may be made without departing from the inventive concepts herein disclosed. Moreover, while the preferred embodiments are described in connection with various illustrative program command structures, one skilled in the art will recognize that the system may be embodied using a variety of specific command structures. Accordingly, the invention should not be viewed as limited except by the scope and spirit of the appended claims. | An automated software process for acquiring and distributing information regarding design guidelines relevant to developers of a software system. The system supports developer decisions regarding design guidelines for operational characteristics, such as “points of variability” (POV), of a system under development. Operational characteristics of the system under development are “profiled” through answers to questions reflecting the high level system design. The collected answers indicate a category of operational characteristics associated with a design guideline. A developer obtains the design guidelines appropriate for a given operational characteristic when the answers entered by the developer with regard to that operational characteristic are used to determine one of the elements in the category array. Technical leadership establishes a high-level system design, and determines questions leading to design guidelines for categories of operational characteristics of the system. The design guidelines may then be conveniently accessed by the developer. | 6 |
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates generally to devices which protect vehicle components that are vulnerable to falling rocks and road debris.
2. Description of Related Art
Various covers for vehicle components have been developed in the past. Vehicle fenders and skid plates are examples of devices that are designed to protect the vehicle body and key components such as the engine and transmission.
Commercial vehicles, particularly rock trucks, are highly vulnerable to falling rocks and earth that are dropped by the excavators of inloaders onto the bed of the vehicle. Typically, the excavator of an inloader scoops up rocks or dirt. The excavator is then swung toward the bed of a rock truck and its contents are released onto the bed. However, during this motion, many rocks fall out of the excavator, missing the bed of the truck. These falling rocks can weigh in excess of ten tons and can seriously damage unprotected vehicle components.
Specifically, the rear axle housing and its proximate components, which may include the oil filter housing and differential sight glass, are susceptible to damage by rocks that are dropped on or near the truck bed. Such components are not heavily protected and they can easily be damaged.
In addition, vehicles, including rock trucks, that are driven on rocky terrains are also vulnerable to damage from road debris. Even lighter debris, such as soil and sand, tends to be "sandblasted" toward the rear of the vehicle, contributing to the general deterioration of these parts.
Debris in the form of large rocks will not only crush lightly protected vehicle components but also dent, crack or warp even the more heavily constructed rear axle housing, causing damage to the axle and differential unit.
Hence, the rear components of the vehicle, including the axle housing and its proximate components, must be frequently cleaned and inspected for damage to properly maintain the vehicle. Any damage to the axle and its proximate components will most certainly add to the cost of maintaining the vehicle.
Accordingly, a need will be seen for a protective device that can shield the axle housing and its proximate components from falling rocks and road debris. In addition, there is a need for a device as described above that is easily mountable and removable (for quick inspection of components and cleanup) and economical to produce.
U.S. Pat. No. 4,813,507 issued to Tanaka et al. on Mar. 21, 1989 describes an axle beam with a protective member designed to prevent deformation of the axle beam. Holes are drilled into the axle beam to accommodate bolts that secure the protective member onto the axle beam. The purpose of the protective member is to deflect or divert the force of impact away from the axle beam by acting as a skid plate. Only one face of the axle is protected and no measures are taken to prevent small dirt particles from flying toward and accumulating onto the axle beam. Further, once installed, the protective member cannot be easily removed to allow for the inspection and cleanup of the axle beam. More importantly, the device cannot protect components from falling rocks.
U.S. Pat. No. 4,044,444 issued to Nobutomo et al. on Jan. 18, 1977 describes a construction that welds a brake case cover, a rear wheel axle case and terminal speed reduction case, to avoid more expensive casting methods of manufacture. It discloses the welding of a fender onto the rear wheel axle housing. A fender attached in this manner cannot adequately prevent debris kicked by the vehicle's tires from damaging the rear axle housing and its proximate components. This device is too lightly constructed to prevent vehicle damage by falling rocks.
U.S. Pat. No. 1,572,460 issued to Banschbach on Feb. 1, 1926 describes an automobile fender and guard combination. The main object of this invention is to ward off damage from accidents or collisions. This device does not provide for a specific guard for the rear axle housing. The rear axle is not protected from road debris. The disclosed extension of the rear bumper, close to the ground, will tend to trap road debris and ricochet some of the debris toward the rear axle housing. This device cannot adequately protect vehicle components from falling debris.
U.S. Pat. No. 4,339,016 issued to Gerresheim on Jul. 13, 1982 describes a tiltable fender for a tractor loader. The fender is tiltable laterally outwardly and downwardly to facilitate easier access to the engine compartment. This device does not adequately protect the axle or its proximate components from falling rocks or road debris.
U.S. Pat. No. 2,769,503 issued to Wagner on Nov. 6, 1956 describes a pivotally mounted fender for cab-over-engine vehicles. The fenders are hinged on one end to the body and can be swung outwardly for easier access to the engine. This device cannot adequately protect vehicle components from falling rocks or road debris.
None of the above noted inventions and patents, taken either singly or in combination, is seen to describe the instant invention as claimed.
SUMMARY OF THE INVENTION
The present invention is a guard for protecting the axle housing and proximate components of a vehicle from falling rocks and road debris. The device has a central mount that attaches onto the differential unit portion of the axle housing. The mount partially protects the differential unit. In addition, at least two shields are hinged onto the central mount to allow the shields to be swung from an open position to a protective position for use during travel by the vehicle. The shields cover the segments of the exposed axle housing and the shields can be locked into place while in the protective position. The shields can be unlocked and swung into the open position to allow for inspection, maintenance, and cleanup of the axle housing and its proximate components.
Accordingly, it is a principal object of the present invention to provide a guard for vehicles which effectively shields substantial portions of the axle housing and its proximate components from falling rocks and road debris.
Another of the objects of the present invention is to provide a guard for vehicles which is easily mounted onto the vehicle.
Yet another of the objects of the present invention is to provide a guard for vehicles, parts of which are readily removable to permit easy access to the axle case and its proximate components.
Still another of the objects of the present invention is to provide a guard for vehicles which is economical to produce.
A further object of the present invention is to provide a guard for vehicles which can easily be secured to the vehicle.
An additional object of the present invention is to provide a guard for vehicles which includes attachments on the vehicle for the rear guard to attach.
A final object of the present invention is to provide a guard for vehicles which includes shields that can be independently opened and closed while the guard is still mounted to the vehicle.
These and other objects will more readily appear as the nature of the invention is herein after more fully described, illustrated and claimed with reference being made to the attached drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is an end view of the guard attached near the rear axle housing of a rock truck.
FIG. 2 is a plan view of the guard shown in FIG. 1.
FIG. 3 is a plan view of the guard shown in FIG. 1 with the left and right shields in partially open positions.
FIG. 4 is an environmental view of the guard attached near the rear axle of a rock truck.
FIG. 5 is a side elevational view of the guard attached onto the safety latch housing and shock housing of a truck.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
The device of the applicant's invention effectively protects substantial portions of the rear axle housing of vehicles and key components, including the oil filter housing and differential sight glass, as well as segments of various cables, hydraulic lines, etc. that are positioned proximate to the axle housing. The invention requires few moving components and it is highly durable and economical to produce.
Embodiments of the aspects of the present invention will now be explained with reference to the accompanying drawings. By way of illustration and not limitation, FIGS. 1 to 5 are presented to show the preferred embodiments of the applicant's invention.
FIG. 4 is an environmental perspective view of a guard 2 attached to a heavy truck, preferably a rock truck as shown. The end view of a rock truck is shown in FIG. 1 with the guard 2 fixedly attached onto a pre-existing safety latch housing 10 (see plan views of the present invention in FIGS. 2 and 3). The safety latch housing 10 protrudes generally horizontally from the center-portion of the axle housing 30 toward the rear of the vehicle. The safety latch housing comprises a pair of parallel eyes spaced apart to define a horizontal passage (not shown) into which the guard 2 seats, each eye including a receiving aperture 11 (a vertical channel) . During normal truck operations, the safety latch housing 10 is intended to receive cables (not shown) that are attached to the truck bed 56. A latch locking means 32 (a modified pin) is provided for insertion into the receiving aperture 11 to hold the cables which secure the bed 56 to the truck axle.
The guard employs the safety latch housing 10 as a mounting support. The guard includes a center mount 8 which includes a slide-in member 70 (a tang) with a receiving aperture (not shown), the tang cooperating with the safety latch housing 10 so that the receiving aperture aligns in registry with the receiving aperture of each eye of the safety latch housing 10 while the tang resides in the horizontal passage. The latch locking means 32 can therefore be inserted through the receiving aperture (not shown) of the slide-in member 70 to secure the center mount 8 to the safety latch housing 10.
The guard includes a pair of shields 6a and 6b that are hinged onto the center mount 8 by hinging mechanisms 18a and 18b. It is preferred that a standard hinge known in the art and shown in FIG. 1 is utilized in the present invention. The hinging mechanisms 18a,18b allow each shield 6a,6b to be swung from an open position to a protective position for use during vehicle movement or when rocks and earth are dropped onto the bed of the vehicle. The shields are dimensioned and configured in a squared-C shape to cover the segments of the exposed axle housing and hinged to rotate horizontally towards the longitudinal centerline of the truck, enabling quick inspection, cleanup and repair of axle components.
To prevent the movement of the shields while in a protective position, a pair of mounting brackets 12a and 12b (see FIGS. 2 and 3) secure each one of the shields to a different one of each of the shock housings 26a,26b of the vehicle. The mounting brackets 12a,12b are attached to the pair of shock housings 26a and 26b preferably by arc welding. The mounting brackets 12a,12b include a hole which is positioned in registry with a corresponding shield opening (7a or 7b) of the shields 6a and 6b. Threaded bolts, 20a and 20b, are provided to secure each of the shields to the mounting bracket 12a, 12b. The bolt is passed through both the shield opening 7a,7b and the hole of the mounting bracket 12a,12b and secured with a matingly threaded nut, 58a and 58b, threaded onto its respective bolt 20a,20b, thereby tightening the bolt, shield and nut assembly to the mounting bracket.
When the shields 6a and 6b are locked into place, lateral end segments 50a and 50b of the axle housing 30 and its proximate components, including an oil filter housing 16, differential sight glass 28, and covered segments of various lines, cables, etc. 52 are effectively protected from most debris and falling rocks.
FIG. 2 shows a plan view of the guard 2 that is secured onto the safety latch housing 10 and mounting brackets 12a and 12b. The first shield 6a includes a contoured portion 7 defining a recess that matches the outer oval shape of the oil filter housing 16. The shield 6a therefore effectively protects the most vulnerable portions of the oil filter housing 16 without need for alteration of the axle component. It is preferred that the applicant's invention is shaped to custom-fit around the components that need protection.
FIG. 3 shows a plan view of the guard 2 with the bolts 20a and 20b detached from their respective mounting brackets 12a and 12b, and corresponding nuts 58a and 58b. In FIG. 3, the shields 6a and 6b are shown partially swung outward toward the rear of the vehicle. These types of shield movements allow for the quick inspection, maintenance and cleanup of the components that are enclosed by the guard 2.
FIG. 5 is an elevated side view of the guard attached to the left shock housing 26a and safety latch housing 10 of the rock truck in FIG. 4. A left contoured edge 22 is preferably welded onto the shield 6a to reinforce the overall structure. The contoured edge 22 is tailored to prevent lateral penetration of debris into the guard toward the axle housing 30, since the edge 22 matches the rounded face of the shock housing 26a. One such customized edge is substantially a half-moon design. Likewise, the right edge (not shown) of shield 6b is comparably made.
In terms of manufacture, metal plates, preferably steel, are cut and welded to form the guard 2. In another embodiment, components of the guard 2 are shaped by using specialized metal plate bending machines that are known to persons skilled in the art, to substantially reduce the number of welds that are necessary to make the guard 2. Hinge means 18a and 18b are derived from designs that are known to persons skilled in the art.
It is to be understood that the present invention is not limited to the embodiments described above, but encompasses any and all embodiments within the scope of the following claims. | A guard for vehicles protects the axle housing and proximate components from falling rocks and road debris. The device has a central mount that attaches onto the differential unit portion of the axle housing. The mount partially protects the differential unit. In addition, at least two shields are hinged onto the central mount. The shields can cover the segments of the exposed axle housing and said shields can be locked into place. The shields can be unlocked and swung from the central mount to allow for inspection, maintenance, and cleanup of the axle housing and its proximate components. | 1 |
BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention relates to digital signal processing; and, in particular, this invention relates to equalization and demodulation of signals which are modulated with a repetitive component.
2. Discussion of the Related Art
In many applications involving digital signals (i.e. signals which are sampled at discrete times), the transmitted signals are digitally modulated. Often, digital modulation results in a signal ("structured signal") which is not completely random but has some repetitive structure. For example, under a time-division multiplexing (TDM) protocol, multiple data streams ("tributary data streams") are interleaved to form a signal having a repetitive structure. Such a signal is typically divided into frames consisting of a number of time slots each assigned to a tributary data stream for transmission of its data. Usually, one or more markers ("fixed bits") are placed at predetermined time slots of a frame for synchronization. Often, multiple frames in turn form a "superframe", which is an even larger repetitive unit of the transmitted signal. Synchronization between the recipient and the signal transmitter is further enhanced by additional markers placed at predetermined time slots to demarcate the superframe. In addition, in a typical TDM signal, training sequences are periodically inserted at for synchronization of baud and carrier signals at the receiver, and for equalization adaptation. Hence, a number of inserted bit sequences form repetitive components in the TDM signal. In addition, if a tributary data stream is self-correlated, the resulting time-multiplexed signal will be periodically correlated.
A channel or transmission medium can impose distortion upon a signal transmitted through it. For example, in a crowded communications environment, signals can interfere with each other. In a mobile communications system, a signal may arrive at a receiving point via multiple paths at different times, leading to multipath distortions. These and other distortions can cause errors in demodulating the signal, leading to errors in recovering the transmitted symbols at the receiver. To mitigate the distortions in the channel, an adaptive equalizing filter ("adaptive equalizer") is often applied to the received signal. In such an adaptive equalizer, the weights of the filter adapt to the changing characteristics of the channel. 1 One class of adaptive equalizers is collectively known as adaptive linear equalizers 2 .
FIG. 1 is a block diagram representing the signal equalization and demodulation system 100 in a receiver. As shown in FIG. 1, a received signal is demodulated by element 101 to a base band signal by removing the carrier frequency f c . The base band signal is then sampled by sampling device 102, at either the symbol interval, or a fraction of the symbol interval. In many systems, a tracking device 103 is provided to maintain sampling at a proper phase of the base band signal, The samples of the base band signal are then provided to an adaptive linear equalizer 110, represented in FIG. 1 by filter 105, error means 108 and filter weight update means 107. (When the base band signal is sampled at the symbol interval, the equalizer is known as a "T-spaced equalizer". Otherwise, i.e. when the base band signal is sampled at a fraction of the symbol interval, the equalizer is known as a "fractionally spaced equalizer".)
Generally, in an adaptive linear equalizer, such as adaptive linear equalizer 110, a finite transversal filter 105 computes a weighted sum of a number samples of the base band signal. This weighted sum is then provided to a decision device 106 to determine the symbol received (the "symbol decision"). In one type of equalizer, which is shown in FIG. 1, the decision device 106 provides a feedback signal to adaptively modify the weights of finite transversal filter 105. Such an equalizer is known as a "decision-directed", or "blind", equalizer.
As shown in FIG. 1, a phase-corrected output value 121 of transversal filter 105 and the symbol decision 122 of decision device 106 are fed back to error means 108 to generate an error signal 120. In FIG. 1, phase correction in the output value 121 of transversal filter 105 is provided by circuit 109, which compares the phases of the symbol decision 122 and the output value 123 of transversal filter 105 to detect any residual carrier-tracking phase error. The error signal 120 generated by error means 108 represents, assuming that the data symbol is correctly recovered, both amplitude and phase errors in the phase-corrected output value 121 of finite transversal filter 105. When a training sequence of data symbols is available, error signal 120 is generated by computing, at each time point, a complex difference between the phase-corrected sample 121 of the equalizing digital filter and the expected corresponding data symbol in the training sequence. Error signal 120 is fed into filter weight update means 107 to modify the weights of finite transversal filter 105. In FIG. 1, the phase error detected by phase correction device 109 is reintroduced into error signal 120, which is then provided to filter weight update means 107.
The feedback signal received by filter weight update means 107 can also be obtained by biasing ("respinning") symbol decision device 106 by the phase error and computing the complex difference between the respun symbol decision and the output value 123 of transversal filter 105.
Several algorithms exist to generate adaptively the weights of an adaptive linear equalizer. One common method is the least-mean-square (LMS) algorithm, first described by R. W. Lucky et al ("Lucky's LMS algorithm"). An overview of Lucky's LMS algorithm can be found in "Adaptive Equalization," by Shahid Qureshi, published in IEEE Communications Magazine, March, 1982, pp. 9-16. Improvements based on Lucky's LMS algorithm include (i) the recursive least squares (RLS) methods, such as those described in "Application of Fast Kalman Estimation to Adaptive Equalization," by D. D. Falconer and L. Ljung in IEEE Transactions of Communications, Vol. Com-26, No. 10, October 1978, pp. 1439-45; and (ii) the adaptive lattice methods, such as those described in "Lattice Filters for Adaptive Processing," by B. Friedlander in Proceedings of the IEEE, Vol. 70, No. 8, August 1982, pp. 829-67. These improvements are designed to converge more rapidly than Lucky's LMS algorithm. Other improvements upon Lucky's LMS method include methods which adjust the weights of the equalizing digital filter to optimize a characteristic of the desired signal. One example of such methods is the dispersion-directed method described in "Self-recovering Equalization and Carrier Tracking in Two-dimensional Data Communication Systems," by D. Godard, IEEE Transactions on Communications, Vol. Com-28, No. 11, November 1980, pp. 1867-75.
Another architecture for adaptive linear equalization is the decision feedback equalizer (DFE). The DFE equalizer architecture consists of both a forward digital filter, which computes a weighted sum of input samples, similar to those based on Lucky's LMS described above, and a feedback digital filter which computes a weighted sum of data symbols determined in previous symbol decisions. In a DFE equalizer, the numbers of coefficients in the forward and feedback filters can be different. The decision process is applied to the sum of the output values of the forward and backward equalization filters to generate a symbol. As in all adaptive equalizers, an error signal is provided to update the filter weights and to improve filter performance.
Yet another adaptive equalization method, which uses an artificial neural network (ANN), is described by S. Siu, G. J. Gibson and C. F. N. Cowan in "Decision Feedback Equalizer Using Neural Network Structures," IEE Proceedings, 137(4): 221-5, 1990. In the ANN method, the signal samples are sequentially provided as input; samples into each ANN processing unit of a first layer of a neural network. The output samples of the first layer's processing units are then provided as input samples into each processing unit of a second layer of the ANN. The output samples of the processing units in this second layer are then provided as input samples into a single output processing unit. A decision process is then applied to each output sample of the output processing unit to generate a symbol. In this ANN, each processing unit consists of a finite transversal filter with adjustable weights, and a nonlinear functional operator which operates on the output sample of the finite transversal filter. The filter weights of the transversal filter are computed during the processing of a training sequence. The error signal for the ANN is obtained by subtracting from each data symbol of a training sequence from the corresponding data symbol output of the output processing unit. A back propagation algorithm is used to generate new coefficients for each processing unit. The ANN architecture can also incorporate feedback using previously decided symbols to become a decision feedback ANN architecture.
Each of the methods discussed above in the prior art processes sequential signal samples to generate, for each iteration, one output symbol and an error signal. The error signal is used in an updating procedure for filter weights to adaptively modify the transversal filters of the equalizer for the next iteration. The equalizer, with the updated filter weights, is then used to generate the next symbol. The process continues until all symbols are decoded one by one.
The methods used in the prior art assume that the symbols in the input data are random. However, when the input signal is a structured signal, i.e. the signal includes a periodic component, the filter adaptation process generates transversal filter weights that are skewed by the periodic component. Consequently, the periodic component of the input signal is amplified while the aperiodic component of the input signal is attenuated. Recalling that, in a structured signal such as a TDM signal, the periodic component is substantially an artifact of the signal protocol, e.g. the framing structure, and often does not relate to the tributary data being transmitted, the amplification of the periodic component is therefore undesirable. Thus, to enhance the performance of a prior art method operating on a signal with a periodic component, one approach requires the signal to be randomized prior to transmission and derandomized at the receiver after equalization. The additional costs of the randomization and derandomization steps add to system cost, complexity, and processing time.
Another approach taken in the prior art to overcome the overweighting of the periodic components of a signal uses an equalizing filter comprising a tapped delay line which takes into account only signal samples spanning a time period shorter than the period of the framing information. However, this approach reduces the frequency resolution of the equalizer and handicaps the equalizing filter's ability to excise signal interference and multipath effects.
Yet another prior art approach prevents further updates to filter weights after the filter has converged to some useful value, but prior to the time the filter weights begin to destroy the aperiodic or "random" data. However, this approach also reduces the equalizer's capability to reject interference and to compensate for distortion.
SUMMARY OF THE INVENTION
In accordance with the present invention, a method and a structure for equalizing and demodulating a structured signal are provided. The structured signal consists of a number of symbols transmitted in a frame. The structure of the present invention comprises a processor for each symbol position in the frame. Each processor comprises a transversal digital filter, which computes a weighted sum of a predetermined number of samples of said structured signal to provide an equalized sample. The equalized sample is used by a decision device to determine the symbol transmitted at the symbol position in the frame.
In one embodiment, each processor includes a single adaptive transversal filter, in which weights are updated according to the error between the equalized sample and the symbol decision. In such an embodiment, an adaptive linear equalization algorithm can be applied. A phase error correction device, which corrects phase errors by comparing the phase of a symbol decision with the phase of an equalized sample of the multiple filter equalizer, can also be provided.
In another embodiment, each processor is provided with more than one transversal filter in a first level structure, which also includes a plurality of non-linear operators each operating on an output value of a corresponding one of the transversal filters. Each of the non-linear operators of the first level structure provides an equalized output value, which is used by a corresponding transversal digital filter in a second level structure to compute an equalized sample. Each output value of this second level structure is provided to a decision device for a symbol decision. The weights in the transversal filters of this multiple level structure can be updated in accordance with a backpropagation algorithm.
The present invention avoids overemphasis of the periodic component of a structured signal by using a processor for equalization and demodulation of each symbol in a frame. The processors can run concurrently and are each tailored to generate a symbol at a specified symbol position in a frame of the structured signal. Since each symbol position, which may correspond to a tributary data stream in a time division multiplexed (TDM) signal, has a distinct equalization processor, the resulting composite signal can be tailored by each these processors to avoid emphasis of a periodic component. Consequently, convergence of filter weights under an adaptive algorithm is not affected by the periodic component of the structured signal. Each processor can also include transversal filters spanning an appropriate number of signal samples to mitigate channel effects and to converge to a set of optimum coefficients or weights. Because the transversal filters are configured to reflect the structure of the signal, interfering signals collocated in the signal band can be suppressed. The coefficients of the individual transversal filter converge to values which minimize the bit-error-rate of the demodulated information symbols.
The present invention is better understood upon consideration of the detailed description below and the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a block diagram showing demodulation and decision-directed equalization of a signal at a receiver, in accordance with prior art methods.
FIG. 2 is a data representation of a structured signal having frames and superframes.
FIG. 3 shows four transversal filters 301a-301d under the equalization methods of the present invention.
FIG. 4 shows a processor 400 of an equalizer in a "single layer architecture" embodiment of the present invention.
FIG. 5 shows a processor 500 of an equalizer in a "multiple layer architecture" embodiment of the present invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
The present invention provides a method for equalizing and symbol demodulating a structured signal, e.g. a time-division multiplexed (TDM) signal. A TDM signal can be modulated by any of a number of modulation schemes, such as phase shift key (PSK), frequency shift key (FSK), or quadrature amplitude modulation (QAM). One of ordinary skill will appreciate from the following discussion that the present invention is not limited by the modulation scheme used.
FIG. 2 shows a two-dimensional representation of data in a structured signal over a time period of four superframes. In FIG. 2, each square represents a data sample, and each row of squares represents the samples of a frame, and each superframe consists of four frames transmitted successively in time. The data are sampled either at symbol interval (i.e. each sample representing a symbol), or at a fraction of the symbol interval (i.e. a number of samples together representing a symbol). As shown in FIG. 2, each frame is aligned in time with each other, so that a vertical column in FIG. 2 consists of samples in corresponding positions in the frames shown. Thus, for example, sample 101 represents the nth sample of frame number 1, and sample 102 represents the nth sample in frame number m. Of course, the number of samples in a frame and the number of frames in a superframe shown in FIG. 2 are merely illustrative. The present invention is applicable to any framing structure.
The present invention provides an equalizer comprising, for each data symbol position in a frame, a "processor", which includes a transversal filter and means for adaptively updating the transversal filter. The transversal filter geometry can be described using the data representation of FIG. 2. In general, the filters can be noncausal. Filter samples separated by integral number of frames compensate for noise in the tributary data stream and avoid artifacts due to the frame structure, the superframe structure, or both. On the other hand, filtering adjacent samples ("horizontal samples") compensates for channel effects, including intersymbol interference and multipath interference.
Four examples of transversal digital filters 301a-301d of the present invention are shown in FIG. 3. In FIG. 3, in each filter, the shaded square represents the expected position in a frame of the filter's output data value. For example, filter 301a computes a weighted sum of five samples, for the sample positioned at the center of these five samples. Filter 301a has the following system function (in Z-transform notation):
H(z)=a.sub.-2 Z.sup.-2 +a.sub.-1 Z.sup.-1 +a.sub.0 Z.sup.0 +a.sub.1 Z.sup.1 +a.sub.2 Z.sup.2
Alternatively, Filter 301b, which computes a weighted sum of corresponding samples over five frames, has the system function:
H(z)=a.sub.-2N Z.sup.-2N +a.sub.-N Z.sup.-N +a.sub.0 Z.sup.0 +a.sub.N Z.sup.N +a.sub.2N Z.sup.2N
where N is the number of samples in a frame.
Another variation of a transversal filter of the present invention is given by filter 301c, which computes a weighted sum of data corresponding samples separated by an integral multiple of frames. Filter 301c has the system function:
H(z)=a.sub.-pN Z.sup.-pN +a.sub.0 Z.sup.0 +a.sub.pN Z.sup.pN
where p and N are, respectively, the number of frames separating the corresponding samples and the number of samples in a frame.
Filter 301d is a filter which takes into account samples both proximate in time and occupying corresponding data sample positions spanning a number of frames. Filter 301d has the system function:
H(z)=a.sub.-pN Z.sup.-pN +a.sub.-N Z.sup.-N +a.sub.-2 Z.sup.-2 +a.sub.-1 Z.sup.-1 +a.sub.0 Z.sup.0 +a.sub.1 Z.sup.1 +a.sub.2 Z.sup.2 +a.sub.N Z.sup.N +a.sub.pN Z.sup.pN
where p and N are as defined above with respect to filter 301c.
Although the filters shown in FIG. 3 give non-zero weights to samples located symmetrically about the output symbol position, such symmetry is not required by the present invention.
FIG. 4 shows a processor 400 of an equalizer in one embodiment of the present invention. The embodiment shown in FIG. 4 is referred to as a "single layer architecture," having one transversal filter per symbol position in a frame. As shown in FIG. 4, a transversal filter 401, receiving input samples shown by the representation in box 402, provides an output value to symbol decision device 403. Symbol decision device 403 determines the demodulated symbol from filter 401's output value.
The modulation format determines how symbol decision device 400 operates to decode a symbol. For example, under a BPSK format, the filter signal is compared to a threshold to determine whether a the symbol is a "1" or a "-1". Under a QAM format, however, the output symbol is the nearest symbol state in the quadrature-phase space. Under an FSK format, if a frequency detection step is performed prior to equalization/demodulation, the symbol decision is similar to the symbol decision under BPSK. However, if the input signal to the equalizer/demodulator is baud sampled data, then a frequency modulation discriminator is applied to the equalized samples of each symbol period to determine the symbol encoded in the frequency of the equalized samples.
An error signal generating device 404 provides an error signal based on the output values of transversal filter 401 and symbol decision device 403. The error signal is fed into weight update device 405 to update the filter weights or coefficients, using any one of the adaptive algorithms described above. Decision-directed carrier tracking can be incorporated using approaches similar to those described above with respect to FIG. 1. For example, phase errors in the filtered output data of transversal filter 401 can be corrected prior to symbol decision at symbol decision device 403. Such phase error, as shown in FIG. 1, can be measured by comparing a previous symbol decision to the corresponding filtered output data of transversal device 401. Thus, processor 400 comprises both a decision-directed equalizer for a specified symbol in a frame, and a decision-directed carrier tracking and down-conversion loop to center the signal spectrum at 0 Hz. When a decision-directed carrier tracking system is used, performance of the multiple-filter equalizer of the present invention is expected to be higher than a conventional equalizer because the multiple-filter equalizer is expected to deliver a higher percentage of correct symbol decisions, which allow better carrier tracking.
As mentioned above, an independent processor is configured in the equalizer of the present invention for each symbol position in the data frame. The input samples provided to each processor are samples selected on the basis of their positions with respect to the symbol being demodulated. In this embodiment, for each frame, all symbols contained in the frame are processed in parallel, so that, for every iteration of the process (i.e. every time the filter weights are updated), all symbols in one frame are equalized and symbol demodulated.
If phase correction is provided by each processor independently of other processors, the Nyquist sampling criterion requires that the bandwidth of the phase error does not exceed one half of the frame rate, which is the rate at which the phase error is sampled. Otherwise, i.e. if the Nyquist sampling criterion is not met, aliasing may affect proper detection of the phase error. In that case, to correct in a processor the phase error detected in a base band signal, phase errors from adjacent processors must be considered, thereby requiring some synchronization between processors. Alternatively, parallelism may be maintained if, for each frame, each processor uses the same phase error correction. Such phase error correction can be obtained by filtering the phase errors of all symbol locations in the previous frame.
Yet another approach to provide phase error correction is to make, for each frame, symbol decisions in a predetermined order based on symbol location. In such a system, the phase error or errors detected in one or more previous symbol decisions are provided to correct the equalizer in the current symbol decision. This approach is equivalent to providing a single carrier correction loop for all symbol locations. Of course, under this approach, symbol decisions would have to be made in a predetermined order.
A processor 500 according to an alternative embodiment of the present invention is shown in FIG. 5. This alternative embodiment, which is referred to as the "multiple layer architectures," provides a processor including multiple transversal filters per symbol position in a frame. A processor of the multiple layer architecture consists of multiple transverse filters arranged in parallel in each level, with the levels of transversal filters connected in series. As shown in FIG. 5, a first layer 520 of transversal filters is shown comprising parallel transversal filters 502a and 502b having different geometries. Filters 502a and 502b are shown to have geometries indicated respectively by representations 510a and 510b. (Of course, the geometries shown in representations 510a and 510b are provided herein for illustration only; the present invention is not limited by the geometries of the filters in representations 510a and 510b.) Representation 510a corresponds to samples adjacent in time within the same frame. Representation 510b, however, corresponds to samples of the same symbol positions in three different frames, with successive samples separated by two frame intervals.
Operators 503a and 503b apply a non-linear function to the respective output values of filters 502a and 502b. Some examples of suitable non-linear functions are sigmoidal, or logistic, functions 3 ,4. The output values of nonlinear operators 503a and 503b are used to compute a weighted sum by a second-layer filter 504. (The non-linear operators 503a and 503b are required to separate the first-layer filters 502a and 502b from the second-layer filter 504. Otherwise, the combination of a first-layer filter and its corresponding second-layer filter can be considered a single linear filter, thereby reducing the combination to an instance of the single-layer architecture.) The output value of filter 504 is then used by a symbol decision device 505 to generate a demodulated symbol.
While FIG. 5 shows two filters 502a and 502b for first layer 520 of processor 500, additional filters with different geometries can be used, depending upon the signal structure and the types of distortion in the channel. For example, processor 500 can incorporate decision-feedback equalization techniques by feeding back, for each symbol position, previous symbol decisions to a designated combination of a first-layer filter and an associated nonlinear operator in layer 520. In this configuration, the benefits of a "decision feedback equalizer" can be incorporated into multiple-filter equalizers of the present invention.
The weights of each transversal filter in a multiple layer architecture processor, such as processor 500, can be updated according to the backpropagation algorithm common in artificial neural network (ANN) processing, or according to any suitable feedforward ANN weight updating procedure. Other suitable weight-update algorithms include generalizations of dispersion-directed algorithms, Kalman algorithms, or any other suitable neural network weight-update algorithm. The backpropagation algorithm requires only that the nonlinear operator be a differentiable function. The aforementioned sigmoidal (or logistic) functions are therefore examples of suitable non-linear operators under the backpropagation algorithm. Other non-linear operators are suitable for one or more of these weight-update approaches.
The same symbol decision methods as described for the single layer architecture can be used for a processor of the multiple layer architecture. Thus, in processor 500, one frame of symbols is equalized and demodulated per iteration. The multiple layer architecture with the backpropagation algorithm can operate in a blind decision-directed mode or use a training sequence.
The above detailed description is provided to illustrate the specific embodiments of the present invention and is not intended to be limiting of the present invention. Numerous modifications and variations are possible within the scope of the present invention. For example, although the above detailed description provides examples of decision-directed carrier tracking, the present invention is equally applicable to systems in which a different carrier-tracking system is used, including a system in which symbol decision feedback is not used. Such a carrier-tracking system, for example, can provide phase error correction prior to equalization. An example of such a method is the "power of N carrier recovery" method described in § 14.2 of Digital Communication, by Edward Lee and David Messerschmitt, Kluwer Academic Publishers, 1988. The present invention is defined by the following claims. | An equalization and demodulation method for a structured digitally modulated signal provides a multiple filter equalizer, which comprises multiple, parallel, automatically adjustable processors. The multiple filter equalizer is applicable to a structured digitally modulated signal, such as a signal from time division multiplexing (TDM) of multiple data sources. The multiple filter equalizer exploits the repetitive structure of TDM signal data by employing multiple parallel processors each constructed according to the specific requirements at the position in the frame of a symbol to be demodulated. Each processor comprises one or more adaptive digital transversal filters, one or more nonlinear threshold operators, and a symbol decision operator. The transversal filters equalize the data, remove interfering signals, reduce intersymbol interference, and mitigate multipath and other propagation effects. After the samples corresponding to one frame of information symbols are equalized in parallel, the equalized samples are demodulated in parallel to generate demodulated information symbols for that frame. The method is applicable to adaptive equalization both with and without a known training sequence. | 7 |
CROSS REFERENCE TO RELATED APPLICATION(S)
[0001] The present application claims the benefit of U.S. Provisional Application Ser. No. 60/532,107 filed on Dec. 22, 2003.
BACKGROUND OF THE INVENTION
[0002] The present invention relates to an exercise weight which was an elongated tubular cover and filled with a particulate material that is flexible so it may conform to various portions of the body. In particular, the exercise weight has a length that is retainable over the shoulders, around the neck or mid-section and includes stirrups or hand loops at the opposite ends of the elongated tubular cover which carry fasteners or a buckle to permit forming the weight into a loop or circular enclosure.
[0003] In the prior art, various types of exercise weights have been used, including multi-functional devices that have various hinged sections, and form elongated weights that can be lifted and twisted. Elongated bars with handles at opposite ends have been used as well. Additionally, the use of flexible members that are elongated and can be grasped by the hands have been provided.
[0004] However, a versatile, adjustable length, conformable and flexible weight that can be used in an enclosed loop, or in an elongated form, is desirable.
SUMMARY OF THE INVENTION
[0005] The present invention includes an exercising device having an elongated tube with a central axis that is filled with a particulate material of a selected weight. The particulate material shifts within the elongated tube to provide flexibility along the length of the tube and wherein the elongated tube compresses when pressure is applied thereto.
BRIEF DESCRIPTION OF THE DRAWINGS
[0006] FIG. 1 is a perspective view of the elongated flexible weight of the present invention;
[0007] FIG. 2 is a sectional view of the elongated flexible weight along section line 2 -- 2 in FIG. 1 ;
[0008] FIG. 3 is a perspective view of the elongated flexible weight secured in a loop about a waist of the exerciser;
[0009] FIG. 4 is a top view of an alternative embodiment of the flexible weight of the present invention;
[0010] FIG. 5 is a perspective view of the alternative embodiment of the present invention in a curved position;
[0011] FIG. 6 is a perspective view of the alternative embodiment of the present invention in a loop configuration;
[0012] FIG. 7 is a perspective view of a flexible hand weight of the present invention;
[0013] FIG. 8 is an alternative embodiment of the flexible hand weight of the present invention;
[0014] FIG. 9 is a perspective view of an exerciser resistance training with the flexible weight of the present invention being looped about a fore arm of the exerciser;
[0015] FIG. 10 is a perspective view of the exerciser of the present invention exercising shoulder muscles with less resistance than in FIG. 9 ;
[0016] FIG. 11 is a perspective view of an exerciser using a single elongated weight to vary resistance;
[0017] FIG. 12 is a perspective view of an exerciser using a plurality of flexible elongated weights positioned about the exercisers waist;
[0018] FIG. 13 is a partial perspective view of an exerciser gripping the first and second handle straps for doing lifting exercises;
[0019] FIG. 14 is a perspective view of an exerciser gripping the elongated flexible weight and doing arm exercises;
[0020] FIG. 15 is another perspective view of an exerciser gripping the elongated flexible weight and doing arm exercises;
[0021] FIG. 16 is a perspective view of an exerciser employing a flexible elongated weight about a nape of the exerciser and performing leg exercises;
[0022] FIG. 17 is a perspective view of an exerciser engaging a foot through a loop of the elongated weight and performing leg exercises;
[0023] FIG. 18 is a perspective view of the exerciser coiling a flexible weight about a leg to reduce a resistance of the weight while performing leg exercises;
[0024] FIG. 19 is a perspective view of the exerciser coiling a flexible weight about the leg and performing leg raising exercises while lying on a side; and
[0025] FIG. 20 is a perspective view of the exerciser having a flexible weight coiled about the arm and performing arm raising exercises.
DESCRIPTION OF THE PREFERRED EMBODIMENT
[0026] A flexible weight of the present invention is illustrated generally at 10 in FIG. 1 . Referring to FIGS. 1 and 2 , the flexible weight 10 has an elongated sleeve or tube 12 filled with a selected amount of a particulate material or granular material 14 such that the flexible weight 10 has a desired weight.
[0027] After being filled with the particulate material or granular material 14 , the tube 12 is closed at its ends 16 and 18 . The tube 12 can be seamed in a suitable manner by sewing it at its ends and along a length, if desired, and can be made of a material that can be pre-formed into a tubular shape with one end open for filling. The tube 12 can be closed by sewing it together or with adhesives or heat sealed, or in other ways as well. The granular material 14 is generally a dry material such as a dry sand, small rock, various type of metal shot, hollow spheres, and the like.
[0028] The tube 12 has a generally circular cross section and a central axis 13 running the length of the tube. The tube 12 is generally of a cloth-like material so that it is comfortable against the skin of a person, and which is a durable material as well to avoid excessive wear.
[0029] Optionally, the tube 12 may be covered by a sleeve 11 . The sleeve 11 is preferably removable from the tube 12 and is capable of being washed to remove dirt and perspiration and also to provide additional protection to the exerciser.
[0030] The tube 12 includes at least one loop 20 at one end 16 of the tube. The loop 20 can be used as a hand grip or a foot stirrup as well as being positioned on a limb. Preferably, a buckle 22 is attached to the loop 20 and engages a strap 24 attached to the other end 18 of the tube 12 . The strap 24 can be used as a hand grip or positioned through the buckle 22 to define a loop of a selected perimeter. The buckle 22 secures the strap 24 in a selected position thereby securing the flexible weight 10 around a portion of the exerciser's body such as a torso or waist 42 of an exerciser 40 as best illustrated in FIG. 3 . The exerciser can utilize the flexible weight 10 secured about the waist 42 while walking, jogging, in-line skating, or other aerobic activity such as martial arts and performing leg exercises including squats or lunges.
[0031] Referring to FIGS. 4-7 , a second loop 26 can be attached to the other end 18 of the tube 12 instead of the strap 24 . The second loop 26 can also be used as a hand grip or a foot stirrup. The loops 20 , 26 define openings that are of size to receive an arm or leg of the exerciser 40 . The loops 20 , 26 and the strap 24 can be made of a material that can either be a non-stretch fabric, rope and the like, or if desired, can be an elastic material such as rubber or suitable elastomer. The material for the loops 20 , 26 and the strap 24 can also run continuously along the entire outer or inner surface of the tube 12 to help in the structural integrity of the design.
[0032] At the outer end of each of the loops 20 , 26 , there alternatively may be an adjustable fastening mechanism 28 that includes mating elements 30 , 32 that can be joined together or held together in some manner. A non-exhaustive list of fastening mechanisms 28 include a buckle, a snap, a hook and loop fastener such as that sold under the Velcro trademark and a buckle with a hasp engaging holes in the other loop. It is apparent that other types of fasteners can be used as well.
[0033] An adjusting buckle 21 is attached to the loop 20 to vary the overall circumference of the elongated weight 10 when positioned into a loop. It is apparent that a second adjusting buckle may also be attached to the loop 26 to further adjust the circumference of the elongated weight 10 .
[0034] The tube 12 can be of any desired length, but for example, a length of about 3 feet has found to be acceptable. A tube diameter of approximately 3-4 inches also is found acceptable. This diameter can vary from about 2 inches up to about 12 inches depending on the weight that is desired. The particulate material 14 can be from 2 pounds up to in excess of 100 pounds depending on the desires of the users, and provides weight suitable for muscle exertion by the exerciser while exercising.
[0035] The tube 12 may have indicia 34 to indicate a selected weight or may have indicia which corresponds to a weight 34 . By indicia is meant any distinctive marking such as printing, a color or a design.
[0036] Referring to FIGS. 7 and 8 , it is also within the scope of the present invention for a flexible weight 50 to be configured to be hand-held and having a generally cylindrical configuration with a central axis 51 . The hand-held weights 50 include an elongated tube 52 that is filled with a selected amount of particulate material or granular material and is sealed at both ends 54 , 56 . The particulate material shifts within the tube 52 such that the hand-held weight conforms to a grip of the exerciser 40 . The hand-held weights 50 are retained to the exerciser's hand 44 by a retaining strap 58 . The retaining strap 58 is secured to the elongated sleeve 52 and can is sized to receive some or all of the digits of the hand.
[0037] The retaining strap 58 is sized to receive all four digits of the hand as illustrated in FIG. 7 . Alternatively, the retaining strap 58 can be sized to receive only one digit as illustrated in FIG. 8 . It is also within the scope of the present invention for the retaining strap 58 to receive two or three digits.
[0038] The elongated flexible weight 10 can be used separately from the hand held weights 50 . The elongated flexible weight 10 can also be used at the same time as the hand held weights.
[0039] The flexible elongated weights 10 , 50 can be used to perform all of the exercises that can be performed with a rigid barbell or dumbbell. One advantage of the flexible elongated weights 10 , 50 is that the particulate material shifts within the tube 12 , 52 , thereby reducing or eliminating the likelihood of the exerciser injuring his/her foot or hand if the flexible weights 10 , 50 is accidentally dropped upon the exerciser. The flexible weights 10 , 50 when dropped will conform to the foot or hand and not injure the exerciser.
[0040] Additionally, a single elongated flexible weight 10 is useful at providing different resistances depending upon a distance D from a center of gravity the flexible elongated weight 10 from the joint that is being articulated by flexing and isolating muscles or muscle groups. By way of example, referring to FIG. 10 , the weight 10 may be positioned along a length of the arm 48 , where the particulate material 14 shifts within the elongated tube to conform to the contour of the arm 48 . Positioning the elongated weight 10 upon the arm 48 shifts the center of gravity proximate the shoulder joint defined by the distance D, and the resistance to the shoulder muscles is lessened as the arm is raised and lowered by articulating the shoulder joint 49 .
[0041] Referring to FIG. 9 , when the same weight is hanging from the arm 48 near the hand 49 , the resistance is increased as the arm 48 is raised and lowered by articulating the shoulder joint 49 because the center of gravity is a further distance D from the shoulder joint 49 . The flexible weights can be positioned anywhere along the length of the arm 48 to increase or decrease the resistance by shifting the distance D from the center of gravity of the weight to the joint being articulated.
[0042] Referring to FIG. 20 , the exerciser 40 can insert the arm through the loop 20 and coil the flexible weight 10 about the arm to adjust the distance D from the shoulder joint 49 to the center of gravity of the flexible weight 10 and thereby varying the resistance on the shoulder muscles. The coils can be moved toward the hand to increase the distance D and therefore the increase the resistance on the shoulder muscles or the coils can be shifted toward the shoulder joint 49 and thereby decrease the resistance on the shoulder muscles by decreasing the distance D.
[0043] As the weight 10 is positioned further from the articulating joint 49 , the resistance is increased and as the weight 10 is positioned closer to the articulating joint 49 , the resistance is decreased. Therefore, the exerciser can achieve a variety of resistances with the same flexible weight 10 , and eliminates the need to add or reduce weight from a barbell or retrieve a different weighted dumbbell. Varying the position of the flexible weight 10 on a leg 47 to vary the resistance to a muscle or muscle group is also within the scope of the present invention.
[0044] Referring to FIG. 11 , another method of use of a single flexible weight 10 that provides a varying amount of resistance is to place a first portion 15 of the flexible weight on a surface such as a bench or the exerciser's lap 45 and lifting only a second portion 17 of the weight 10 by articulating a joint or joints. As more of the weight 10 is positioned upon the surface or lap 45 by increasing a length of the first portion 15 , the muscles used to articulate the joint incur less resistance. Conversely, as the length of the first position 15 decreases, the length of the second portion increases 17 and the resistance upon the muscles used to articulate the joint increases. By varying the lengths of the first portions 15 of the elongated flexible weight 10 upon the surface or lap 45 , a length of the second portion 17 also varies and thereby varies the resistance to a muscle or group of muscles while employing only one weight. In contrast when rigid weights are used to exercise, different weights have to be added to or removed from a barbell or a different set of dumbbells must be used, both of which increase the time and inconvenience in exercising.
[0045] Referring to FIG. 12 , the elongated flexible weight 10 of the present invention is also useful in quickly decreasing the amount of weight being lifted thereby allowing the exerciser to continue exercising as the isolated muscles fatigue. A plurality of elongated flexible weights 10 are positioned about the waist 42 or upon the nape 43 . As the muscles being exercised fatigue one or more of the flexible weights 10 are removed from the exerciser by removing the weight from the nape of the neck or unfastening the buckle 22 and allowing the elongated weight 10 to drop. This procedure can be repeated until no elongated weights 10 remain on the exerciser 40 .
[0046] The elongated flexible weight 10 and/or hand weights 50 are also useful in performing a number of exercises that can be performed using a barbell or a dumbbell. The flexibility of the elongated weight 10 allows a variety of exercises to be performed with a single weight.
[0047] FIG. 13 illustrates a user 40 holding the loops 20 , 26 for lifting in the hands 44 . Aside from grasping the loops 20 , 26 , the tube 12 itself can be gripped by the user's hand 44 at any portion along the tube 12 , the exerciser 40 can perform various exercises and aerobic motions, like curls, press's and others, such as forearm exercises. FIG. 14 shows the exerciser 40 holding the elongated tube 12 proximate the ends 14 , 16 with both hands for performing curls and other upper body exercises, thereby moving both arms simultaneously, or for moving one arm and then the other. Reversing the position of the weight 10 so the major portion of the tube 12 is above the hands 44 , as illustrated in FIG. 15 , permits the exerciser 40 to upright raise exercises and allows for additional exercising versatility.
[0048] In FIG. 16 , the weight 10 is formed into the loop and is placed around the neck 41 and about the nape 43 of a user 40 . In this illustration, the elongated weight 10 adds additional weight to the body, so that doing “squats” by flexing the knees and hips exercises the leg muscles. When positioned about the nape 43 , the elongated flexible weight 10 conforms to the exerciser's shoulders and chest, thereby allowing the back to be in the proper position because the weight is distributed about the spine. The position or location of the weight 10 also serves for adding resistance to movements like lunging, stepping, skating, walking and jogging.
[0049] FIG. 14 shows a leg raise exercise where a foot 45 is positioned within the loop 20 . By inserting the foot 45 into the loop 18 and holding the weight along a leg 47 , the leg muscles can be exercised by front, rear and sideways movement.
[0050] Referring to FIG. 18 , the elongated weight 10 can be coiled about the leg 47 to move the center of gravity a distance from the articulated joint and thereby change the resistant to muscles being exercised with a single weight. As the coils are wound tightly to ward the foot 45 , the center of gravity is shifted from the articulating hop or knee joint. Conversely, as the distance between the coils is increased, the center of gravity is shifted toward the articulating knee or hip joint thereby decreasing the resistance upon the muscles being exercised. The elongated weight 10 can also be coiled about the arm 48 in a similar fashion to increase or decrease the resistance while using a simple elongated weight.
[0051] Referring to FIG. 19 , the exerciser 40 can lay on his/her side with the elongated weight 10 coiled about the leg 47 with the foot 45 positioned within the loop 20 . The exerciser 40 grips the other loop 26 and can perform a variety of leg raises that exercise the upper leg, hip flexor and buttocks. By adjusting the position of the coils about the leg 47 , the resistance created with one elongated weight 10 can be increased by positioning the coils proximate the foot 45 or the resistance decreased by spacing apart the coils such that a center of gravity is nearer the muscles being exercised.
[0052] 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. | An exercising device includes an elongated tube with a central axis that is filled with a particulate material of a selected weight. The particulate material shifts within the elongated tube to provide flexibility along the length of the tube and wherein the elongated tube compresses when pressure is applied thereto. | 0 |
FIELD OF THE INVENTION
The present invention relates generally to circuit breakers and, more particularly, to a high current capacity blade for a circuit breaker.
BACKGROUND OF THE INVENTION
Use of circuit breakers is widespread in modern-day residential, commercial and industrial electric systems, and they constitute an indispensable component of such systems toward providing protection against over-current conditions. Various circuit breaker mechanisms have evolved and have been perfected over time on the basis of application-specific factors such as current capacity, response time, and the type of reset (manual or remote) function desired of the breaker.
One type of circuit breaker mechanism employs a thermo-magnetic tripping device to "trip" a latch in response to a specific range of over-current conditions. The tripping action is caused by a significant deflection in a bi-metal or thermostatmetal element which responds to changes in temperature due to resistance heating caused by flow of the circuit's electric current through the element. The thermostat metal element is typically in the form of a flat metal member and operates in conjunction with a latch so that metal member deflection releases the latch after a time delay corresponding to a predetermined over-current threshold in order to "break" the current circuit associated therewith. Circuit breaker mechanisms of this type often include an electro-magnet operating upon a lever to release the breaker latch in the presence of a short circuit or very high current condition. A handle or push button mechanism is also provided for opening up the electric contacts to the requisite separation width and Sufficiently fast to realize adequate current interruption.
Another type of circuit breaker, referred to as a "double-break" circuit breaker, includes two sets of current-breaking contacts to accommodate a higher level of over-current conditions than is accommodated by the one discussed above. One such double-break circuit breaker implements its two sets of contacts using the respective ends of an elongated rotatable blade as movable contacts which meet non-movable contacts disposed adjacent the non-movable contacts. The non-movable contacts are located on the ends of respective U-shaped stationary terminals, so that an electro-magnetic blow-off force ensues when the current, exceeding the threshold level, passes through the U-shaped terminals. Thus, when this high-level over-current condition is present, the blow-off force causes the elongated rotatable blade to rotate and the two sets of contacts to separate simultaneously.
Another type of double-break circuit breaker implements its two sets of contacts using separate and independent structures. For example, one set of contacts may be implemented using the previously-discussed thermo-magnetic tripping device to trip the current path at low-level current conditions, and the other set of contacts using an intricate and current-sensitive arrangement which separates its contacts in response to high-level blow-off current conditions. See, for example, U.S. Pat. Nos. 3,944,953, 3,96,346, 3,943,316 and 3,943,472, each of which is assigned to the instant assignee.
While providing adequate protection to high-level over-current conditions, there is still a need for a circuit breaker structure, useful with both single-break and double-break circuit breakers, which accommodates extremely high levels of current in a relatively small package.
SUMMARY OF THE INVENTION
An object of the present invention is to provide a circuit breaker blade having a high current capacity. A related object is to provide a circuit breaker blade capable of handling the high contact force required for the high current capacity.
Another object of the present invention is to provide a circuit breaker blade having a high interruption capacity and, therefore, a high operational performance.
In a particular embodiment, these objects are realized by providing a high current capacity blade for a circuit breaker, comprising a conductive blade body having front and rear sections connected to one another, where the rear section includes a surface attachment area for fastening a flexible connector of the circuit breaker thereto. A strain relief tang extending from the rear section of the blade body is used to engage the flexible connector so as to stabilize the fastening of the flexible connector to the surface attachment area. A broad conductive lateral section is connected to and extends laterally from the front section, and includes a blade tab for engaging a toggle spring of the circuit breaker. A broad moveable contact is mounted on the broad lateral section and is adapted to interface with a stationary contact of the circuit breaker. A pair of substantially parallel L-shaped blade legs are spaced from one another to permit the toggle spring to pass therebetween. Each of the blade legs has first and second ends with the first ends connected to the rear portion of the blade body and the second ends including respective blade pivots for engaging notches in a handle of the circuit breaker.
The above summary of the present invention is not intended to represent each embodiment, or every aspect, of the present invention. This is the purpose of the figures and the detailed description which follow.
BRIEF DESCRIPTION OF THE DRAWINGS
Other objects and advantages of the invention will become apparent upon reading the following detailed description and upon reference to the drawings in which:
FIG. 1 is a side view of a series double breaker circuit breaker including a primary blade embodying the present invention;
FIG. 2 is a perspective view of a primary blade embodying the present invention; and
FIG. 3 is a side view of the primary blade shown in FIG. 2.
While the invention is susceptible to various modifications and alternative forms, a specific embodiment thereof has been shown by way of example in the drawings and will be described in detail. It should be understood, however, that it is not intended to limit the invention to the particular form described. On the contrary, the intention is to cover all modifications, equivalents and alternatives falling within the spirit and scope of the invention as defined by the appended claims.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
Turning now to the drawings, FIG. 1 illustrates the basic configuration of a primary blade 32 embodying the present invention in the context of a double-break circuit breaker. The present invention is discussed in the context of such an exemplary double-break circuit breaker for illustrative purposes only, and the particular circuit breaker illustrated and described (FIG. 2) should not be construed to limit the possible applications for the present invention, as these applications encompass a wide variety of circuit breaker types. To fully appreciate the utility of the present invention, however, the double-break circuit breaker of FIG. 1 will first be described, followed by a detailed description of the primary blade 32, which embodies the principles of the present invention.
The circuit breaker of FIG. 1 includes a circuit breaker base 14 which carries all of the internal components of the circuit breaker. The current path through the circuit breaker begins at a line terminal 16, and from the line terminal 16 the current path goes through a flexible pigtail 18. The flexible pigtail 18 is attached to a secondary blade 20 with a moveable contact 22 mating with a stationary contact 24. Current flows through the moveable and stationary contacts 22, 24 to the mid terminal 26, which is configured in an S form. The other side of the mid terminal 26 includes another stationary contact 28 connected thereto. Positioned opposite the stationary contact 28 is a mating moveable contact 30 attached to the primary blade 32. Current flows through the stationary and moveable contacts 28, 30, through the primary blade 32, and into one end of a primary flexible connector or pigtail 34. The other end of the primary flexible connector 34 is attached to a bimetal 36, which provides the thermal tripping characteristics for the circuit breaker. Finally, the current flows from the bimetal 36 through a load terminal 38 and out of the load end of the circuit breaker via a lug 40.
The primary section of the circuit breaker includes the primary blade 32, a trip lever 42, a handle 44, a magnetic armature 46, a pigtail 34, and a primary arc stack 13. The secondary section includes the secondary blade 20, the pigtail 18, an extension spring 48, and a secondary arc stack 10. In the illustrated circuit breaker, using conventional magnetic and thermal trip protection features, the primary section provides the breaking capacity for all levels of current from one ampere to approximately 3000 amperes without operational assistance from the secondary section. The magnetic armature 46 is drawn to a yoke 50 during high current flow. This allows the trip lever 42 to disengage from the magnetic armature 46 and rotate to the trip position, which, in turn, allows the primary blade contact 30 to separate from the stationary contact 28 to break the current flow. As the contacts 28, 30 are separated, an are voltage is generated in the primary arc stack 13. A thermal trip via the bimetal 36 results in the same sequence of events and, additionally, results in the trip lever 42 disengaging from the magnetic armature 46.
The normal ON and OFF operation of the primary blade 32 occurs in response to rotation of the handle 44 in a clockwise or counterclockwise motion. In response to rotation of the handle 44 in either direction, the primary blade 32 either opens or closes the circuit via the primary moveable contact 30 and the primary stationary contact 28. Rotation of the primary blade 32 is tied directly to the handle 44 for the normal ON and OFF operation of the primary blade 32. Furthermore, the secondary section is not affected by the normal ON and OFF operation of the primary blade 32. The secondary blade contact 22 and the secondary stationary contact 24 remain closed.
As previously explained, the secondary section of the circuit breaker has limited operation below 3000 amperes of fault current. However, at current levels above 3000 amperes, the secondary section begins to contribute to interruption performance. In particular, the secondary blade 20 derives contact force from the extension spring 48. The secondary blade 20 pivots about the blade pivot 52 with the extension spring 48 extended as the secondary blade 20 opens up in response to a current fault above 3000 amperes. There is no linkage of the secondary blade 20 to the primary blade 32, but rather the operation of the secondary and primary blades 20, 32 is totally separate and independent.
In response to the occurrence of a current fault above 3000 amperes, the constriction resistance of the secondary blade contact 22 and the secondary stationary contact 24 provides a magnetic force that tries to separate the contacts. Simultaneously, the current path configuration of the mid terminal 26 and the secondary blade 20 forms a magnetic blowoff loop which also tries to separate the contacts 22, 24. The addition of both of these opening forces to the secondary blade 20 causes the secondary blade 20 to separate at the contacts 22, 24. As the secondary blade 20 opens, the extension spring 48 begins to stretch. The extension spring 48 permits the secondary blade 20 to continue to open as long as the force to open the blade is greater than the extension force of the spring 48. As the contacts 22, 24 are separated, an arc voltage is generated in the secondary arc stack 10. The combination of the are voltage generated by the secondary are stack 10 and the arc voltage generated by the primary arc stack 13 make these voltages add together. This allows a very fast rise of are voltage and also allows high levels of arc voltage consistent with double break circuit breakers.
As the current fault level rises higher and higher above 3000 amperes, the faster and higher the secondary blade 20 will be moved. As the interruption takes place and the electric are is extinguished in the primary and secondary sections, the secondary blade 20 is biased to return to the closed position because of the spring bias from the extension spring 48. The primary blade 32 remains in the open or tripped position. At this point, the interruption of the current fault is complete with no opportunity to re-establish itself.
For further information regarding the overall construction and operation of the circuit breaker shown in FIG. 2, reference may be made to U.S. patent application Ser. No. 08/81,289, entitled "Circuit Breaker Having Double Break Mechanism", filed concurrently herewith, assigned to the instant assignee and incorporated herein by reference.
FIGS. 2 and 3 illustrate the high current capacity primary blade 32 embodying the present invention and related to the blade shown in FIG. 12 of U.S. patent application Ser. No. 07/878648 (issuing as U.S. Pat. No. 5,245,302 on Sep. 14, 1993), incorporated herein by reference. The primary blade 32 includes an integral blade body 54 bridging an integral lateral section 56 and a pair of blade legs 58. At one end, the lateral section 56 includes the moveable contact 30 connected thereto and interfacing with the stationary contact 28 (see FIG. 1). At the other end, the lateral section 56 includes a blade tab 60 for engaging one end of a toggle spring (not shown). The primary blade 32 is z-axis assembled into the base 14 of the circuit breaker in such a way as to attach the blade tab 60 to a triplever hook via the toggle spring. Also, the blade legs 58 are engaged with respective notches in the circuit breaker handle 44. The primary blade 32 is situated in the base 14 with the blade body 54 positioned substantially parallel to the inner surface of base 14 and the lateral section 56 extending upwardly in a direction away from the inner surface of the base 14.
The blade body 54 is integrally connected to the lateral section 56 and is positioned substantially orthogonal to the lateral section 56. The blade body 54 includes a rear portion 62 and a front portion 64 adjacent the lateral section 56. The rear and front portions 62, 64 are configured in the manner illustrated in FIG. 2. In particular, the rear portion 62 is wider than the front portion 64, and the front portion is connected to the approximate middle of the rear portion 62. The flexible connector 34 (see FIG. 1) is fastened to the surface attachment area 76 of the rear portion 62. This attachment is stabilized using a strain relief tang 66 connected to the rear portion 62 and extending laterally from the rear portion 62 in a direction opposite the lateral section 56. To stabilize the connection between the flexible connector 34 and the area 76 using the strain relief tang 66, the flexible connector 34 is inserted into the region labelled 68 and crimped therein by the strain relief tang 66. In crimping the flexible connector 34 in the region 68, the strain relief tang 66 is rotatably bent toward the rear portion 62 so that the flexible connector 34 is "sandwiched" between the strain relief tang 66 and the rear portion 62. The design of the strain relief tang 66 permits the strain relief tang 66 to secure a large flexible connector or multiple flexible connectors in the region 68.
The pair of blade legs 58 are integrally connected to the rear portion 62 of the blade body 54 via a lateral waist section 70 extending in the same direction as the lateral section 56. The blade legs 58 are formed substantially parallel to one another and are spaced from one another to permit the toggle spring to pass therebetween. The blade legs 58 are formed with respective right-angled bends as shown in FIG. 2 and terminate in blade pivots 72. The blade pivots 72 are biased to sit in notches in the circuit breaker handle 44 shown in FIG. 1 because of the force applied by the toggle spring in connecting the blade tab 60 to the triplever hook adjacent the handle 44.
Since the primary blade 32 is a high current capacity blade, the contact force required for the blade 32 is relatively high (28 to 30 ounces). This contact force is generated from a relatively strong force applied by the toggle spring, and the blade 32 includes several features designed to withstand this relatively strong force. First, the blade pivots 72 are rounded, i.e., have rolled radii. The rolled radii facilitate pivoting of the pivots 72 within the notches of the circuit breaker handle 44. Second, as best shown in FIG. 3, the upper "thigh" portion of one of the blade legs 58 abuts against the rear edge 74 of the blade body 54. The purpose of having the blade leg 58 touch the blade body 54 is to provide additional support to the blade body 54. Since the toggle spring applies a relatively strong force to the blade body 54 which is partially directed toward the blade legs 58, the blade body 54 exerts a torque about the waist section 70. The abutment between the blade leg 58 and the blade body 54 prevents the waist section 70 from bending due to this torque. Third, the blade tab 60 is provided with additional strength to withstand the relatively strong force generated by the toggle spring connected thereto. This additional strength stems from the integrity of the primary blade 32. In particular, the blade tab 60 is formed within the integral lateral section 56, and the lateral section 56 is integrally connected to the blade body 54.
The primary blade 32 is designed to carry currents in excess of 100 amperes. In the primary blade 32, current flows from the moveable contact 30, through the lateral section 56 and the blade body 54, and to the interface 76 with the flexible connector 34. In order for the primary blade 32 to have a high current capacity, the moveable contact 30 is designed larger in size than the moveable contacts of existing blades. Similarly, the large lateral section 56 supporting the moveable contact 30 not only increases the current capacity of the blade 32, but also increases the interruption capacity of the blade 32. As the current flows through the lateral section 56 into the blade body 54, the current capacity of the blade 32 is increased due to the relatively long current path between the lateral section 56 and the flexible connector attachment region 76, as well as the relatively large thickness of the blade body 54. For high end interruption, a slide fiber 32 (FIG. 1) is hooked into the region 74 of the blade 32 and is used to provide the gas pressure to push the arc into the arc stack 13.
As an alternative embodiment to the blade shown in FIGS. 2 and 3, reference may be to the blade illustration and description in U.S. patent application Ser. No. 07/878648 (and its progeny and ancestors) (DC-0137), entitled "Automatic Miniature Circuit Breaker With Z-Axis Assemblable Trip Mechanism", filed Apr. 5, 1992, assigned to the instant assignee and incorporated herein by reference.
Those skilled in the art will readily recognize that various modifications and changes may be made to the present invention without departing from the true spirit and scope thereof, which is set forth in the following claims. | A high current capacity blade for a circuit breaker, comprises a conductive blade body having front and rear sections connected to one another, where the rear section includes a surface attachment area for fastening a flexible connector of the circuit breaker thereto. A strain relief tang extending from the rear section of the blade body is used to engage the flexible connector so as to stabilize the fastening of the flexible connector to the surface attachment area. A broad conductive lateral section is connected to and extends laterally from the front section, and includes a blade tab for engaging a toggle spring of the circuit breaker. A broad moveable contact is mounted on the broad lateral section and is adapted to interface with a stationary contact of the circuit breaker. A pair of substantially parallel L-shaped blade legs are spaced from one another to permit the toggle spring to pass therebetween. Each of the blade legs has first and second ends with the first ends connected to the rear portion of the blade body and the second ends including respective blade pivots for engaging notches in a handle of the circuit breaker. The assembly accommodates automated Z-axis assembly. | 7 |
CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] This application is based upon and claims the benefit of priority from the prior Japanese Patent Application No. 2012-275592, filed on 18th Dec. 2012, the entire contents of which are incorporated herein by reference.
FIELD
[0002] The present invention relates to a display device, and specifically to a display device which includes an organic EL display panel for displaying a white image and an electrochromic layer stacked thereon and thus is capable of providing high-definition color display easily.
BACKGROUND
[0003] Organic EL display devices including an organic light emitting diode (OLED) which uses organic electroluminescence (EL) are splendid in power consumption, lightweightedness, thinness, moving picture characteristic and viewing angle characteristic. Recently, organic EL display devices have been actively developed and put into practice.
[0004] As organic EL display panels for providing color display, the following two types of organic EL display panels are known (see, for example, Patent Document 1: Japanese Laid-Open Patent Publication No. 2005-85683; and Patent Document 2: Japanese Laid-Open Patent Publication No. 2011-35087).
[0005] (1) A three color type organic EL display panel in which red (R), green (G) and blue (B) light emitting elements are used as organic light emitting diodes (OLEDs) to provide color display.
[0006] (2) A color filter type organic EL display panel in which an organic light emitting diode (OLED) for emitting white light is used and the white light is transmitted through red (R), green (G) and blue (B) color filters to provide color display.
[0007] The above-described three color type organic EL display panel has the following problems. One problem is that at least three sub pixels are required for one pixel, which makes it difficult to provide high-definition display. Another problem is that a structure including RGB light emitting elements for providing high-definition display requires costly production facilities in order to obtain sufficient large process margins.
[0008] The above-described color filter type organic EL display panel also has a problem that there is a limit to the definition improvement and it is difficult to reduce the cost.
[0009] The present invention for solving the above-described problems of the conventional art has an object of providing a display device capable of displaying a high-definition color image easily without using color filters or red (R), green (G) or blue (B) sub pixels.
[0010] The above-described and other objects and novel features of the present invention will be made apparent by the description in this specification and the attached drawings.
SUMMARY
[0011] A brief overview of an illustrative embodiment of the invention disclosed in this application is as follows.
[0012] According to the present invention, an electrochromic layer acting as a filter is stacked on a display panel for displaying a white image. In synchronization with display of the white image (image of only a luminance) for, for example, red (R), green (G) or blue (B) on the display panel, a driving voltage to be applied to the electrochromic layer is controlled such that light transmitted through the electrochromic layer is red (R), green (G) or blue (B). In this manner, a color image is displayed in a field sequential system.
[0013] Owing to this, according to the present invention, high-definition color display is realized easily without using color filters or red (R), green (G) or blue (B) sub pixels.
[0014] Patent Document 1 described above discloses that a photochromic material is used to guarantee a certain level of clearness for the image displayed on a bottom emission type organic EL display panel even under strong external light.
[0015] Patent Document 2 described above discloses that an electrochromic material is used for an ND filter (light reduction filter) for reducing the luminance of the image displayed on the organic EL display panel.
[0016] However, neither Patent Document 1 nor Patent Document 2 discloses stacking an electrochromic layer on the display panel for displaying a white image so that the electrochromic layer acts as a filter.
[0017] An effect of an illustrative embodiment of the invention disclosed in this application can be described as follows briefly.
[0018] The present invention provides a display device capable of displaying a high-definition color image easily without using color filters or red(R), green (G) or blue (B) sub pixels.
BRIEF DESCRIPTION OF DRAWINGS
[0019] FIG. 1 is a cross-sectional view showing a structure of a display device in Example 1 of the present invention;
[0020] FIG. 2 shows a method for driving the display device in Example 1 of the present invention;
[0021] FIG. 3 is a cross-sectional view showing a structure of a display device in Example 2 of the present invention;
[0022] FIG. 4 is a cross-sectional view showing a structure of a display device in Example 3 of the present invention;
[0023] FIG. 5 is a cross-sectional view showing a structure of a display device in Example 4 of the present invention;
[0024] FIG. 6 shows another method for driving the display device in each of the examples of the present invention; and
[0025] FIG. 7 shows a segment type display device driven in a static manner.
DESCRIPTION OF EMBODIMENTS
[0026] Hereinafter, examples of the present invention will be described in detail with reference to the drawings.
[0027] In all the figures provided to illustrate the examples, elements having the same functions have the same reference signs, and the descriptions thereof will not be repeated. The following examples are not intended to limit the interpretation of the scope of the claims of the present invention.
[0028] FIG. 1 is a cross-sectional view showing a structure of a display device in Example 1 of the present invention.
[0029] In this example, a top emission type organic EL display panel (PNL; see FIG. 2 ) is formed on the side of a first substrate (SUB 1 ). As shown in FIG. 1 , the top emission type organic EL display panel (PNL) includes the first substrate (SUB 1 ), a TFT circuit formation section 101 , a reflective layer 102 , an OLED lower electrode 103 , an insulating layer 104 , a white light emitting layer 105 , an OLED upper transparent electrode 106 , and a sealing/filling layer 107 .
[0030] On the side of a second substrate (SUB 2 ), an electrochromic layer (EC) acting as a filter is formed.
[0031] The electrochromic layer (EC) is held between an EC upper transparent electrode 10 and an EC lower transparent electrode 11 . A voltage (EV in FIG. 1 ) to be supplied to the EC upper transparent electrode 10 and the EC lower transparent electrode 11 is controlled to control the driving voltage to be applied to the electrochromic layer (EC), and thus the spectrum of light transmitted through the electrochromic layer (EC) is changed. The EC upper transparent electrode 10 and the EC lower transparent electrode 11 hold an insulating layer therebetween when necessary.
[0032] The electrochromic layer (EC) is formed of, for example, a conjugated polymer selected from the group consisting of polyparaphenylene, polythiophene, polyphenylenevinylene, polypyrrole, polyaniline, arylamine-substituted polyarylenevinylene, and polyfluorene polymer.
[0033] FIG. 2 shows a method for driving the display device in Example 1 of the present invention.
[0034] Referring to FIG. 2 , in this example, the display device is operated as follows. A white image (luminance image) is displayed on the organic EL display panel (PNL) by an OLED driving circuit (CIROLED). A driving voltage to be applied to the electrochromic layer (EC) is controlled by an EC driving circuit (CIREC) in synchronization with the display by the OLED driving circuit (CIROLED), and thus the spectrum of the light transmitted through the electrochromic layer (EC) is changed. In this manner, a color image is displayed by the field sequential system.
[0035] For example, one frame is divided into first through third periods. In the first period, a white image (luminance image) for red (R) is displayed on the organic EL display panel (PNL) by the OLED driving circuit (CIROLED). Also in the first period, a driving voltage to be applied to the electrochromic layer (EC) is controlled by the EC driving circuit (CIREC) such that the light transmitted through the electrochromic layer (EC) is red (R).
[0036] In the second period, a white image (luminance image) for green (G) is displayed on the organic EL display panel (PNL) by the OLED driving circuit (CIROLED). Also in the second period, a driving voltage to be applied to the electrochromic layer (EC) is controlled by the EC driving circuit (CIREC) such that the light transmitted through the electrochromic layer (EC) is green (G).
[0037] In the third period, a white image (luminance image) for blue (B) is displayed on the organic EL display panel (PNL) by the OLED driving circuit (CIROLED). Also in the third period, a driving voltage to be applied to the electrochromic layer (EC) is controlled by the EC driving circuit (CIREC) such that the light transmitted through the electrochromic layer (EC) is blue (B). In this manner, a color image is displayed by the field sequential system.
[0038] Light transmitted through the electrochromic layer (EC) is of a plurality of colors among red (R), green (G), blue (B), yellow (Y), cyan (Cy), magenta (Mg) and white (W). Color display is provided by light of a mixture of such a plurality of colors.
[0039] According to this example, images of red (R), green (G) and blue (B) are displayed by one sub pixel. Therefore, as compared with the conventional three color type organic EL display panel including red (R), green (G) and blue (B) sub pixels, the same size of pixels can be used to display at least three times the number of images. This can improve the definition easily. In addition, according to this example, color filters are not used. Therefore, high-definition color display can be provided easily. Since color mixing is not performed, viewing angle dependence is reduced.
[0040] FIG. 3 is a cross-sectional view showing a structure of one pixel of a display device in Example 2 of the present invention.
[0041] In this example, unlike in Example 1 described above, the EC upper transparent electrode 10 and the electrochromic layer (EC) are provided on the OLED upper transparent electrode 106 , the sealing/filling layer 107 is provided on the EC upper transparent electrode 10 , and the OLED upper transparent electrode 106 also acts as the EC lower transparent electrode 11 . Except for these points, the display device in Example 2 is the same as the display device in Example 1 in terms of the structure and the manner of operation. The same descriptions will not be repeated.
[0042] In this example, the OLED upper transparent electrode 106 and the EC lower transparent electrode 11 can be realized by one electrode. Therefore, the display device in this example has a simpler structure and is produced more easily than the display device in Example 1.
[0043] As compared with the display device in Example 1, the number of layers is smaller by one since the OLED upper transparent electrode 106 is also used as the EC lower transparent electrode 11 . Therefore, reduction in the light emitted by the white light emitting layer 105 of the OLED can be decreased.
[0044] FIG. 4 is a cross-sectional view showing a structure of one pixel of a display device in Example 3 of the present invention.
[0045] In this example, unlike in Example 1 described above, two electrochromic layers, namely, a first electrochromic layer (EC 1 ) and a second electrochromic layer (EC 2 ), are stacked on the sealing/filling layer 107 .
[0046] The first electrochromic layer (EC 1 ) is held between an EC intermediate transparent electrode 21 and an EC lower transparent electrode 22 , and the second electrochromic layer (EC 2 ) is held between an EC upper transparent electrode 20 and the EC intermediate transparent electrode 21 .
[0047] Voltages to be supplied to the EC upper transparent electrode 20 , the EC intermediate transparent electrode 21 and the EC lower transparent electrode 22 are controlled to control driving voltages to be applied to the first electrochromic layer (EC 1 ) and the second electrochromic layer (EC 2 ). Thus, the spectrum of light transmitted through the first electrochromic layer (EC 1 ) and the second electrochromic layer (EC 2 ) is changed. The EC upper transparent electrode 20 and the EC intermediate transparent electrode 21 , and the EC intermediate transparent electrode 21 and the EC lower transparent electrode 22 , hold an insulating layer therebetween when necessary.
[0048] The first electrochromic layer (EC 1 ) and the second electrochromic layer (EC 2 ) are each formed of, for example, a conjugated polymer selected from the group consisting of polyparaphenylene, polythiophene, polyphenylenevinylene, polypyrrole, polyaniline, arylamine-substituted polyarylenevinylene, and polyfluorene polymer.
[0049] In this example, the display device is operated as follows. A white image (luminance image) is displayed on the organic EL display panel (PNL) by the OLED driving circuit (CIROLED). Driving voltages to be applied to the first electrochromic layer (EC 1 ) and the second electrochromic layer (EC 2 ) are controlled by the EC driving circuit (CIREC) in synchronization with the display by the OLED driving circuit (CIROLED), and thus the spectrum of the light transmitted through the first electrochromic layer (EC 1 ) and the second electrochromic layer (EC 2 ) is changed. In this manner, a color image is displayed by the field sequential system.
[0050] For example, one frame is divided into first through third periods. In the first period, a white image (luminance image) for red (R) is displayed on the organic EL display panel (PNL) by the OLED driving circuit (CIROLED). Also in the first period, driving voltages to be applied to the first electrochromic layer (EC 1 ) and the second electrochromic layer (EC 2 ) are controlled by the EC driving circuit (CIREC) such that the light transmitted through the first electrochromic layer (EC 1 ) and the second electrochromic layer (EC 2 ) is red (R).
[0051] In the second period, a white image (luminance image) for green (G) is displayed on the organic EL display panel (PNL) by the OLED driving circuit (CIROLED). Also in the second period, driving voltages to be applied to the first electrochromic layer (EC 1 ) and the second electrochromic layer (EC 2 ) are controlled by the EC driving circuit (CIREC) such that the light transmitted through the first electrochromic layer (EC 1 ) and the second electrochromic layer (EC 2 ) is green (G).
[0052] In the third period, a white image (luminance image) for blue (B) is displayed on the organic EL display panel (PNL) by the OLED driving circuit (CIROLED). Also in the third period, driving voltages to be applied to the first electrochromic layer (EC 1 ) and the second electrochromic layer (EC 2 ) are controlled by the EC driving circuit (CIREC) such that the light transmitted through the first electrochromic layer (EC 1 ) and the second electrochromic layer (EC 2 ) is blue (B). In this manner, a color image is displayed by the field sequential system.
[0053] Light transmitted through the first electrochromic layer (EC 1 ) and the second electrochromic layer (EC 2 ) is of a plurality of colors among red (R), green (G), blue (B), yellow (Y), cyan (Cy), magenta (Mg) and white (W). Color display is provided by light of a mixture of such a plurality of colors.
[0054] The color of the light to be transmitted through the two electrochromic layers, namely, the first electrochromic layer (EC 1 ) and the second electrochromic layer (EC 2 ), may be controlled by use of either one of the first electrochromic layer (EC 1 ) and the second electrochromic layer (EC 2 ), or may be controlled by use of both of the first electrochromic layer (EC 1 ) and the second electrochromic layer (EC 2 ) in combination.
[0055] For example, in the case where the light transmitted through the two electrochromic layers is to be red (R), the control may be performed such that the light transmitted through the first electrochromic layer (EC 1 ) is red while the light transmitted through the second electrochromic layer (EC 2 ) is transparent. Alternatively, the control may be performed such that a mixture of the light transmitted through the first electrochromic layer (EC 1 ) and the light transmitted through the second electrochromic layer (EC 2 ) is red (R).
[0056] In this example also, images of red (R), green (G) and blue (B) are displayed by one sub pixel. Therefore, as compared with the conventional three color type organic EL display panel including red (R), green (G) and blue (B) sub pixels, the same size of pixels can be used to display at least three times the number of images. This can improve the definition easily.
[0057] In addition, according to this example, color filters are not used. Therefore, high-definition color display can be provided easily. Since color mixing is not performed, viewing angle dependence is reduced.
[0058] In this example, the degree of freedom of the color of light transmitted through the electrochromic layers is higher than in Examples 1 and 2 described above. Two colors are mixed to display an image of colors in a wider range.
[0059] In this example also, as in Example 2, the EC upper transparent electrode 20 , the second electrochromic layer (EC 2 ), the EC intermediate transparent electrode 21 and the first electrochromic layer (EC 1 ) may be provided on the OLED upper transparent electrode 106 , the sealing/filling layer 107 may be provided on the EC upper transparent electrode 20 , and the OLED upper transparent electrode 106 may also act as the EC lower transparent electrode 22 .
[0060] FIG. 5 is a cross-sectional view showing a structure of one pixel of a display device in Example 4 of the present invention.
[0061] In this example, unlike in Example 1 described above, three electrochromic layers, namely, a first electrochromic layer (EC 1 ), a second electrochromic layer (EC 2 ) and a third electrochromic layer (EC 3 ), are stacked on the sealing/filling layer 107 .
[0062] The first electrochromic layer (EC 1 ) is held between an EC intermediate transparent electrode 1 ( 32 ) and an EC lower transparent electrode 33 . The second electrochromic layer (EC 2 ) is held between an EC intermediate transparent electrode 2 ( 31 ) and the EC intermediate transparent electrode 1 ( 32 ). The third electrochromic layer (EC 3 ) is held between an EC upper transparent electrode 30 and the EC intermediate transparent electrode 2 ( 31 ).
[0063] Voltages to be supplied to the EC upper transparent electrode 30 , the EC intermediate transparent electrode 2 ( 31 ), the EC intermediate transparent electrode 1 ( 32 ) and the EC lower transparent electrode 33 are controlled to control driving voltages to be applied to the first electrochromic layer (EC 1 ) through the third electrochromic layer (EC 3 ). Thus, the spectrum of light transmitted through the first electrochromic layer (EC 1 ) through the third electrochromic layer (EC 3 ) is changed. The EC upper transparent electrode 30 and the EC intermediate transparent electrode 2 ( 31 ), the EC intermediate transparent electrode 2 ( 31 ) and the EC intermediate transparent electrode 1 ( 32 ), the EC intermediate transparent electrode 1 ( 32 ) and the EC lower transparent electrode 33 , hold an insulating layer therebetween when necessary.
[0064] The first electrochromic layer (EC 1 ), the second electrochromic layer (EC 2 ) and the third electrochromic layer (EC 3 ) are each formed of, for example, a conjugated polymer selected from the group consisting of polyparaphenylene, polythiophene, polyphenylenevinylene, polypyrrole, polyaniline, arylamine-substituted polyarylenevinylene, and polyfluorene polymer.
[0065] In this example, the display device is operated as follows. A white image (luminance image) is displayed on the organic EL display panel (PNL) by the OLED driving circuit (CIROLED). Driving voltages to be applied to the first electrochromic layer (EC 1 ) through the third electrochromic layer (EC 3 ) are controlled by the EC driving circuit (CIREC) in synchronization with the display by the OLED driving circuit (CIROLED), and thus the spectrum of the light transmitted through the first electrochromic layer (EC 1 ) through the third electrochromic layer (EC 3 ) is changed. In this manner, a color image is displayed by the field sequential system.
[0066] For example, one frame is divided into first through third periods. In the first period, a white image (luminance image) for red (R) is displayed on the organic EL display panel (PNL) by the OLED driving circuit (CIROLED). Also in the first period, driving voltages to be applied to the first electrochromic layer (EC 1 ) through the third electrochromic layer (EC 3 ) are controlled by the EC driving circuit (CIREC) such that the light transmitted through the first electrochromic layer (EC 1 ) through the third electrochromic layer (EC 3 ) is red (R).
[0067] In the second period, a white image (luminance image) for green (G) is displayed on the organic EL display panel (PNL) by the OLED driving circuit (CIROLED). Also in the second period, driving voltages to be applied to the first electrochromic layer (EC 1 ) through the third electrochromic layer (EC 3 ) are controlled by the EC driving circuit (CIREC) such that the light transmitted through the first electrochromic layer (EC 1 ) through the third electrochromic layer (EC 3 ) is green (G).
[0068] In the third period, a white image (luminance image) for blue (B) is displayed on the organic EL display panel (PNL) by the OLED driving circuit (CIROLED). Also in the third period, driving voltages to be applied to the first electrochromic layer (EC 1 ) through the third electrochromic layer (EC 3 ) are controlled by the EC driving circuit (CIREC) such that the light transmitted through the first electrochromic layer (EC 1 ) through the third electrochromic layer (EC 3 ) is blue (B). In this manner, a color image is displayed by the field sequential system.
[0069] Light transmitted through the first electrochromic layer (EC 1 ), the second electrochromic layer (EC 2 ) and the third electrochromic layer (EC 3 ) is of a plurality of colors among red (R), green (G), blue (B), yellow (Y), cyan (Cy), magenta (Mg) and white (W). Color display is provided by light of a mixture of such a plurality of colors.
[0070] The color of the light to be transmitted through the third electrochromic layers, namely, the first electrochromic layer (EC 1 ), the second electrochromic layer (EC 2 ) and the third electrochromic layer (EC 3 ), may be controlled by use of either one of the first electrochromic layer (EC 1 ), the second electrochromic layer (EC 2 ) and the third electrochromic layer (EC 3 ), or may be controlled by use of all of the first electrochromic layer (EC 1 ), the second electrochromic layer (EC 2 ) and the third electrochromic layer (EC 3 ) in combination.
[0071] For example, in the case where the light transmitted through the three electrochromic layers is to be red (R), the control may be performed such that the light transmitted through the first electrochromic layer (EC 1 ) is red while the light transmitted through the second electrochromic layer (EC 2 ) and the light transmitted through the third electrochromic layer (EC 3 ) are transparent. Alternatively, the control may be performed such that a mixture of the light transmitted through the first electrochromic layer (EC 1 ) and the light transmitted through the second electrochromic layer (EC 2 ), a mixture of the light transmitted through the second electrochromic layer (EC 2 ) and the light transmitted through the third electrochromic layer (EC 3 ), or a mixture of the light transmitted through the first electrochromic layer (EC 1 ) and the light transmitted through the third electrochromic layer (EC 3 ) is red (R).
[0072] In this example also, images of red (R), green (G) and blue (B) are displayed by one sub pixel. Therefore, as compared with the conventional three color type organic EL display panel including red (R), green (G) and blue (B) sub pixels, the same size of pixels can be used to display at least three times the number of images. This can improve the definition easily.
[0073] In addition, according to this example, color filters are not used. Therefore, high-definition color display can be provided easily. Since color mixing is not performed, viewing angle dependence is reduced.
[0074] In this example, the degree of freedom of the color of light transmitted through the electrochromic layers is higher than in Examples 1, 2 and 3 described above. Two or three colors are mixed to display an image of colors in a wider range.
[0075] In this example also, as in Example 2, the EC upper transparent electrode 30 , the third electrochromic layer (EC 3 ), the EC intermediate transparent electrode 2 ( 31 ), the second electrochromic layer (EC 2 ), the EC intermediate transparent electrode 1 ( 32 ) and the first electrochromic layer (EC 1 ) may be provided on the OLED upper transparent electrode 106 , the sealing/filling layer 107 may be provided on the EC upper transparent electrode 30 , and the OLED upper transparent electrode 106 may also act as the EC lower transparent electrode 33 .
[0076] In each of the above-described examples, each of the electrochromic layers (EC, EC 1 , EC 2 , EC 3 ) is driven as a whole. Alternatively, as shown in, for example, FIG. 6 , each of the electrochromic layers (EC, EC 1 , EC 2 , EC 3 ) may be driven in a divided manner. FIG. 6 shows such another method for driving the display device in each of the examples.
[0077] Referring to FIG. 6 , each of the electrochromic layers (EC, EC 1 , EC 2 , EC 3 ) is divided into a plurality of areas (six areas in FIG. 6 ), and the EC driving circuit (CIREC) drives the divided areas in a time division manner or independently.
[0078] According to the driving method shown in FIG. 6 , the capacitance of each of the electrochromic layers (EC, EC 1 , EC 2 , EC 3 ), which is a load capacitance of the EC driving circuit (CIREC), can be decreased. Thus, higher-speed driving is realized.
[0079] In each of the above-described examples, in a bright site, the organic EL display panel (PNL) may stop emitting light and use the reflective layer 102 so that the organic EL display panel (PNL) acts as a reflection type device. In this case, low power consumption driving is realized.
[0080] The present invention is applicable to a display device including pixels arranged in a matrix and driven in a dynamic manner, and also is applicable to a segment type display device driven in a static manner as shown in FIG. 7 .
[0081] In the case where the present invention is applied to the segment type display device driven in the static manner as shown in FIG. 7 , seven segments A through G each include an OLED for displaying a white image and an electrochromic layer (EC, EC 1 through EC 3 ).
[0082] So far, the invention made by the present inventors has been described by way of the examples. The present invention is not limited to these examples and may be modified in various manners without departing from the gist thereof, needless to say. In the examples, the display devices include an OLED. Alternatively, a liquid crystal element for displaying a white image may be used in a display device according to the present invention instead of the OLED. In this case also, substantially the same effects are provided, needless to say. | A display device includes a display panel for displaying a white image; an electrochromic layer stacked on the display panel; a voltage application unit for applying a driving voltage to the electrochromic layer; and a display unit for displaying the white image on the display panel. The electrochromic layer allows a spectrum of light to be transmitted therethrough to be controlled in accordance with the driving voltage applied thereto; and the voltage application unit controls the driving voltage to be applied to the electrochromic layer in synchronization with display of the image on the display panel by the display unit, thus to control the spectrum of the light to be transmitted through the electrochromic layer. | 6 |
This application is a continuation of Ser. No. 857,512, filed Apr. 21, 1986, now abandoned, and a continuation of Ser. No. 543,326, filed Oct. 19, 1983, now abandoned.
BACKGROUND OF THE INVENTION 1. Field of the Invention
The present invention relates to a radiation image recording and reproducing method and a radiation image storage panel employed for the same, and more particularly, to a radiation image recording and reproducing method utilizing a divalent emporium activated complex halide stimulable phosphor and a radiation image storage panel employed for the same.
2. Description of Prior Art
For obtaining a radiation image, there has been conventionally employed a radiography utilizing a combination of a radiographic film having an emulsion layer containing a sensitive silver salt material and an intensifying screen. As a method replacing the above-mentioned conventional radiography, a radiation image recording and reproducing method utilizing a stimulable phosphor as described, for instance, in U.S. Pat. No. 4,239,968, has been recently paid much attention. The radiation image recording and reproducing method involves steps of causing the stimulable phosphor to absorb a radiation having passed through an object or having radiated by an object; exciting the phosphor with an electromagnetic wave such as visible light or infrared rays (stimulating rays) to release the radiation energy stored in the phosphor as light emission (stimulated emission); photo-electrically converting the emitted light to electric signals; and reproducing the electric signals as a visible image on a recording material such as a radiographic film or on a recording apparatus such as CRT.
Examples of the stimulable phosphor employed in the above-described radiation image recording and reproducing method, for instance, include a cerium and samarium activated strontium sulfide phosphor (SrS:Ce,Sm), an europium and samarium activated strontium sulfide phosphor (SrS:Eu,Sm), an erbium activated thorium dioxide phosphor (ThO 2 :Er), and an europium and samarium activated lanthanum oxisulfide phosphor (La 2 O 2 S Eu,Sm), as disclosed in U.S. Pat. No. 3,859,527. Further, the above-mentioned U.S. Pat. No. 4,239,968 discloses an alkaline earth metal fluorohalide phosphor having the formula (Ba 1-x ,M 2+ x )FX:yA, in which M 2+ is at least one divalent metal selected from the group consisting of Mg, Ca, Sr, Zn and Cd; X is at least one halogen selected from the group consisting of Cl, Br and I; A is at least one element selected from the group consisting of Eu, Tb, Ce, Tm, Dy, Pr, Ho, Nd, Yb and Er; and x and y are numbers satisfying the conditions of 0≦x≦=0.6 and 0≦y≦0.2, respectively.
In the above-described radiation image recording and reproducing method, a radiation image can be obtained with a sufficient amount of information by applying a radiation to the object at a considerably smaller dose, as compared with the conventional radiography. Accordingly, the radiation image recording and reproducing method is of great value, especially when the method is used for medical diagnosis.
The radiation image recording and reproducing method, as described above, is very useful for obtaining a radiation image as a visible image. However, it is desired that the sensitivity to a radiation of the method is further enhanced to decrease the exposure dose for a human body and facilitate the procedure for converting the stimulated emission to electric signals. Especially when the radiation is applied to a human body, the enhancement in the sensitivity to a radiation is of much value from the viewpoint of adverse effect of the radiation on the human body, even if the level of the enhancement is not so remarkable.
SUMMARY OF THE INVENTION
A principal object of the present invention is to provide a radiation image recording and reproducing method improved in the sensitivity.
The object is accomplished by the radiation image recording and reproducing method of the present invention comprising steps of:
causing a specific divalent europium activated complex halide phosphor to absorb a radiation having passed through an object or radiated by an object,
exposing said phosphor to an electromagnetic wave having a wavelength within the range of 450-800 nm to release the radiation energy stored therein as light emission, and
detecting the emitted light.
The divalent europium activated complex halide phosphor employed in the present invention has the formula (I):
M.sup.II FX·aM.sup.I X'·bM'.sup.II X".sub.2 ·cM.sup.III X'".sub.3 ·xA:yEu.sup.2+ (I)
in which M II is at least one alkaline earth metal selected from the group consisting of Ba, Sr and Ca; M I is at least one alkali metal selected from the group consisting of Li, Na, K, Rb and Cs; M' II is at least one divalent metal selected from the group consisting of Be and Mg: M III is at least one trivalent metal selected from the group consisting of Al, Ga, In and Tl; A is at least one metal oxide; X is at least one halogen selected from the group consisting of Cl, Br and I; each of X', X"and X"' is at least one halogen selected from the group consisting of F, Cl, Br and I; a, b and c are numbers satisfying the conditions of 0≦a≦2, 0≦b≦10 -2 , 0≦c≦10 -2 and a+b+c≧10 -6 ; and X and y are numbers satisfying the conditions of 0<x≦0.5 and 0<y≦0.2, respectively.
According to the study of the inventors, it has been discovered that the divalent europium activated complex halide phosphor having the above-mentioned formula (I) shows light emission of high luminance when excited with an electromagnetic wave having a wavelength within the range of 450-800 nm after exposure to a radiation such as X-rays, and that the radiation image recording and reproducing method has higher sensitivity than the known ones have.
In the radiation image recording and reproducing method of the present invention, the above-mentioned phosphor having the formula (I) is preferably employed in the form of a radiation image storage panel containing thereof (also called a stimulable phosphor sheet).
A radiation image storage panel has a basic structure comprising a support and a phosphor layer provided on one surface of the support. Further, a transparent protective film is generally provided on the free surface of the phosphor layer (surface not facing the support) to keep the phosphor layer from chemical deterioration or physical shock.
Accordingly, the radiation image recording and reproducing method of the invention is preferably carried out by employing a radiation image storage panel of the invention comprising a support and at least one phosphor layer which comprises a binder and a stimulable phosphor dispersed therein, in which at least one phosphor layer contains the divalent europium activated complex halide phosphor having the above-described formula (I).
BRIEF DESCRIPTION OF THE DRAWING
FIG. 1 is a schematic view showing the radiation image recording and reproducing method in accordance with the present invention, in which the numbers are used to designate the followings:
11: radiation generating device, 12: object, 13: panel, 14: source of stimulating rays, 15: photosensor, 16: image reproducing device, 17 display device, 18: filter.
DETAILED DESCRIPTION OF THE INVENTION
The present invention provides the prominent enhancement in the sensitivity of the radiation image recording and reproducing method by employing the above-described divalent europium activated complex halide phosphor having the formula (I) as a stimulable phosphor used therein.
The radiation image recording and reproducing method having the high sensitivity as mentioned above is now described more in detail with respect to an example in which the stimulable phosphor having the formula (I) is employed in the form of a radiation image storage panel containing thereof, by referring to a schematic view shown in FIG. 1.
In FIG. 1 which shows the total system of the radiation image recording and reproducing method of the present invention, a radiation generating device 11 such as an X-ray source emits a radiation for irradiating an object 12 with the radiation; a radiation image storage panel 13 containing the stimulable phosphor having the above-described formula (I) absorbs and stores energy of the radiation having passed through the object 12; a source of stimulating rays 14 emits an electromagnetic wave (stimulating rays) for impinging upon the panel 13 to release the radiation energy stored in the panel 13 as light emission; a photosensor 15 such as a photomultiplier faces the panel 13 for detecting the light emitted from the panel 13 and converting it to electric signals; an image reproducing device 16 is connected with the photosensor 15 to reproduce a transmitted radiation image from the electric signals obtained by the photosensor 15; a display device 17 is connected with the reproducing device 16 to display the reproduced image in the form of a visible image on a CRT or the like; and a filter 1B is disposed in front of the photosensor to cut the stimulating rays reflected by the panel 13 and allow only the light emitted by the panel 13 to pass through.
FIG. 1 illustrates an example of the system according to the method of the invention employed for obtaining a transmitted radiation image of an object. In the case that the object 12 itself emits a radiation, it is unnecessary to provide the above-mentioned radiation generating device 11 in the system. Further, the devices 15 through 17 in the system can be replaced with other appropriate devices which can reproduce a transmitted radiation image having the information of the object 12 from the light emitted by the panel 13.
Referring to FIG. 1, when the object 12 is exposed to a radiation such as X-rays emitted by the radiation generating device 11, the radiation passes through the object 12 in proportion to the radiation transmittance of each portion of the object. The radiation having passed through the object 12 impinges upon the radiation image storage panel 13, and is absorbed by the phosphor layer of the panel 13 in proportion to the intensity of the radiation. Thus, a radiation energy-stored image (a kind of latent image) corresponding to the transmitted radiation image of the object 12 is formed on the panel 13.
Then, when the radiation image storage panel 13 is exposed to an electromagnetic wave having a wavelength within the range of 450-800 nm, emitted from the source of stimulating rays 14, the radiation energy-stored image formed on the panel 1S is released as light emission. The luminance of so released light is in proportion to the intensity of the radiation energy which has been absorbed by the phosphor layer of the panel 13. The light signals having the luminance of the emitted light are converted to electric signals by means of the photosensor 15. The electric signals are reproduced as an image by the image reproducing device 16, and the reproduced image is displayed on the display device 17. In the concrete, the detection of the radiation image stored in the panel 13 can be, for instance, carried out by scanning the panel 13 with the electromagnetic wave emitted from the source of stimulating rays 14 and detecting the light emitted from the panel 13 under scanning by means of the photosensor 15 to sequentially obtain the electric signals.
In the radiation image recording and reproducing method of the present invention, there is no specific limitation on the radiation employable for exposure of an object so as to obtain a transmitted radiation image thereof, as far as the above-described phosphor shows stimulated emission upon excitation with the above-mentioned electromagnetic wave after exposure to the radiation. Examples of the radiation employable in the invention include those generally known such as X-rays, cathode rays and ultraviolet rays. Likewise, there is no specific limitation on the radiation emitted by an object for obtaining a radiation image thereof, as far as the radiation is absorbed by the above-described phosphor in the from of an energy source for producing the stimulated emission. Examples of the radiation include γ rays, α rays and β rays.
As the source of stimulating rays for exciting the phosphor which has absorbed the radiation having passed through or emitted by the object, there can be employed light sources emitting the light having the band spectrum distribution in the wavelength region of 450-800 nm; and light sources emitting the light having a wavelength such as an Ar + ion laser (457.9 nm, 488.0 nm, 54.5 nm, etc.), a He-Ne laser (632.8 nm) and a ruby laser (694 nm). Among the above-mentioned sources of stimulating rays, the lasers are preferred because the radiation image storage panel can be exposed thereto with a high energy density per unit area. Particularly preferred are an Ar + ion laser and a He-Ne laser.
The radiation image storage panel employable in the radiation image recording and reproducing method of the invention will be described hereinafter.
The radiation image storage panel, as described hereinbefore, comprises a support and at least one phosphor layer provided thereon comprising a binder and the divalent europium activated complex halide phosphor having the above-mentioned formula (I) dispersed therein.
The radiation image storage panel having the above-described structure can be prepared, for instance, in the manner described below.
In the first place, the divalent europium activated complex halide phosphor having the formula (I) will be described.
From the viewpoint of enhancement in the luminance of stimulated emission of the phosphor, each of X', X" and X"' in the formula (I) are preferably Br or I, and particularly preferred is Br. M I is preferably Li or Na, and particularly preferred is Na. As for M' II , there is no specific preference between Be and Mg, and both can give almost the same results. M III is preferably Al or Ga. The preferred numbers for a indicating the content of M I X', b indicating the content of M' II X" 2 and c indicating the content of M III X"' 3 are within the ranges of 10 -5 ≦a≦0.5, 0≦b≦10 -3 and 0≦c≦10 -3 , respectively.
The metal oxide indicated by A in the formula (I) is desired to be at least one metal oxide selected from the group consisting of BeO, MgO, CaO, SrO, BaO, ZnO, Al 2 O 3 , Y 2 O 3 , La 2 O 3 , In 2 O 3 , SiO 2 , TiO 2 , ZrO 2 , GeO 2 , SnO 2 , Nb 2 O 5 , Ta 2 O 5 and ThO 2 . From the viewpoint of the enhancement in the luminance of stimulated emission of the phosphor, Al 2 O 3 and SiO 2 are preferred, and particularly preferred is SiO 2 . The number for x indicating the amount of the metal oxide is preferred within the range of 10 -5 ≦x≦0.1, from the viewpoint of the enhancement in the luminance of stimulated emission of the phosphor and of the afterglow characteristics thereof.
In the formula (I), the number for y indicating the amount of the divalent europium activator is preferred within the range of 10 -4 ≦y≦3×10 -2 , from the viewpoint of the enhancement in the luminance of stimulated emission of the phosphor.
The divalent europium activated complex halide phosphor employed in the present invention can be prepared, for instance, in the following process.
A mixture of starting materials for the phosphor is prepared by using at least an alkaline earth metal halide, a metal oxide source and a trivalent europium compound in specific amounts. Then, the mixture of starting materials for the phosphor is fired. The so fired product is pulverized and classified, if desired. For obtaining the homogeneous mixture of starting materials, it is preferred to prepare the mixture in the form of an aqueous suspension, and in this case the suspension is heated to dryness prior to the above-mentioned firing stage.
Particularly, the divalent europium activated complex halide phosphor employed in the invention is preferred to prepare in the following manner.
After preparing a mixture of starting materials comprising specific amounts of an alkaline earth metal halide, a metal oxide source and a trivalent europium compound, the mixture is fired at least two times and at least a portion of the metal oxide source is added to the fired product obtained after the first firing stage.
It has been found that the phosphor prepared in the above-described manner in which the firing is carried out in two stages shows stimulated emission of prominently high luminance.
Examples of the binder to be employed in the phosphor layer include: natural polymers such as proteins (e.g. gelatin), polysaccharides (e.g. dextran) and gum arabic; and synthetic polymers such as poly(vinyl butyral), poly(vinyl acetate), nitrocellulose, ethylcellulose, vinylidene chloride-vinyl chloride copolymer, poly(methyl methacrylate). vinyl chloride-vinyl acetate copoymer, polyurethane, cellulose acetate butyrate, poly(vinyl alcohol), and linear polyester. Particularly preferred are nitrocellulose, linear polyester, and a mixture of nitrocellulose and linear polyester.
The phosphor layer can be formed on a support, for instance, by the following procedure.
In the first place, the phosphor particles and a binder are added to an appropriate solvent, and then they are mixed to prepare a coating dispersion of the phosphor particles in the binder solution.
Examples of the solvent employable in the preparation of the coating dispersion include lower alcohols such as methanol, ethanol, n-propanol and n-butanol; S5 chlorinated hydrocarbons such as methylene chloride and ethylene chloride; ketones such as acetone, methyl ethyl ketone and methyl isobutyl ketone; esters of lower alcohols with lower aliphatic acids such as methyl acetate, ethyl acetate and butyl acetate; ethers such as dioxane, ethylene glycol monoethylether and ethylene glycol monoethyl ether; and mixtures of the above-mentioned compounds.
The ratio between the binder and the phosphor in the coating dispersion may be determined according to the characteristics of the aimed radiation image storage panel and the nature of the phosphor employed. Generally, the ratio therebetween is within the range of from 1:1 to 1:100 (binder : phosphor, by weight), preferably from 1:8 to 1:40.
The coating dispersion may contain a dispersing agent to assist the dispersibility of the phosphor particles therein, and also contain a variety of additives such as a plasticizer for increasing the bonding between the binder and the phosphor particles in the phosphor layer. Examples of the dispersing agent include phthalic acid, stearic acid, caproic acid and a hydrophobic surface active agent. Examples of the plasticizer include phosphates such as triphenyl phosphate, tricresyl phosphate and diphenyl phosphate; phthalates such as diethyl phthalate and dimethoxyethyl phthalate; glycolates such as ethylphthalyl ethyl glycolate and butylphthalyl butyl glycolate; and polyesters of polyethylene glycols with aliphatic dicarboxylic acids such as polyester of triethylene glycol with adipic acid and polyester of diethylene glycol with succinic acid.
The coating dispersion containing the phosphor particles and the binder prepared as described above is applied evenly to the surface of a support to form a layer of the coating dispersion. The coating procedure can be carried out by a conventional method such as a method using a doctor blade, a roll coater or a knife coater.
The support material employed in the present invention can be selected from those employed in the conventional radiographic intensifying screens. Examples of the support material include plastic films such as films of cellulose acetate, polyester, poly(ethylene terephthlate), polyamide, polyimide, triacetate and polycarbonate; metal sheets such as aluminum foil and aluminum alloy foil; ordinary papers; baryta paper; resin-coated papers; pigment papers containing titanium dioxide or the like; and papers sized with poly(vinyl alcohol) or the like. From a viewpoint of characteristics of a radiation image storage panel as an information recording material, a plastic film is preferably employed as the support material of the invention. The plastic film may contain a light-absorbing material such as carbon black, or may contain a light-reflecting material such as titanium dioxide. The former is appropriate for preparing a high sharpness type radiation image storage panel, while the latter is appropriate for preparing a high sensitive type radiation image storage panel.
In the preparation of a known radiation image storage panel, one or more additional layers are occasionally provided between the support and the phosphor layer, so as to enhance the adhesion between the support and the phosphor layer, or to improve the sensitivity of the panel or the quality of an image provided thereby For instance, a subbing layer or an adhesive layer may be provided by coating a polymer material such as gelatin over the surface of the support on the phosphor layer side. Otherwise, a light-reflecting layer or a light-absorbing layer may be provided by forming a polymer material layer containing a light-reflecting material such as titanium dioxide or a light-absorbing material such as carbon black. In the invention, one or more of these additional layers may be provided depending on the type of the radiation image storage panel to be obtained.
As described in Japanese Patent Application No. 57(1982)-82431 (which corresponds to U.S. patent application No. 496,278 and the whole content of which is described in European Patent Publication No. 92241), the phosphor layer side surface of the support (or the surface of an adhesive layer, light-reflecting layer, or light-absorbing layer in the case that such layers are provided on the phosphor layer) may be provided with protruded and depressed portions for enhancement of the sharpness of radiographic image, and the constitution of those protruded and depressed portions can be selected depending on the purpose of the radiation image storage panel.
After applying the coating dispersion to the support as described above, the coating dispersion is then heated slowly to dryness so as to complete the formation of a phosphor layer. The thickness of the phosphor layer varies depending upon the characteristics of the aimed radiation image storage panel, the nature of the phosphor, the ratio between the binder and the phosphor, etc. Generally, the thickness of the phosphor layer is within the range of from 20 μm to 1 mm, preferably from 50 to 500 μm.
The phosphor layer can be provided on the support by methods other than that given in the above. For instance, the phosphor layer is initially prepared on a sheet (false support) such as a glass plate, metal plate or plastic sheet using the aforementioned coating dispersion and then thus prepared phosphor layer is overlaid on the genuine support by pressing or using an adhesive agent.
The phosphor layer placed on the support can be in the form of a single layer or in the form of plural (two or more) layers. When the plural phosphor layers are placed, at least one layer contains the aforementioned divalent europium activated complex halide phosphor having the formula (I), and the plural layers may be placed in such a manner that a layer nearer to the surface shows stimulated emission of higher luminance. In any case, namely, in either the single phosphor layer or plural phosphor layers, a variety of known stimulable phosphors are employable in combination with the above-mentioned stimulable phosphor.
Examples of the stimulable phosphor employable in combination with the above-mentioned stimulable phosphor in the radiation image storage panel of the present invention include the phosphors described hereinbefore and the phosphors described below;
ZnS:Cu,Pb, BaO.xAl 2 O 3 :Eu, in which x is a number satisfying the condition of 0.8≦x≦10, and M 2+ O. xSiO 2 :A in which M 2+ is at least one divalent metal selected from the group consisting of Mg, Ca, Sr, Zn, Cd and Ba, A is at least one element selected from the group consisting of Ce, Tb, Eu, Tm, Pb, Tl, Bi and Mn, and x is a number satisfying the condition of 0.5≦x≦2.5, as described in U.S. Pat. No. 4,326,078;
(Ba 1-x-y , Mg x , Ca y ) FX:aEu 2+ , in which X is at least one element selected from the group consisting of Cl and Br, x and y are numbers satisfying the conditions of 0≦x+y≦0.6, and xy=0, and a is a number satisfying the condition of 10 -6 ≦a≦5×10 -2 , as described in Japanese Patent Provisional Publication No. 55(1980)-12143; and
LnOX:xA, in which Ln is at least one element selected from the group consisting of La, Y, Gd and Lu, X is at least one element selected from the group consisting of Cl and Br, A is at least one element selected from the group consisting of Ce and Tb, and x is a number satisfying the condition of 0<x<0.1, as described in the above-mentioned U.S. Pat. No. 4,236,078.
A radiation image storage panel generally has a transparent film on a free surface of a phosphor layer to physically and chemically protect the phosphor layer. In the panel of the present invention, it is preferable to provide a transparent film for the same purpose.
The transparent film can be provided on the phosphor layer by coating the surface of the phosphor layer with a solution of a transparent polymer such as a cellulose derivative (e.g. cellulose acetate or nitrocellulose), or a synthetic polymer (e.g. poly(methyl methacrylate), poly(vinyl butyral), poly(vinyl formal), polycarbonate, poly(vinyl acetate), or vinyl chloride vinyl acetate copolymer), and drying the coated solution. Alternatively, the transparent film can be provided on the phosphor layer by beforehand preparing it from a polymer such as poly(ethylene terephthalate), polyethylene, poly(vinylidene chloride) or polyamide, followed by placing and fixing it onto the phosphor layer with an appropriate adhesive agent. The transparent protective film preferably has a thickness within the range of approximately 3 to 20 μm.
The present invention will be illustrated by the following examples, but these examples by no means restrict the invention.
EXAMPLE 1
175.4 g. of barium fluoride (BaF 2 ) and 333.3 g. of barium bromide (BaBr 2 .2H 2 O) were mixed well using an alumina mortar for 30 min. and heated to 150° C. for 2 hours to produce barium fluorobromide (BaFBr). To the barium fluorobromide was added a hydrobromic acid solution (HBr; 47 weight %) containing 0.352 g. of europium oxide (Eu 2 O 3 ), and the resultant was mixed well to give a suspension. The suspension was dried at 130° C. under reduced pressure for 2 hours. The dried product was pulverized using an automortar made of highly pure alumina for 1 hour to obtain a mixture of barium fluorobromide and europium bromide (EuBr 3 ). To the mixture was added 0.617 g. of sodium bromide and the resultant was mixed to prepare a mixture of starting materials for a phosphor.
100 g. of the mixture of starting materials was then placed in a quartz boat, which was, in turn, placed in a tubular furnace for carrying out the first firing. The first firing was conducted at 900° C. for 2 hours in a stream of nitrogen gas containing 3 weight % of hydrogen gas flowing at the rate of 300 ml/min. After the firing was complete, thus fired product was taken out of the furnace and allowed to stand for cooling.
Subsequently, the product obtained in the above first firing stage was pulverized for 20 hours by means of an alumina ball mill. To the pulverized fired product was then added 0.1 g. of silicon dioxide (0.0039 mol. per 1 mol. of barium fluorobromide; the same expression shall be employed in the examples hereinafter), and the resultant was mixed using a V-type blender. The mixture was again placed in a quartz boat and fired in a tubular furnace for carrying out the second firing. The second firing was conducted at 600° C. for 2 hours in the same stream as employed in the first firing stage. After the second firing stage was complete, the fired product was taken out of the furnace and allowed to stand for cooling to obtain a powdery divalent europium activated complex halide phosphor containing SiO 2 (BaFBr.0.003NaBr.0.0039SiO 2 :0.001Eu 2+ ).
EXAMPLE 2
The procedure of Example 1 was repeated except that a mixture of starting materials for a phosphor was prepared by adding 0.473 g. of silicon dioxide (0.039 mol.) as well as 0.617 g. of sodium bromide to the mixture of barium fluorobromide and europium bromide, to obtain a powdery divalent europium activated complex halide phosphor containing SiO 2 (BaFBr.0.003NaBr.0.0078SiO 2 :0.001Eu 2+ ).
EXAMPLE 3
The procedure of Example 3 was repeated except that 0.473 g. of silicon dioxide (0.0039 mol.) as well as 0.617 g. of sodium bromide was added to the mixture of barium fluorobromide and europium bromide to prepare a mixture of starting materials for a phosphor, and that the addition of silicon dioxide to the product of the first firing stage was omitted, to obtain a powdery divalent europium activated complex halide phosphor containing SiO 2 (BaFBr.0.003NaBr.0.0039SiO 2 :0.001Eu 2+ ).
COMPARISON EXAMPLE 1
The procedure of Example 1 was repeated except that the addition of silicon dioxide to the produce of the first firing stage was omitted, to obtain a powdery divalent europium activated complex halide phosphor (BaFBr.0.003NaBr:0.001Eu 2+ ).
The phosphors prepared in Examples 1 through 3 and Comparison Example 1 were measured on the luminance of stimulated emission when excited with a He-Ne laser (oscillation wavelength: 632.8 nm) after exposure to X-rays at the voltage of 80 KVp, to evaluate the luminance of stimulated emission thereof.
The results on the evaluation of the phosphors are set forth in Table 1. The amount of SiO 2 introduced into the phosphor is expressed in a molar ratio to 1 mol. of barium fluorobromide (BaFBr).
TABLE l______________________________________ Amount of SiO.sub.2 Relative Before FF After FF Luminance______________________________________Example 1 0 0.0039 140 2 0.0039 0.0039 130 3 0.0039 0 120Com. Ex. 1 0 0 100______________________________________ Remark: "Before FF" means "SiO.sub.2 added in the stage of preparation of the mixture before the first firing stage", and "After FF" means "SiO.sub.2 added after the first firing stage"; the same expression shall be used hereinafter.
EXAMPLE 4
The procedure of Example 1 was repeated except for adding 0.1 g. of aluminum oxide (Al 2 O 3 ;0.0023 mol.) instead of 0.1 g. of silicon dioxide (0.0039 mol.) to the product of the first firing stage, to obtain a powdery divalent europium activated complex halide phosphor containing Al 2 O 3 (BaFBr.0.003NaBr.0.0023Al 2 O 3 :0.001Eu 2+ ).
EXAMPLE 5
The procedure of Example 1 was repeated except for adding 0.1 g. of magnesium oxide (MgO; 0.0059 mol.) instead of 0.1 g. of silicon dioxide (0.0039 mol.) to the product of the first firing stage, to obtain a powdery divalent europium activated complex halide phosphor containing MgO (BaFBr.0.003NaBr.0.0059MgO:0.001Eu 2+ ).
EXAMPLE 6
The procedure of Example 1 was repeated except for adding 0.1 g. of calcium oxide (CaO; 0.0042 mol.) instead of 0.1 g. of silicon dioxide (0.0039 mol.) to the product of the first firing stage, to obtain a powdery divalent europium activated complex halide phosphor containing CaO (BaFBr.0.003NaBr.0.0042CaO:0.001Eu 2+ ).
The phosphors prepared in Examples 4 through 6 were measured on the luminance of stimulated emission when excited with a He-Ne laser (oscillation wavelength: 632.8 nm) after exposure to X-rays at the voltage of 80 KVp, to evaluate the luminance of stimulated emission thereof.
The results on the evaluation of the phosphors are set forth in Table 2. The aforementioned result on the evaluation of the phosphor prepared in Comparison Example 1 is also set forth in Table 2. The amount of the metal oxide introduced into the phosphor is expressed in a molar ratio to 1 mol. of BaFBr.
TABLE 2______________________________________ Amount Added To Relative Metal Oxide Fired Product Luminance______________________________________Example 4 Al.sub.2 O.sub.3 0.0023 135 5 MgO 0.0059 120 6 CaO 0.0042 120Com. Ex. 1 None 0 100______________________________________
EXAMPLE 7
The procedure of Example 1 was repeated except that a mixture of starting materials for a phosphor was prepared by adding 1.01 g. of beryllium bromide instead of 0.617 g. of sodium bromide to the mixture of barium fluorobromide and europium bromide, to obtain a powdery divalent europium activated complex halide phosphor containing SiO 2 (BaFBr.0.003BeBr 2 .0.0039SiO 2 :0.001Eu 2+ ).
EXAMPLE 8
The procedure of Example 1 was repeated except that a mixture of starting materials for a phosphor was prepared by adding 1.60 g. of aluminium bromide instead of 0.617 g. of sodium bromide to the mixture of barium fluorobromide and europium bromide, to obtain a powdery divalent europium activated complex halide phosphor containing SiO 2 (BaFBr.0.003AlBr 3 .0.0039SiO 2 :0.001Eu 2+ ).
The phosphors prepared in Examples 7 and 8 were measured on the luminance of stimulated emission when excited with a He-Ne laser (oscillation wavelength: 632.8 nm) after exposure to X-rays at the voltage of 80 KVp, to evaluate the luminance of stimulated emission thereof.
The results on the evaluation of the phosphors are set forth in Table 3. The aforementioned result on the evaluation of the phosphor prepared in Example 1 is also set forth in Table 3. The amount of the metal halide is expressed in a molar ratio to 1 mol. of BaFBr.
TABLE 3______________________________________ Relative Metal Halide Amount Added Luminance______________________________________Example 7 BeBr 0.003 120 8 AlBr.sub.3.sup.2 0.003 120 1 NaBr 0.003 140______________________________________
EXAMPLE 9
To a mixture of the powdery divalent europium activated complex halide phosphor containing SiO 2 (BaFBr.0.003NaBr.0.0039SiO 2 :0.001Eu 2+ ) obtained in Example 1 and a linear polyester resin were added successively methyl ethyl ketone and nitrocellulose (nitrification degree: 11.5%), to prepare a dispersion containing the phosphor and the binder (10:1, by weight). Subsequently, tricresyl phosphate, n-butanol and methyl ethyl ketone were added to the dispersion. The mixture was sufficiently stirred by means of a propeller agitater to obtain a homogeneous coating dispersion having a viscosity of 25-35 PS (at 25° C.).
The coating dispersion was applied to a polyethylene terephthalate sheet containing carbon black (support, thickness: 250 μm) placed horizontally on a glass plate. The application of the coating dispersion was carried out using a doctor blade. The support having a layer of the coating dispersion was then placed in an oven and heated at a temperature gradually rising from 25° to 100° C. Thus, a phosphor layer having thickness of 300 μm was formed on the support.
On the phosphor layer was placed a transparent polyethylene terephthalate film (thickness: 12 μm; provided with a polyester adhesive layer on one surface) to combine the transparent film and the phosphor layer with the adhesive layer.
Thus, a radiation image storage panel consisting essentially of a support, a phosphor layer and a transparent protective film was prepared.
COMPARISON EXAMPLE 2
The procedure of Example 9 was repeated except for using a powdery divalent europium activated barium fluorohalide phosphor (BaFBr:0.001Eu 2+ ) as a stimulable phosphor instead of the powdery divalent europium activated complex halide phosphor containing SiO 2 , to prepare a radiation image storage panel consisting essentially of a support, a phosphor layer and a transparent protective film.
The radiation image storage panels prepared in Example 9 and Comparison Example 2 were measured on the sensitivity when excited with a He-Ne laser (oscillation wavelength: 632.8 nm) after exposure to X-rays at the voltage of 80 KVp, to evaluate the sensitivity thereof.
The results on the evaluation of the panels are set forth in Table 4.
TABLE 4______________________________________ Relative Sensitivity______________________________________Example 9 100Com. Example 1 70______________________________________ | A radiation image recording and reproducing method comprising steps of:
causing a stimulable phosphor to absorb a radiation having passed through an object or radiated by an object,
exposing said stimulable phosphor to an electromagnetic wave having a wavelength within the range of 450-800 nm to release the radiation energy stored therein as light emission, and
detecting the emitted light,
in which said stimulable phosphor is a divalent europium activated complex halide phosphor having the formula (I):
M.sup.II FX.aM.sup.I X'.bM'.sup.II X".sub.2.cM.sup.III
X'" 3 .xA:yEu 2+ (I)
in which M II is at least one alkaline earth metal selected from the group consisting of Ba, Sr and Ca; M I is a least one alkali metal selected from the group consisting of Li, Na, K, Rb and Cs; M' II is at least one divalent metal selected from the group consisting of Be and Mg; M III is at least one trivalent metal selected from the group consisting of Al, Ga, In and Tl; A is at least one metal oxide; X is at least one halogen selected from the group consisting of Cl, Br and I; each of X', X" and X'" is at least one halogen selected from the group consisting of F, Cl, Br and I; a, b and c are numbers satisfying the conditions of 0≦a≦2, 0≦b≦10 -2 , 0≦c≦10 -2 and a+b+c≧10 -6 ; and x and y are numbers satifying the conditions of 0<x≦0.5 and 0<y≦0.2, respectively. A radiation image storage panel employed for the method is also disclosed. | 2 |
This Application: is a continuation of application Ser. No. 09/011,910, filed: Feb. 17, 1998, which is a National Stage regular U.S. Application claiming priority of PCT/IB96/00943, filed, Aug. 30, 1996, which claims priority of GBRI 9517926.3, filed, Sep. 1, 1995, all applications, incorporated by reference in their entireties. This application claims benefit of International Application No. PCT/IB96/00943; filed on Aug. 30, 1996, which was published under PCT Article 21(2) in English.”
FIELD OF THE INVENTION
The present invention relates to proteins capable of binding the E2 envelope protein of hepatitis C virus (HCV) and to processes for production and purification.
The invention also relates to the use of the proteins in therapy and diagnosis and to pharmaceutical compositions and diagnostic kits for such uses. The invention also relates to a process for screening putative molecules for competition with HCV for receptor binding. The invention also relates to an animal model for HCV infection.
BRIEF DESCRIPTION OF THE PRIOR ART
HCV (previously known as Non-A Non-B hepatitis—NANBV)is a positive sense RNA virus of about 10000 nucleotides with a single open reading frame encoding a polyprotein of about 3000 amino acids. Although the structure of the virus has been elucidated by recombinant DNA techniques (1, 2), the virus itself has not been isolated and the functions of the various viral proteins produced by proteolysis of the polyprotein have only been inferred by analogy with other similar viruses of similar genomic organisation (3).
The viral proteins are all available in recombinant form, expressed in a variety of cells and cell types, including yeast, bacteria, insect and mammalian cells (4,5).
Two proteins, named E1 and E2 (corresponding to amino acids 192-383 and 384-750 respectively) have been suggested to be external proteins of the viral envelope which are responsible for the binding of virus to target cells (3).
HCV research is hindered very considerably by the limited host range of the virus. The only reliable animal model for HCV infection is the chimpanzee and it is not possible to propagate HCV in tissue culture.
In our copending International patent application PCT/IB95/00692, we describe a method employing flow cytometry to identify cells carrying the HCV receptor. We have shown that, by labelling cells with recombinant E2 envelope protein, it is possible to sort cells using flow cytometry, isolating those cells capable of specific binding to the E2 and therefore potentially carrying the HCV receptor. Employing this technique, we have identified a protein capable of binding to the E2 envelope protein of HCV which we believe to be the receptor for HCV, thereby enabling overcoming many problems in the art.
SUMMARY OF THE INVENTION
According to the present invention, there is provided a protein having a molecular weight of about 24 kD and capable of specifically binding to a protein of hepatitis C virus, or a functionally equivalent variant or fragment thereof.
It will be understood by the skilled person that molecular weights measured as described below using electrophoresis are inherently subject to interpretation since they are measured relative to standard molecular weight markers. However, in the context of this specification the expression “24 kd” is unambiguous when read in context, since only one such protein is obtained by following the processes described below with the defined characteristic of binding to hepatitis C virus.
A significant characterising feature of the protein according to the present invention is its ability to bind specifically to an HCV protein, preferably an envelope protein, particularly the E2 protein.
On the basis of this specificity and other features described below, we infer that the 24 kd protein of the invention is a cellular receptor for HCV.
We have shown that the protein is ubiquitous in humans amongst the cell types we have tested, paralleling the situation found for many other viruses of this type (such as vaccinia virus and influenza virus).
We have shown that the protein is species specific in a manner which matches the species specificity of HCV itself.
Our experiments have shown that the 24 kd protein is functionally unglycosylated. Treatment with glycosidases does not affect the ability of the 24 kd protein to bind to the E2 protein and does not appear significantly to reduce the molecular weight. We infer therefore that, if the protein is glycosylated at all, glycosylation must be restricted to a small number of sugar moieties and is not necessary for functional activity of the protein.
Our experiments have also shown that the protein is a transmembrane protein, again suggesting that it is a cellular receptor.
Finally, experiments with cell lines hyperexpressing the protein indicate that such cells are prone to aggregation suggesting that the protein may be an adhesion molecule of some form.
The 24 kd protein may be in its naturally occurring form, albeit isolated from its native environment, or may be modified, provided that it retains the functional characteristic of at least binding to the E2 protein of HCV. For example, the 24 kd protein may be modified chemically to introduce one or more chemical modifications to the amino acid structure. It may include modifications of the amino acid sequence involving one or more insertions, deletions or replaced amino acids. It may, for example, be truncated by the removal of a functional part of the transmembrane domain to facilitate ready production by recombinant DNA means in a suitable mammalian host cell (6).
The protein of the present invention may be purified from cells exhibiting binding to an HCV protein, such as the E2 protein.
According to the present invention there is provided a process for the preparation of a protein according to the invention or a functionally equivalent variant or fragment thereof comprising the step of culturing cells exhibiting binding to an HCV protein and purifying from a cell preparation a protein according to the invention.
The cells may be transformed or untransformed mammalian cells and are suitably human cells.
The cells may be screened for binding to an HCV protein using fluorescence flow cytometry or any other suitable assay. For example, the present description provides the information necessary to produce the 24 kd protein or a functionally equivalent variant or fragment thereof which then itself be used to assay for further cells carrying the protein.
The cell preparation may be a cell membrane preparation but is preferably a plasma cell membrane preparation.
Preferably the cells are selected and cloned to provide hyperexpression of the protein of the present invention.
We have discovered that the protein is precipitated by ammonium sulphate at between 33 and 50% of saturation.
Preferably, therefore, the cell preparation is subjected to an ammonium sulphate precipitation purification step employing ammonium sulphate at between 33 and 50%. Suitably a first precipitation is conducted at less than 33% and precipitated material discarded followed by precipitation of the desired material at between 33 and 50%, most preferably 50%.
Preferably, the purification involves at least one step of hydrophobic interaction chromatography.
We have also discovered that the protein is stable to acetone precipitation, thereby providing a still further characterisation and a useful purification process step.
Most preferably in optimised form, the process of purification comprises the steps of:
i) preparing a plasma cell membrane preparation of mammalian cells selected for hyperexpression of the 24 kd protein of the invention,
ii) subjecting the preparation to ammonium sulphate precipitation at less than 33% saturation and retaining the supernatant,
iii) subjecting the supernatant to ammonium sulphate precipitation at between 33 and 50% saturation and retaining the precipitate, and
iv) resuspending the precipitate and subjecting it to hydrophobic interaction chromatography
As an alternative to purification from wild-type cell lines, the protein of the invention or a functionally equivalent variant or fragment thereof may be made by any suitable synthetic process including chemical synthesis. Suitably, the protein or a functionally equivalent variant or fragment thereof is made by expression of a gene encoding the protein in a suitable host cell or animal.
According to a further aspect of the invention, there is provided a method for treating an infection of HCV comprising administering to a patient an amount of the protein of the invention or a functionally equivalent variant or fragment thereof effective to reduce the infectivity of the virus.
Since the infection mechanism of HCV appears to depend, in part, upon the availability of a cell surface receptor, making available a soluble form of the protein of the invention will act as an antagonist of binding of HCV to the cellular receptor thus reducing or preventing the infection process and thereby treating the disease.
A suitable form of the protein of the invention might comprise, for example, a truncated form of the protein from which the transmembrane domain has been removed either by a protein cleavage step or, by design, in a chemical or recombinant DNA synthesis.
Alternatively, a hybrid particle comprising at least one particle-forming protein, such as hepatitis B surface antigen or a particle-forming fragment thereof, in combination with the protein of the invention or a functionally equivalent variant or fragment thereof could be used as an antagonist of binding of HCV to the cellular receptor.
According to a further aspect of the invention, there is provided a pharmaceutical composition comprising a protein of the invention or a functionally equivalent variant or fragment thereof, optionally as a pharmaceutically acceptable salt, in combination with a pharmaceutically acceptable carrier.
The pharmaceutical composition may be in any appropriate form for administration including oral and parenteral compositions.
A process is also provided for making the pharmaceutical composition, in which a protein of the present invention or a functionally equivalent variant or fragment thereof is brought into association with a pharmaceutically acceptable carrier.
According to a further aspect of the invention, there is provided a protein of the invention or a functionally equivalent variant or fragment thereof for use as a pharmaceutical.
According to a further aspect of the invention, there is provided the use of a protein of the invention or a functionally equivalent variant or fragment thereof in the manufacture of a medicament for the treatment of an HCV infection.
The ability of a protein of the invention or a functionally equivalent variant or fragment thereof to bind to HCV permits the use of the protein or a functionally equivalent variant or fragment thereof as a diagnostic for HCV infection, for example in an ELISA or RIA.
A soluble form of the protein could, for example, be used in an ELISA form of assay to measure neutralising antibodies in serum.
According to a further aspect of the invention, there is provided an assay for HCV antibodies in a serum sample comprising the step of allowing competitive binding between antibodies in the sample and a known amount of an HCV protein for binding to a protein of the invention or a functionally equivalent variant or fragment thereof and measuring the amount of the known HCV protein bound.
Preferably, the protein of the invention or functionally equivalent variant or fragment thereof is immobilised in a solid support and the HCV protein, which may suitably be E2 HCV envelope protein, optionally recombinant E2 protein, is labelled, suitably enzyme labelled.
In an assay of this form, competitive binding between antibodies and the HCV protein for binding to the protein of the invention results in the bound HCV protein being a measure of antibodies in the serum sample, most particularly, neutralising antibodies in the serum sample.
A significant advantage of the assay is that measurement is made of neutralising antibodies directly (i.e those which interfere with binding of HCV envelope protein to the cellular receptor). Such an assay, particularly in the form of an ELISA test has considerable applications in the clinical environment and in routine blood screening.
Also, since the assay measures neutralising antibody titre, the assay forms a ready measure of putative vaccine efficacy, neutralising antibody titre being correlated with host protection.
In a further aspect of the invention, there is provided a diagnostic kit comprising the protein of the invention or a functionally equivalent variant or fragment thereof. Preferably the kit also contains at least one HCV labelled HCV protein, optionally enzyme labelled.
The protein of the invention or a functionally equivalent variant or fragment thereof may be used to screen for chemical compounds mimicking the HCV surface structure responsible for binding to the HCV receptor.
According to a further aspect of the invention, there is provided a method for screening chemical compounds for ability to bind to the region of HCV responsible for binding to a host cell, comprising measuring the binding of a chemical compound to be screened to a protein of the invention or a functionally equivalent variant or fragment thereof.
This aspect of the invention encompasses the products of the screening process whether alone, in the form of a pharmaceutically acceptable salt, in combination with one or more other active compounds and/or in combination with one or more pharmaceutically acceptable carriers. Processes for making a pharmaceutical composition are also provided in which a chemical compound identified by the process of the invention is brought into association with a pharmaceutically acceptable carrier.
The chemical compound may be an organic chemical and may contain amino acids or amino acid analogues. Preferably however the chemical compound is a polypeptide or a polypeptide which has been chemically modified to alter its specific properties, such as the affinity of binding to the protein of the invention or a functionally equivalent variant or fragment thereof or its stability in vivo.
At present, the only available animal model is the chimpanzee, which is a protected species. Experiments on such animals pose a number of difficulties which together result in a very considerable expense (a one year experiment with one chimpanzee can cost $70,000). Compared to this, a mouse model would be far more acceptable. Unfortunately, as described below the HCV receptor, whilst ubiquitous in humans and found in chimpanzees, is absent in other mammals. A transgenic mammal, for example a mouse, carrying the HCV receptor on the cell surface would be of great benefit to HCV research and the development of vaccines.
According to a further aspect of the invention, there is provided a transgenic non-human mammal, suitably a mouse, carrying a transgene encoding a protein of the invention or a functionally equivalent variant or fragment thereof.
The transgenic animal of the invention may carry one or more other transgenes to assist in maintaining an HCV infection.
There is also provided a process for producing a transgenic animal comprising the step of introducing a DNA encoding a protein of the invention or a functionally equivalent variant or fragment thereof into the embryo of a non-human mammal, preferably a mouse.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a schematic diagram describing an assay in which HCV receptor-binding ligands bind to receptors on HCV receptor target cells and are measured by first binding rabbit anti-HCV antibody and then by binding a labelled anti-rabbit IgG-FITC F(ab′) fragment prior to cell separation by FACScan analysis.
FIG. 2 is a computer-generated histogram depicting the results of a FACScan analysis of binding of HCV protein to haematopoietic cells (MOLT-4, Jurkat, K562, Daudi, EBV-B) and epithelial cells (Hela, Adenocarcinoma and Huh 7) resulting from binding with HCV proteins (filled curve unlabelled control, open curve labelled). The plot is of cell population against fluorescence intensity.
FIG. 3 is a computer-generated histogram depicting the results of a FACScan analysis of purified RA, purified RO, cord blood purif. RA, cord blood RA pha stim., KC3 T-cell clone (TCC) and SAG S9 TCC, which were tested for binding to recombinant HCV E2 protein expressed in CHO cells (filled curve unlabelled control, open curve labelled). The plot is of cell population against fluorescence intensity.
FIG. 4 is a set of computer-generated histograms depicting the results of a FACScan analysis of the binding of E2 CHO to MOLT-4 cells with and without treatment with beta mercaptoethanol (BSH) an S—S linkage reducing agent (filled curve unlabelled control, open curve labelled). The plot is of cell population against fluorescence intensity.
FIG. 5 is a set of computer-generated histograms depicting the results of a FACScan analysis of the binding of E2 CHO to MOLT-4 cells with and without treatment with Endo-H, a deglycosylating enzyme (filled curve unlabelled control, open curve labelled). The plot is of cell population against fluorescence intensity.
FIG. 6 is a western-blot of membranes prepared from MOLT-4 cells and solubilized in different buffers (see page 22 for lane descriptions).
FIG. 7 is a western blot of plasmatic membrane from MOLT-4 cells (see page 23 for lane descriptions).
FIG. 8 is a western blot of MOLT-4 and PBMC membrane proteins (see page 23 for lane descriptions).
FIG. 9 is a western blot of MOLT 4 cells membrane proteins treated with N-Glycosidase F (see page 26 for lane descriptions).
FIG. 10 is a western Blot of MOLT-4 and COS-7 membranes electrophoresed in reducing and non reducing conditions (see page for 27 lane descriptions).
FIG. 11 is a western blot of an experiment demonstrating immunoprecipitation of an E2-CHO/putative receptor complex (see page 29 for lane descriptions).
FIG. 12 is a western blot of ammonium sulphate fractions from MOLT-4 cells membranes (see page 31 for lanes).
FIG. 13 is a western blot of samples from a hydrophobic interaction chromatography experiment with an acetone precipitation step (see page 32 for lanes).
DETAILED DESCRIPTION OF THE INVENTION
The arrangement of the detailed description is as follows:
1.
General Description
13
2.
Cellular Assay
13
2.1.
FACS analysis of cells binding to E2
13
2.2.
Effect of E2 modification on binding
15
2.2.1.
E2 reduction
16
2.2.2.
E2 deglycosylation
16
2.3.
Monoclonal antibody production
17
3.
Preparation of 24 kd putative receptor
17
3.1.
24 kd protein preparation from MOLT-4 cells
17
3.1.1.
Membrane purification
17
3.1.2.
Plasma membrane purification
18
3.2.
Hyperexpressing MOLT-4 cells
20
4.
Characterisation of Receptor
20
4.1.
Western blot protocol
20
4.1.1.
Membrane proteins
21
4.1.2.
Plasma membrane proteins
22
4.1.3.
Western blot of PBMC cells
23
4.2.
Cell surface expression of receptor
23
4.3.
Effect of enzymes on 24 kd protein binding
24
4.3.1.
Flow cytometry
24
4.3.2.
Western blot on MOLT-4/N-Glycosidase F
26
4.4.
Effect of reducing condition on binding
26
5.
Optimising Purification
27
5.1.
Immunoprecipitation
27
5.2.
Ammonium Sulphate Fractionation
30
5.3.
Hydrophobic Interaction Chromatography
31
5.4.
Acetone precipitation
32
6.
Sequencing and cloning
33
6.1.
Amino acid sequence
33
6.2.
DNA sequence cloning and sequencing
33
1. General Description
The practice of the present invention will employ, unless otherwise indicated, conventional techniques of immunology, cytofluorimetry and molecular biology, which are within the skill of the art. Such techniques are explained fully in the literature (7).
The skilled person will understand and be familiar with the general methods and techniques of assay design and practice. The invention is described herein in sufficient detail for the skilled person to understand and repeat the experiments disclosed.
Standard abbreviations for virus and proteins are used in this specification. All publications, patents and patent applications cited herein are incorporated by reference. Envelope 1 (E1) and Envelope 2 (E2) of HCV refer to the proteins, and fragments thereof, the nucleotide sequence of which are published (EP-A-0318216 and EP-A-0388232 cited above). The nucleotides of the E1 and E2 genes and of the encoded proteins vary in different HCV isolates. Therefore, the E1 and E2 for any HCV isolates are identified because included in the amino acid sequences 192-383 and 384-750 respectively.
E1 and E2 have been produced by recombinant DNA techniques using different expression systems (Spaete et al and Chien et al cited above).
2. Cellular Assay
2.1. FACS Analysis of Cells Binding to E2
An experiment was performed with the aim of measuring the ability of HCV protein to bind to various cell types which should have the putative HCV receptor.
Cells (10 5 /well) from the human T cell lymphoma, Molt-4 (commercially available and obtainable from the American Type Culture Collection), were pelleted in 96 U-bottom microplates (Costar) by centrifugation at 200× g for 5 minutes at 4° C. Twenty microliters of HcV proteins (CHO expressed recombinant E2 protein) diluted in PBS in different concentrations (from 10 μg/ml to 0.001 μg/ml) were mixed with the pellet of Molt-4 cells and incubated at 4° C. for 60 minutes. Non bound HCV proteins were removed by two centrifugations in PBS at 200× g for 5 minutes at 4° C.
Cells were subsequently incubated for 30 minutes at 4° C. with various dilutions (from 1/10 to 1/300000) of sera from humans, chimps, rabbits or mice that were either infected with HCV or have been immunised with HCV recombinant proteins or the corresponding pre-immune sera as control.
The cells were washed twice in PBS and incubated for 30 minutes with the appropriate dilutions of fluorescein-isothiocyanate-conjugated antisera (either to human IgG, or rabbit IgG, or mouse IgG).
Cells were subsequently washed in PBS at 4° C., resuspended in 100 μl PBS and cell-bound fluorescence was analyzed with a FCScan flow cytometer (Becton & Dickinson). By using a dot plot display of forward and side scatter, the machine is gated to include viable single cells and to exclude cell debris and clumps of cells. A total of 5000 events were collected and analyses of the data was done by using the Lysis II software program from Becton & Dickinson. This program produces histograms of each cell sample and calculates the mean channel fluorescence of the cell population, which directly relates to the surface density of fluorescently labelled HCV proteins bound to the cells.
Mean fluorescence values (mean channel number) of cells incubated with or without HCV proteins and with immune or preimmune sera were compared. The threshold for positivity is set for each experiment by flow cytometric analysis of cells without HCV proteins bound which have been incubated with antisera to HCV proteins and the FITC labelled second antibody. A representative binding experiment is shown in FIG. 1 which shows the separation achieved by flow cytometric analysis.
The experiment was also conducted with a variety of cell lines (for example haematopoietic cells other than MOLT-4 such as Jurkat, K562, Daudi, EBV-B (B-cell line transformed with Epstein-Barr virus and epithelial cells such as Hela, Adenocarcinoma and Huh 7) to identify cells capable of binding HCV proteins and therefore cells that have the putative receptor(s) for HCV following the protocol described above. It will be appreciated that repetition of this experiment is not necessary for the working of the present invention, but serves to prove the ubiquitous nature of the putative receptor (most of the cells are, in any event commonly available and were, in fact, obtained from the ATCC). The results were shown in FIG. 2, together with those for MOLT-4 and demonstrate that the specific binding of E2 to cells is widespread, suggesting that the HCV receptor is ubiquitous.
In a similar series of experiments, purified RA, purified RO, cord blood purif. RA, cord blood RA pha stim., KC3 TCC and SAG S9 TCC, which were tested for binding to recombinant HCV E2 protein expressed in CHO cells (E2-CHO) and found to bind confirming that binding occurs to non-transformed cell lines. The results are shown in FIG. 3 .
2.2. Effect of E2 Modification on Binding
The effects of modifying the recombinant HCV protein E2, expressed in CHO cells (E2-CHO) on binding to MOLT-4 cells were investigated using a reducing agent and a deglycosylating enzyme.
2.2.1. E2 Reduction
25 μl of E2-CHO SMC-PC (130 μg/ml) in 20 mM potassium phosphate, 0.1 M NaCl, pH 6.0 were buffered at pH 8.0 with 1M Tris-base (total 1 μl) and then added with BSH (beta mercaptoethanol) to a final concentration of 500 mM; tubes were flushed with nitrogen and the reaction allowed to proceed for 100 minutes at 37° C.
Samples from above were diluted 1:20 with RPMI medium and used for a FACS binding assay with MOLT-4 cells as described above. The final concentration of BSH in the FACS assay was 12.5 mM and under these conditions, cells were verified to be alive in previous preliminary experiments (over 90% of cells still alive at 50 mM BSH).
The results in FIG. 4 show that binding of MOLT-4 cells to recombinant E2 is substantially reduced on reduction with beta-mercaptoethanol, indicating a requirement for a correct E2 conformation maintained by S—S bridges.
2.2.2. E2 Deglycosylation
25 μl of E2-CHO SMC-PC (130 μg/ml) in 20 mM potassium phosphate, 0.1 M NaCl, pH 6.0 were added with 30 μl of 0.2 M NaH 2 PO 4 to a final pH of 5.5 plus SDS to a final concentration of 0.01%. Then 10 μl of Endo-H stock was added to a final concentration of 200 mU/ml keeping the pH constant and the resulting sample was kept at 37° C. for 20 hours. The sample was then diluted 1:20 with RPMI and used for in a FACS binding assay as described above.
The results in FIG. 5 show that binding of MOLT-4 cells to recombinant E2 is substantially reduced on deglycosylation with Endo-H, indicating a requirement for glycosylation of E2 for binding.
2.3. Monoclonal Antibody Production
Monoclonal antibodies were prepared using standard procedures and by immunising mice with recombinant HCV E2 produced in CHO cells (E2-CHO). Several cell lines were established which were capable of binding to E2-CHO as were cell lines capable of binding to E2 bound to MOLT-4 cells and cell lines capable of neutralising the binding of E2-CHO to MOLT-4 cells.
3. Preparation of 24 kd Putative Receptor
3.1. 24 kd Protein Preparation from MOLT-4 Cells
The 24 kd protein was purified from MOLT-4 cells by membrane purification and by plasma membrane purification, the latter giving the better yield of protein.
3.1.1.Membrane Purification
MOLT-4 cells were grown at 37° C., 5% CO 2 in RPMI buffered with 25 mM Hepes in a growth medium containing Fetal Calf Serum (FCS—final concentration 5%), 1 mM glutamine, 100 μg/ml kanamicin, MEM vitamins (Gibco), 1 mM sodium pyruvate, MEM non essential amino acids (Gibco), 5×10 −5 M β-mercaptoethanol.
Cells were harvested after reaching a density of 750,000-1,000,000 cells per ml.
The growth medium containing cells was centrifuged at 300 g for 10 minutes to pellet down the cells. Pelleted cells were washed three times in PBS Buffer (resuspended and recentrifuged).
The cell pellet was resuspended in hypotonic solution at 1 ml of hypotonic solution per 100×10 6 cells.
The hypotonic solution contained Tris (10 mM), NaCl (10 mM), CaCl 2 (0.2 mM), MgCl 2 (1.5 mM), PMSF (1.0 mM), aprotinin (2.0 μg/ml), pepstatin (0.7 μg/ml) and leupeptin (0.5 μg/ml).
Cells were left at 4° C. under gentle shaking for 20 minutes and then disrupted with 25 strokes of a Potter manual homogenizer.
Membranes were recovered after sequential centrifugation of the supernatant at 100 g for 7 minutes, 3500 g for 10 minutes and 40,000 g for 60 minutes. The pellet obtained from the above was dissolved in suitable buffer.
The buffer used for dissolution of the 40,000 g membrane pellet contained 1% Triton X-100 in PBS buffer pH 7.4, 8 mM Chaps in PBS buffer pH 7.4 and 4 M Urea in sodium phosphate buffer pH 7.4.
All the buffers used for membrane solubilisation contained protease inhibitors at the concentrations reported above for the hypotonic solution and were used at a ratio of 200 μl of buffer per 5×10 8 cells.
Solubilised material was centrifuged at 100,000 g for 60 minutes and the supernatant kept for further use after estimation of protein content by BCA method.
The material obtained was subjected to analyses as described below.
3.1.2. Plasma Membrane Purification
The procedure for plasma membrane purification was based on Morre' D. J. et al. (8).
MOLT-4 cells were grown at 37° C., 5% CO 2 in RPMI buffered with 25 mM Hepes in a growth medium containing Fetal Calf Serum (FCS—final concentration 5%), 1 mM glutamine, 100 μl/ml kanamicin, MEM vitamins (Gibco), 1 mM sodium pyruvate, MEM non essential amino acids (Gibco), 5×10 −5 M β-mercaptoethanol.
Cells were pelleted from culture medium and washed three times with PBS.
The pelleted cells were resuspended in 0.2 mM EDTA, 1 mM NaHCO 3 containing the following protease inhibitors: PMSF (1.0 mM), aprotinin (2.0 μg/ml), pepstatin (0.7 μg/ml), leupeptin (0.5 μg/ml) at a ratio between buffer and cells of 2 ml per each 10 8 cells.
Resuspended cells were disrupted with a Polytron homogenizer using an S25 N10 G probe for 40 seconds at 9500 rpm. Cell disruption was verified by optical microscope. The homogenate was centrifuged at 300 g and the resulting supernatant further centrifuged at 23,500 g for 60 minutes. The resulting pellet was resuspended in 0.2 M potassium phosphate pH 7.2 containing protease inhibitors in the ratios described above. The buffer volume was 1 ml each 5×10 8 cells.
The membrane suspension was partitioned across the following two phase system:
20% (w/w) T500 Dextran
13.2
g
40% (w/w) PEG 3350
6.6
g
0.2 KP, pH 7.2
0.8
ml
membrane susp.
5.0
g
Distilled water
up to 35
g
The sample as chilled at 4° C. and the tubes were inverted 30 to 40 times keeping the temperature constant. The sample was then centrifuged on a swinging bucket rotor at 150-200 g for 5 minutes at 4° C. The upper phase was removed and five-fold diluted with 1 mM sodium bicarbonate containing protease inhibitors. The membranes were collected by centrifugation at 30,000 g for 30 minutes.
The pellet was dissolved in a suitable buffer and centrifuged at 100,000 g for 60 minutes to eliminate undissolved material.
The material obtained was subjected to analyses as described below.
3.2. Hyperexpressing MOLT-4 Cells
A further cell line capable of hyperexpression of the characteristic binding ability for E2 was prepared by selecting and recloning MOLT-4 cells binding E2 strongly. The resulting cell-line showed a markedly greater binding affinity for E2 than the wild-type strain.
4. Characterisation of Receptor
4.1. Western Blot Protocol
The following experiments demonstrate binding of E2 to purified 24 kd protein in a western blot of proteins from MOLT-4 cells purified from membranes and from plasma membranes and from peripheral blood mononuclear cells (PBMC).
Unless otherwise indicated, all SDS-PAGE experiments were performed according to Laemmli et al (9), samples of solubilised membranes were run under non-reducing conditions and without boiling before each electrophoretic run.
After electrophoretic transfer (Western blot) in buffer containing 25 mM Tris, 192 mM glycine, 20% methanol at constant electric field of 10 Volts/cm, blotted transfer supports were saturated for 2 hours in PBS buffer pH 7.4 containing 0.05% Tween 20 and 10% powdered skimmed milk at room temperature. After 1×15 minutes and 2×5 minutes, washes in PBS, 0.05% Tween 20 containing 1% powdered skimmed milk, transfer supports were incubated overnight with E2-CHO recombinant protein at a concentration of 1-2 μg/ml dissolved in PBS buffer containing 0.05% Tween 20, 1% milk, 0.02% sodium azide. Negative control transfer supports (blotted with the same samples) were incubated for the same time in the same buffer without E2-CHO protein.
To detect E2-CHO recombinant protein bound to the transfer supports, these were incubated with the culture supernatant of an hybridoma named 291A2 (a monoclonal antibody that recognises epitopes exposed on E2 when bound to its putative receptor) at 1:500 dilution in PBS, Tween 0.05%, milk 1% for 2 hours.
After this step, transfer supports were washed 1×15 minutes and 2×5 minutes with PBS Tween 0.05% milk 1% solution. Transfer supports were then incubated for 1 hour with biotin conjugated goat anti-mouse immunoglobulin specific polyclonal antibody of commercial source (PharMingen, San Diego, Calif., USA) at 1:2000 dilution in the PBS/Tween/Milk solution mentioned above. After this step, transfer supports were washed 1×15 minutes and 2×5 minutes with PBS/Tween/Milk. Finally transfer supports were incubated for 1 hour with Extravidin™-Peroxidase (Sigma Immunochemicals Co., St Louis, Mo., USA) at 1:2500 dilution in PBS/Tween/Milk. Transfer supports were then washed 1×15 minutes and 4×5 minutes with PBS buffer pH 7.4 containing 0.05% Tween 20. Chemiluminescent staining was performed using ECL™ western blotting detection reagents (Amersham, UK).
4.1.1. Membrane Proteins
A membrane preparation was prepared as described above.
Membrane pellets resulting from 40,000 g centrifugation were dissolved in buffers reported below and centrifuged at 100,000 g to remove undissolved material. Pellets were reextracted with 1% Triton X-100 in PBS pH 7.4.
Following SDS-PAGE (15 μg/lane) and blotting, the transfer supports were incubated with E2-CHO recombinant protein as described above.
The results are shown in FIG. 6 .
Lane
Description
1A
4M Urea in 50 mM sodium phosphate pH 7.2
2A
Pellet from lane 1A sample solubilized in 1%
Triton X-100 in PBS pH 7.4
3A
1% Triton X-100 in PBS pH 7.4
4A
Pellet from lane 3A sample solubilized in 1%
Triton X-100 in PBS pH 7.4
5A
0.01% Triton X-100 in PBS pH 7.4
6A
Pellet from lane 5A sample solubilized in 1%
Triton X-100 in PBS pH 7.4
1B to 6B are negative controls for the corresponding samples in lanes 1A to 6A.
The protein band at 24 kd is clearly visible.
4.1.2.Plasma Membrane Proteins
A plasma membrane preparation was prepared as described above.
Plasma membranes were solubilized in PBS pH 7.4 containing 1% Triton X-100 and subjected to Laemmli SDS-PAGE. The transfer support was incubated with E2-CHO recombinant protein.
The results are shown in FIG. 7 .
Lane
Description
1A
plasma membranes, 10 μg total protein content
2A
plasma membranes, 5 μg total protein content
Lanes 1B and 2B are negative controls for the corresponding samples in lanes 1A and 2A.
The protein band at 24 kd is clearly visible.
4.1.3. Western Blot of PBMC Cells
To assess whether the 24 kd protein could be identified in normal cells a sample of peripheral blood mononuclear cells was purified using the procedure described above and subjected to western blotting as described above.
The results are described in FIG. 8 .
Lane
Description
1/2
Molt-4 membrane proteins
3
PBMC membrane proteins (22 μg/ml)
4
PBMC membrane proteins (44 μg/ml)
The negative control lanes are marked “−E2 CHO”
4.2. Cell surface Expression of Receptor
Employing the protocols described above, various cell types were analysed using FACscan and western blotting for the presence of the 24 kd protein putative HCV receptor.
The results are depicted below:
FACS
W B
HCV
T and B lympho
human
+++
+++
+++
Monocytes
human
+++
+++
HeLa
human
++
+++
Gastric carcinoma
human
++
+++
Hepatoma cells
human
+++
+++
+++
Myoblastoma
human
+
−
Fresh liver cells
Green monkeys
−
−
−
Lymphomonocytes
rabbit
−
−
Fresh liver cells
rabbit
−
−
Any cells
mouse
−
−
These results demonstrate that the species distribution of the 24 kd protein matches that of HCV infection susceptibility.
4.3. Effect of Enzymes on 24 kd Protein Binding
4.3.1. Flow Cytometry
The biochemical nature of the cell surface component (receptor) that mediates attachment of E2 CHO envelope protein to Molt 4 cells was investigated. Pretreatment of Molt 4 cells with V. cholerae neuraminidase, which has a α-2,3 specificity does not reduce E2 CHO binding.
The proteinaceous nature of the receptor was demonstrated when cells pretreated with proteases abolished binding capability of E2 CHO whereas phospholipase treatment of cells did not affect the binding, suggesting that the cellular attachment proteins were not glycosylphosphatilylinositol anchor linked. The E2 binding site on Molt 4 cells was sensitive to all protease used, which included both serine proteases, such as trypsin, and a thiol protease, such as papain.
The results of proteolytic treatment demonstrated the involvement of membrane proteins in envelope protein binding and were as follows:
Fluorescence intensity
Treatment
Concentration
(% of control)
Control
100
Pronase E
10
μg/ml
36
Pronase E
100
μg/ml
34
Trypsin
100
μg/ml
33
Papain
100
μg/ml
42
Phospholipase C
3
U/ml
100
(from Bacillus
cereus )
Phospholipase C
25
U/ml
96
Neuraminidase
50
mU/ml
100
Cells (10 6 ml −1 ) were incubated for 60 min at 37° C. in RPMI 1640/Hepes medium plus the enzymes indicated above. The cells were centrifuged, resuspended in fresh medium and incubated with E2 CHO protein (3 μg/ml). Purified anti E2 CHO monoclonal antibody (1.5 μg/ml) was used as a second step. Purified phycoerythrin-labelled rabbit anti mouse antibody (5 μg/ml) was used as a third step reagent. A total of 5000 cells per sample was evaluated with a FACScan flow cytometer.
Enzymes were used at a concentration that did not affect cell viability as measured by propidium iodine exclusion during FACS analysis.
Fluorescence was recorded as arbitrary units (channel numbers) on a logarithmic scale and median intensities determined. Data from individual experiments were normalized with respect to the fluorescence of unstained control samples and value are expressed as percentages of the fluorescence intensities in the stained control samples.
4.3.2. Western Blot on MOLT-4/N-Glycosidase F
Peptide N-Glycosidase F treatment was performed incubating membrane proteins (50 μg) overnight at 37° C. in phosphate buffer pH 7,4,25 mM EDTA plus enzyme (50 U/ml) and successively loaded on 12% SDS PAGE.
To show the activity N-Glycosidase F enzyme (PNGase F), as control, gp 120 polypeptide was used in the same experiment (data not shown).
The results are shown in FIG. 9 .
Lane
Description
1
+/ve control
2
treated and boiled membrane
3
untreated and boiled membrane
4
treated membrane
5
untreated membrane
These results show that treatment of a MOLT 4 membrane preparation with Peptide-N-glycosidase F, which hydrolyzes all N-linked glycanes, does not abolish E2 CHO binding.
4.4. Effect of Reducing Condition on Binding
A western blot of MOLT-4 and COS-7 membranes, prepared as described above, were electrophoresed in reducing and non reducing conditions to establish the requirement or otherwise for disulphide bridges in the 24 kd protein, by measuring the binding of E2-CHO to the transfer support.
Transfer supports were incubated with E2-CHO recombinant protein as described above.
The results are shown in FIG. 10 .
Lane
Description
1A
COS-7 membranes in non reducing SDS Laemmli
buffer
2A
MOLT-4 membranes in non reducing SDS
Laemmli buffer
3A
COS-7 membranes in SDS Laemmli buffer
containing 5% β-SH
4A
MOLT-4 membranes in SDS Laemmli buffer
containing 5% β-SH
1B to 4B are negative controls for the corresponding lanes 1A to 4A.
5. Optimising Purification
5.1. Immunoprecipitation
Membrane Proteins Solubilization
A membrane preparation from 400 million MOLT-4 cells (A2A6 subclone) was treated with 200 μl of PBS buffer, pH 7.4, containing CHAPS 7.5 mM and the following protease inhibitors in μl/ml: PMSF 35, aprotinin 2, pepstatin 0.7, leupeptin 0.5. After treatment with the above buffer, the resulting suspension was centrifuged at 100,000 g for 1 hour and the clear supernatant underwent immunoprecipitation experiments. The final protein concentration based on BCA protein assay (Pierce, USA) was 2.7 mg/ml.
Incubation with E2 Recombinant Envelope Protein
200 μl of membrane protein solution (2.7 mg/ml) in PBS-CHAPS were added to 15 μl of CHO-produced E2 (Batch P4) solution. The stock concentration of E2-P4 protein was 130 μl/ml and its final concentration in the protein membrane solution was 9.75 μg/ml.
The mixture was kept overnight under stirring at 4° C.
Incubation with Rabbit Anti-E2 Antisera
The resulting solution was divided into two aliquots of 100 μl and each was mixed with 5 μl of preimmune and postimmune antiserum from a rabbit (R#1) previously immunized with E2 protein. The final dilution of antisera was 1:20. Incubation was performed for 1 hour at 4° C.
Addition of Protein-A Sepharose CL-4B
Protein-A Sepharose CL-4B resin (Pharmacia, Sweden) was extensively washed with PBS containing 7.5 mM CHAPS at pH 7.4, and 30 μl of compact slurry (capacity of matrix is 20 mg of human Ig per ml of slurry) were added to each 100 μl sample resulting from the step above. Incubation was performed under stirring for 1 hour at 4° C.
The samples were centrifuged to pellet down the resin and the supernatant was removed, mixed with Laemmli-Buffer (without reducing agent) and kept for SDS-PAGE. The resin pellet was washed twice with 500 μl of PBS-CHAPS (10 min each wash at 4° C.) and then the pellet was treated with 50 μl of Laemmli Buffer containing 5M urea. The resulting supernatant was subjected to SDS-PAGE.
SDS-PAGE and Immunoblot
The samples from the steps above, that is, supernatant containing material not absorbed on Protein-A matrix (SN) and material desorbed from Protein-A matrix (ProtA) from both preimmune and postimmune antisera, were loaded on SDS-PAGE gel in non reducing buffer and without heating. After the run, the gels were electroblotted on nitrocellulose paper in 20% methanol Tris-Glycine buffer and were subjected immunostaining as described above. Incubation with E2 protein was performed overnight using E2 SMC-PC at 1.73 μg/ml in PBS 0.05% Tween 20.1% milk.
The samples loaded on SDS-PAGE were:
A) Supernatant (material not retained by Prot-A) from Preimmune antiserum,
B) Prot-A desorbed material from PREimmune antiserum,
C) Supernatant from POSTimmune antiserum, and
D) Prot-A desorbed material from POSTimmune antiserum
Three sets of these samples were loaded on gel, one was stained directly on gel the other two underwent immunostain, one incubated with E2 the other as negative control.
The nitrocellulose transferred support was incubated with E2-CHO SMC-PC recombinant protein at 1.73 μg/ml followed by 291A2 hybridoma culture supernatant (containing a monoclonal antibody that recognises epitopes exposed on E2 when bound to its putative receptor), biotinylated polyclonal anti-mouse Ig antibodies and peroxidase labelled Extravidin™ (Sigma Immunochemicals, USA). Chemiluminescent staining obtained with ECL-Luminol (Amersham, GB), exposure 1 minute.
The results are shown in FIG. 11 .
Lane
Description
1A
molecular weight standard
2A
empty
3A
sample incubated with preimmune rabbit
serum - supernatant
4A
sample incubated with preimmune rabbit
serum - Protein-A bound
5A
sample incubated with postimmune rabbit
serum - supernatant
6A
sample incubated with postimmune rabbit
serum - Protein-A bound
The negative controls employed the nitrocellulose membrane incubated with 291A2 hybridoma culture supernatant followed by biotinylated polyclonal anti-mouse Ig antibodies and peroxidase labelled streptavidin. 1B to 4B correspond to 3A to 6A respectively.
5.2. Ammonium Sulphate Fractionation
Membranes were prepared as reported in the membrane preparation protocol from MOLT-4 cells and solubilized in PBS buffer pH 7.4 containing 8 mM CHAPS. The protein concentration estimated on the basis of BCA assay ranges from 1.8 and 2.5 mg/ml.
Solubilized membranes were mixed with an ammonium sulphate (AS) saturated solution in a volume sufficient to obtain 25% saturation of ammonium sulphate (i.e. the final concentration of AS is 25% of the starting saturated solution). The sample was allowed to stand in melting ice for 2 hours and then centrifuged at 15800 g for 30 minutes.
The supernatant was mixed with AS saturated solution to a final saturation of 50%. The sample was allowed to stand for 2 hours on melting ice and then filtered on a Spin-X™ centrifuge filter unit (Costar, Cambridge, Mass., USA) for 15 minutes at 4° C.
The precipitates obtained above were dissolved in suitable buffers and undergo further treatment.
The pellets were redissolved in PBS pH 7.4 containing 10M urea and underwent Laemmli SDS-PAGE. The volumes of AS fractions were loaded in such a way that the amount of putative receptor should be comparable in different samples.
The transfer support was incubated with E2-CHO recombinant protein as described above.
The results are shown in FIG. 12 and show that precipitation of p24 occurs in the range of 33 to 50% of saturation.
Lane
Description
1A
Starting membranes
2A
20% AS fraction
3A
33% AS fraction
4A
43% AS fraction
5A
50% AS fraction
6A
60% AS fraction
5.3. Hydrophobic Interaction Chromatography
1.5 ml of solubilized membranes from MOLT-4 cells (protein concentration 2.5 mg/ml) were pre-fractionated at 25% of saturation of ammonium sulphate and the supernatant from this step was brought to 50% saturation of AS. The precipitate obtained was resuspended in 200 μl of PBS containing ammonium sulphate at 25% of saturation. The undissolved material was pelleted by centrifugation at 15800 g for 30 minutes. The supernatant obtained was incubated with 200 μl of Phenyl-Sepharose matrix (Pharmacia, Uppsala, Sweden), previously equilibrated in PBS pH 7.2 containing AS at 25% of saturation, for 2 hours at room temperature.
The non retained material was recovered by filtering on a Spin-X™ centrifuge filter units (Costar, USA).
The matrix of Phenyl-Sepharose was washed twice with 100 μl of PBS, 25% AS saturation and once with 300 ml of the same buffer. The matrix was then eluted with PBS pH 7.4 (200 μl) and then with PBS, pH 7.4 containing 20 MeOH. Finally, the matrix was treated with 40 μl of non reducing Laemmli buffer.
Samples containing ammonium sulphate (i.e. non retained and wash material) were dialysed against 8M urea in PBS, pH 7.4.
All samples underwent SDS-PAGE analysis and Western Blot.
5.4. Acetone Precipitation
50 μl of membranes from MOLT-4 cells solubilized in 8 mM CHAPS in PBS, pH 7.4 were mixed with 200 μl of acetone.
The sample was centrifuged at 15800 g for 15 minutes and the supernatant was discarded. The obtained precipitate was dissolved in non reducing Laemmli sample buffer and underwent SDS-PAGE and Western Blot. The transfer supports incubated with E2-CHO recombinant protein as described above.
The results of the combined HIC and acetone precipitation experiment are shown in FIG. 13 .
Lane
Description
1A
Starting membranes (16 μl total protein
content)
2A
material non retained on matrix
3A
wash
4A
material eluted with PBS, pH 7.4
5A
material eluted with PBS, pH 7.4 containing
20% Methanol
6A
material eluted with Laemmli Buffer
7A
membranes solubilized in Triton 1% PBS, pH
7.4 (26 μg total protein)
8A
acetone precipitate from sample 7A
Samples from 1B to 8B correspond to samples from 1A to 8A
These experiments show that ammonium sulphate precipitated material can be redissolved in suitable conditions and undergo hydrophobic interaction chromatography. The 24 kd HCV putative receptor protein binds to Phenyl Sepharose and can be recovered from this matrix.
The membrane extract can be precipitated with acetone without loss of binding capacity of HCV putative receptor.
6. Sequencing and Cloning
6.1. Amino Acid Sequence
The amino acid sequence of the 24 kd protein may be elucidated either by inference from the cloned DNA or by microsequencing of protein prepared by one of the processes described above. Based upon the molecular weight of the protein (and the knowledge that, if glycosylated it is only glycosylated to a small extent) it is expected that the protein will have approximately 210-230 amino acids (allowing the average of 110 daltons per amino acid).
6.2. DNA Sequence Cloning and Sequencing
The DNA sequence of the 24 kd protein may be determined by one of a number of techniques known to the art, such as λgt11 “shotgun” cloning where a DNA library is produced, suitably from a hyperexpressing cell-line (see above) and fragments of DNA were caused to express in prokaryotic or eukaryotic cell, the products being screened using antibodies to the 24 kd protein or by binding to recombinant E2-CHO.
Once identified, the DNA encoding the 24 kd protein may be used to produce large quantities of the protein which, as a result of its binding to HCV may prove useful in an assay for HCV infection or for the manufacture of a medicament for treating HCV infection.
Alternatively, the DNA may be used to prepare transgenic animals bearing the 24 kd protein which may then serve as animal models for HCV infection.
It will be understood that the invention is described above by way of example and modifications within the scope and spirit of the invention may be made without the need for undue experiment or the exercise of inventive ingenuity.
References
1. European patent application EP-A-0318216
2. European patent application EP-A-0388232
3. Choo et al PNAS USA (1991) 88 2451-2455
4. Chien, D. Y. et al PNAS USA (1992) 89 10011-10015
5. Spaete, R. R. et al Virology (1992) 188 819-830
6. Gething et al Nature [needs complete reference]
7. “Flow Cytometry” in Methods of Cell Biology, 1990 Vol. 33 Academic Press San Diego
8. Morre{acute over ( )}D. J. et al., Methods Enzymol. (1994) 228, 448-450.
9. Laemmli et al Nature (1970) 27 680 | A 24 kd protein capable of binding the E2 envelope protein of hepatitis C virus (HCV), and functionally equivalent variants or fragments of the 24 kd protein, are disclosed. Processes for production and purification of the 24 kd protein, and functionally equivalent variants or fragments thereof, are also disclosed. | 2 |
CROSS REFERENCE TO RELATED APPLICATIONS
This application is a continuation-in-part of my previously filed application, filed Mar. 20, 1978, Ser. No. 888,169, now abandoned.
BACKGROUND OF THE INVENTION
(1) Field of the Invention
This invention relates to pipes and more particularly to plastic protectors for the threaded end of pipe.
(2) Description of the Prior Art
Tubular goods, such as oil field production pipe, is very expensive and is handled in large quantities. One oil well may require more than four hundred joints of thirty foot pipe. The joints usually are stored out of doors where they are subjected to the deleterious effects of the atmosphere. The threaded ends of a pipe are especially susceptible to oxidation and must be suitably protected.
In handling pipe joints, it is customary to place protectors onto the threaded marginal ends thereof, with one protector being utilized on the pin end and another different size protector being employed on the box end of the pipe.
The protectors usually are screwed into threaded relationship respective to the threaded marginal ends of the pipe, and sometime changes in climatic conditions causes the protectors to become firmly engaged with the pipe threads so that it is very difficult to subsequently remove the protector from the end of the pipe. At other times temperature changes cause the protectos to loosen so that it easily becomes disengaged from the end of the pipe. Moreover, many protectors are provided with an irregular outer surface area so that as one pipe joint makes rolling contact with another, the protectors will inadvertently be unscrewed from the pipe.
There are two main problems with plastic protectors for pipe, particularly oil field pipe. One, the difference in temperature expansion between plastic and steel, and two, the rough handling.
The plastic has thermal expansion which greatly exceeds that of steel. Furthermore, the plastic when warm is soft and more deformable wherein at cold temperatures it is less deformable and more brittle.
The plastic thread protectors may be applied either in hot or cold climates. If they are applied in hot climates, they will contract in cold climates which may cause the protectors to crack and break. If they are applied in cold climates when they warm up and expand if they are on the outside of the threads they may expand to an extent that they are loose.
It will be understood that the temperatures can be extreme, they range all the way from the tropics and desert climates where the pipe sitting in the sun reaches extremely high temperatures or it may be in the artic wherein the pipe goes to extrememly cold temperatures. In the sunshine with the sun shining on the pipe, the pipe can often reach temperatures above 160° F. (72° C.) while in the artic the pipe temperature can be below -60° F. (-50° C.).
Due to the rough handling of the pipe, the external thread protector can be impacted which may either cause cracking of the thread protector if it is cold and brittle; when it will also have greater tensile stresses upon it. If the protector ever cracks it will be loose and will be susceptible to coming off in the event of further vibrations. If the temperature is warm, the rough handling will cause greater deformation of the threads into the thread protector. This impact upon the thread protector will cause the threads to make greater indentations into the thread protector, which further vibrations or rough handling can cause it to come loose.
Joints of pipe are available in many different diameters and it is, therefore, necessary for the manufacturer of the thread protector to supply two different size protectors (internal and external) for each size of pipe. This represents a large capital investment in manufacturing facilities and stock.
Accordingly, it is desirable to be able to reduce the number of protectors required for a finite number of pipe joints. Furthermore, it is desirable to provide a protector which does not loosen nor tighten an appreciable amount during ambient changes in temperature. Moreover, it is desirable to provide a protector which is low in cost, easily installed and removed from the threaded ends of the pipe, and which does not inadvertently become unscrewed during the handling of the pipe. Such a protector is the subject of this invention.
Also in many cases where the pipe is coated internally, it is desired to seal the ends of the pipe to protect the coating and not leave it exposed.
In the parent application, the Examiner considered the following patents to be pertinent:
Gray, Jr., U.S. Pat. No. 3,104,681
Ferguson, U.S. Pat. No. 2,551,834
Pfeil et al., U.S. Pat. No. 2,632,479
GRAY JR. disclose a plastic closure for protecting pipe threads. It discloses a tapered plug. The thread engaging portions of it are smooth, both internally and externally.
FERGUSON discloses a protective plastic cap made of vinylite, cellulose acetate, cellulose acetate butyrate or the like. If is disclosed for use with machine type threads, i.e., non-tapered threads. The entire description of the gripping action is by the deformation of the threads into the ribs.
PFEIL ET AL. discloses a thread protector which has ribs or protuberances 12 of perferable triangular shape which are softer than the threads to be protected.
SUMMARY OF THE INVENTION
(1) New and Different Function
According to my invention, the tension upon the thread protector or the force by which the thread protector is held upon the threads is greater than mere stretching. I.e., the material between the ribs is bent so that it becomes a different geometric shape. Therefore, the resilience and the movement due to temperature changes or due to other items, such as rough handling, which would tend to loosen this is taken up by the greater ability to return to its original shape because of the change in geometric form. I.e., the thread protector between the ribs bends rather than just retaining its original shape and stretching.
It will be understood that if the protectors are applied in cold weather, and they are the outside protectors on the pin end, when the protectors are driven over the pipe, the threads of the pipe will tend to shear and remove the top of the ribs but still there will be the deformation of the geometric shape between the ribs which will cause the protectors to form a tight fit. The cold will cause the plastic to be more brittle and less deformable. The threads will not bite into or form indentations into the ribs to an appreciable extent. If, on the other hand, the protectors are applied in hot weather, the protectors will be expanded. The threads will not remove any material from the ribs as they are going on because there will not be enough pressure between the protector and the ribs. However, the protector will be geometrically deformed between the ribs and there will be more deforming of the material by the threads making more indentations in the material. The warmer the plastic the easier it is for the threads to bite into or make indentations in the ribs. In either event, the shape of the protector will be deformed to such an extent that the sleeve of the protector between the ribs will be near the threads if not in acutal contact with the threads between the ribs.
(2) Objects of this Invention
An object of this invention is to protect the threads upon the end of a pipe.
Another object of this invention is to prevent foreign material from entering the pipe.
Further objects are to achieve the above with a device that is sturdy, compact, durable, lightweight, simple, safe, efficient, versatile, ecologically compatible, energy conserving, and reliable, yet inexpensive and easy to manufacture, and install.
Other objects are to achieve the above with a method that is versatile, ecologically compatible, energy conserving, rapid, efficient, and inexpensive, and does not require skilled people to install.
The specific nature of the invention, as well as other objects, uses, and advantages thereof, will clearly appear from the following description and from the accompanying drawing, the different views of which are not scale drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
FIGS. 1 and 2 are perspective view of a deformable pipe thread protector made in accordance with the present invention;
FIGS. 3 and 4 are opposed end views of the pipe thread protector disclosed in FIGS. 1 and 2;
FIG. 5 is a side elevational view of the apparatus disclosed in the foregoing figures, with some parts thereof being removed therefrom and some of the remaining parts being shown in cross section;
FIG. 6 is a fragmentary, part cross sectional representation, taken along line 6--6 of FIG. 5;
FIG. 7 is a lateral, cross sectional view showing the apparatus disclosed in the foregoing figures in operative relationship respective to a joint of pipe;
FIG. 8 is a fragmentary, part cross sectional representation, taken along line 8--8 of FIG. 5; and
FIG. 9 is a longitudinal sectional representation illustrating the pipe thread protector apparatus of FIG. 1 in operative relationship with various different marginal threaded ends of pipe.
FIG. 10 is a perspective view of a second embodiment of a deformable pipe thread protector.
FIG. 11 is a sectional view of a portion thereof showing the particular shape of the ribs set therein taken substantially on line 11--11 of FIG. 10.
FIG. 12 is a sectional view taken longitudinally through the rib taken substantially on line 12--12 of FIG. 10 with the pipe outline shown in phantom line thereon. The thickness and taper of the elements has been greatly exaggerated for the purposes of clarity of illustration.
FIG. 13 is a sectional view taken substantially similar to FIG. 12 showing another pipe outline in phantom lines thereon. The thickness and taper of the elements has been greatly exaggerated for the purposes of clarity of illustration.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
In the various figures of the drawings, and in particular FIGS. 1-6, there is disclosed a deformable pipe thread protector apparatus 10 made of resilient material, e.g., PVC, Styrene, high density polyethylene, and various other plastics and rubber like compositions having good weathering properties. The pipe thread protector includes a small diameter end 12 opposed to a large diameter end 14. The opposed ends are generally described by spaced planes which are disposed parallel to one another and perpendicular to the longitudinal axial centerline of the apparatus.
The protector is generally a cylindrical sleeve in form and inwardly tapers from the large toward the small diameter end and, therefore, is representative of a frustum of a cone.
The marginal large diameter end is in the form of a continuous circumferentially outward extending shoulder 16 which continues toward the small diameter end portion in the form of radially spaced outwardly directed ribs 18. Hence the ribs and the shoulder can be said to result from the removal of material in an area defined by two adjacent spaced apart ribs together with the intermediate edge of the shoulder. The ribs continue towards the reduced diameter end of the protector and at numeral 20 the ribs lose their identity and become a part of a circumferentially extending marginal small diameter end thereof.
Radially spaced apart lugs 22 are located on an imaginary circle which is of smaller diameter respective to the reduced diameter end of the apparatus. The lugs facilitate removal of the protector from a pipe end. Cut-outs 24 are formed on the opposed end of the protector. The cut-outs are radially spaced from one another and located within the marginal end portion of shoulder 16.
Numeral 26 indicates the marginal inside peripheral wall surface which is opposed to the shoulder 16, while numeral 28 indicates a bulkhead located at the small diameter end of the apparatus. The bulkhead is apertured as indicated by numeral 30, thereby providing a lightening hole and enabling the interior of a pipe to breathe.
Rib 32 is an integral part of the apparatus and extends inwardly from the inside wall surface in opposition to the outer ribs 18. Numeral 34 indicates the inner wall surface of the bulkhead. The ribs commence at wall surface 34 and terminate at 35 in spaced relationship to the large diameter end such that the before mentioned marginal wall surface 26 is provided.
Accordingly, there is an inside wall surface 26 which is uninterrupted by ribs which continue as another wall surface 36 located between the spaced ribs. Numeral 37 indicates the joinder area between the ribs 18 and the intermediate edge of shoulder 16.
FIGS. 7 and 9 illustrate the pipe protector operatively affixed to the pin end of a metal pipe 38. Pipes 38 and 39 are of different diameters and it will be noted that the protector 10 is used on either of the pipe ends. As seen in FIG. 7, the ribs 32 force the cylindrical sidewall of the protector radially away from the pipe threads while the inner wall surface located between adjacent ribs contact the pipe threads as indicated by numeral 40. Accordingly, the protector of the present invention is distorted from the circular or round configuration as seen illustrated in FIG. 8, e.g., into the oblated configuration as seen in FIGS. 7 and 9.
The geometry of the distorted protector depends upon the number of ribs employed, and in the preferred embodiment of the present invention, there are disclosed four ribs. Accordingly, the resulting oblated geometrical configuration is related to a four sided figure having corners 42 and sides 43, with there being a side located between each adjacent inner rib.
Numeral 46 generally indicates the pin end of a two and three-eighths EVE eight round tubing or pipe, having a marginal threaded end 48 placed into engagement with the inner ribs of the protector such that the protector is deformed into the configuration illustrated in FIG. 7.
Numeral 50 generally illustrates the box end of an upset oil string, such as two and seven-eighths EVE eight round tubing. Upset tubing usually is provided with a circumferentially extending shoulder at 52 and tapered threads 54 which commence at the inner end of the shoulder and extend towards the interior of the pipe. It will be noted that shoulder 16 of the protector is seated within the pipe shoulder while the ribs 18 engage the threads 54 with sufficient force to deform the intervening sidewalls in a manner analogous to FIGS. 7 and 8.
Referring to the drawings, and particularly FIG. 9, it may be seen that the pipe threads, both on the pin end of pipe 38 and the box end of pipe 39, are tapered, i.e., the surface extends toward a common point located along the longitudinal axis thereof. Not only are the ribs tapered as described above, but the ribs have the same taper as the pipe threads as clearly seen in FIG. 9. Furthermore, as seen in FIG. 9, the threads have a tip diameter which extends away from the pipe and a root diameter which is cut into the pipe. Both the pin and box end have a tip and root diameter. The ribs obviously contact the tip of the threads at the tip diameter. However, in the method according to this invention, the sleeve of the protector is telescoped along the pipe to a point where the undeformed defector would have a "rib diameter" or the distance between the ribs at any point of contact with the threads more nearly the root diameter of the threads than the tip diameter of the threads. Thus, the telescoping of the protector along the tapered threads produces the oblate shape. Further it may be seen by having the rib taper equal to the thread taper that the ribs will contact the threads with uniform pressure throughout the contact therebetween.
The pipe protector of the present invention preferably is placed with the large diameter end encompassing the outer threaded pin end 46 of the tubing, and is driven into place with a mallet or wooden two-by-four. This causes the protector to telescopingly engage the marginal threaded end of the pipe with sufficient force to be deformed into the configuration illustrated in FIG. 7. The memory of the plastic causes the ribs to be inwardly biased against the pipe threads with sufficient force to hold the protector in place until it is desired to remove the protector from the pipe. The protector can be fitted to the pin end of a two and three-eighths inch pipe or to the box end of a two and seven-eighths inch pipe, and accordingly; one protector suffices for two different size pipe ends thereby eliminating fifty percent of a pipe protector inventory.
The protector is removed by engaging the lugs 22 with any suitable elongated apparatus, e.g., a large screw driver, thereby enabling the protector to be unscrewed. The protector is reusable until the ribs have become appreciative worn from usage.
The protector is placed on the box end of the larger pipe in the illustrated manner of FIG. 9 by driving the protector into place with a mallet or wooden two-by-four so that the shoulder 52 of the pipe "shoulders up" with the shoulder 16 of the protector. Simultaneously, the outer ribs engage the threads of the pipe with sufficient force to deform the protector in a manner similar to FIG. 7 wherein the outer ribs thereof are inwardly deformed to provide for the oblated configuration. The protector is removed from the box end by engaging the lugs 24 with a suitably sized screw driver or similar elongated piece of metal.
The present invention provides a protector for use on two different size pipes, wherein the outer or inner ribs engage the threaded pipe surface, while shoulder 16 or bulkhead 28 enables proper positioning of the apparatus. The staggered relationship of the outer and inner ribs, together with the opposed marginal ends 16 and 20, provide the unexpected advantage of a protector which resiliently mates with a pipe end in an improved and superior manner. The method of jointly using the ribs and memory of the plastic to provide a protector which is resiliently distorted from a circular into an oblated geometrical configuration provides a new protector having advantages not found in the prior art.
Specifically, because such a large portion of the sleeve of the protector is distorted, it is capable of retaining firm contact with the pipe as a result of expansion and contraction due to temperature changes as discussed above in the Background of the Invention.
Another unexpected and unusual attribute of the ribs and shoulder combination of this invention lies in the cooperative action of the protectors as two adjacent pipe joints make rolling contact with one another. In such an instance, the shoulder 16 and small diameter marginal end of the protector make low friction engagement thereby preventing the ribs 18 of the two protectors from contacting one another. This action prevents the protectors from being inadvertently unscrewed from the pipe ends.
The deformation of the protector from a round into an oblated configuration avoids undue stresses and breakage of the wall structure as the apparatus is driven onto the end of a pipe.
Referring more particularly to the embodiment shown in FIGS. 10-13, there may be seen a thread protector for the external threads of a pipe.
The protector has a sleeve like body 60. As seen in the drawings, sleeve 60 has a slight taper to it. This taper is no greater than the taper of the threads upon the end of the pipe. The pipe threads will generally have a taper of 1:16, although in some cases they will have a taper of 1:32. I would prefer the sleeve 60 to be cylindrical, however, in the manufacture of plastic parts it is difficult to form a cylindrical sleeve and, therefore, a small taper is included with it. Preferably, the taper is as small as possible. The sleeve has open end 62 and shoulder end 64. If the sleeve 60 has any taper at all the shoulder end 64 will be at the smaller end and open end 62 at the larger end.
A shoulder, in the form of inwardly extending flange 66, is formed at the shoulder end. The shoulder has raised lugs 68. The lugs are in the form of reinforced projections. They provide diametrically opposed slots 70 by which a tool may be used to rotate the protector to remove the protector from a pipe. In the event it is desired to protect the bore of the pipe from dirt or other contaminants, the shoulder 66 may extend all the way across the protector forming a closed end to thereby protect the bore of the pipe from the entry of dirt and the like.
Four longitudinal ribs 72 are located within the sleeve 60. The ribs 72 run for their full height from the shoulder 66 to a point which is about 1/3 the length of the sleeve. Thereafter, the ribs taper at 73 into the sleeve so that 1/3 of the sleeve next to open end 62 is smooth and unribbed. I.e., the sleeve is divided into thirds. The third next to the open end is smooth and has no ribs. The middle third has the tapered rib 73. The third next to the shoulder has the ribs 72 at full height. As shown in the drawing, the ribs 72 will have a certain height "h" and certain width "w". Normally, the width "w" of the ribs will be over twice the height "h" of the ribs. The ribs will normally be curved in cross section as seen in FIG. 11. Normally, the ribs will not have a greater height "h" than the thickness "t" of the sleeve 60.
It is desired that the sleeve 60 have as little taper as possible and no greater taper than the pipe threads of which the sleeve is to protect. Likewise, the ribs 72 should have as little taper as possible and in no event have a greater taper than the pipe threads which they protect. As explained above, the sleeve of the protector will be distorted from its normal circular configuration into an oblate configuration, the same as the previous embodiment, as illustrated in FIG. 7. However, the shoulder 66 at the shoulder end 64 makes it difficult to distort the sleeve at that end. Therefore, it is more desirable to have the sleeve distorted in the mid part of the sleeve, i.e., between the shoulder end 64 and the open end 62. The open end 62 will be only slightly larger than the unthreaded pipe itself. Therefore, any distortion of the sleeve at the open end brings the sleeve into contact with the unthreaded portion of the pipe and, therefore, the sleeve will not be greatly distorted in this area. On the other hand, distortion at the shoulder end 64 is more difficult and will sometimes result in cracking or breaking of the sleeve beginning at the shoulder which is undesirable. However, in the mid section of the sleeve well away from the ends 62 and 64, the sleeve can readily be distorted. Of course, the distortion of the sleeve is highly desirable between the two ends and is a sought after feature of the invention. Therefore, it is desirable that the ribs 72 have a lesser taper than the threads which they engage so that this desired distortion pattern is achieved.
FIG. 12 illustrates the sleeve in connection with short pipe 74. The pipe is called a short pipe because it is threaded by short threads 76, the pipe being only threaded about 2/3's the length of the sleeve. I.e., the pipe threads begin at about the same point taper ribs 73 begin. It may be seen that with the ribs 72 having a less taper than the pipe threads that the maximum interference between the ribs 72 and the pipe threads 76 is in the area located about 1/3 of the way from the shoulder end.
FIG. 13 illustrates the protector in use with long pipe 78 called a long pipe because it has long threads 80. I.e., the threads extend for approximately the full length of the sleeve 60. Even so, it may be seen that the maximum contact or interference between the threads and the ribs is located about 1/3 of the way from the shoulder end.
This relation can also be expressed that the diametrical distance between the ribs is less than the diameter of the threads at a point between the ends of the sleeve when the sleeve is fully telescoped over the pipe. Also, the thread diameter will exceed the distance between the ribs by a greater amount between the ends of the sleeve than at either end of the sleeve. As illustrated in FIGS. 12 and 13, this point where the thread diameter exceeds the distance between the ribs will be a point 1/3 the distance from the shoulder end. Of course, this difference between the thread diameter and the distance between the ribs will cause the sleeve to deform from a circular to an oblate configuration and this deformation will be between the ends of the sleeve.
It will be emphasized that FIGS. 11, 12 and 13 are not scale drawings and particularly in FIGS. 12 and 13, the thicknesses and the tapers have been exaggerated for the purposes of illustration. Also, the protector is shown in a non-distorted condition. I.e., the protector is shown according to its shape and size at normal temperatures (about 70° F. and 22° C.). The phantom pipe outline is shown also according to what it would be. Therefore, the interference between the ribs and the pipe as shown indicating what the changes and movement necessary of the protector and the location where this change and movement will occur. Of course, it is understood as explained above that the protector does not move fully to the extent of the interference shown in FIGS. 12 and 13 but there is a deformation of the ribs by the threads being indented into the ribs and further that in certain conditions there will be a shaving or that the ribs will be scrapped away when the protector is driven onto the threads.
Also, it will be understood that providing the protector for the external threads is more critical and more difficult than providing the protector for the interior threads. The interior threads are not subjected to the impacts, rough handling, rubbing against other pipes and the like that the external threads are subjected to. Therefore, the protectors for internal threads are much easier to maintain in place than the protectors for the external threads.
The ribs themselves may be thought of as stress bars. I.e., it is the ribs which produce the tensions, stresses and strains which produce the distortion of the protector.
Thus it may be seen that I have provided for a protector for pipe threads which has as its basic principle the basic change in shape of the protector from its original circular configuration into that oblate configuration when it is placed upon the pipe.
The embodiments shown and described above are only exemplary. I do not claim to have invented all the parts, elements or steps described. Various modifications can be made in the construction, material, arrangement, and operation, and still be within the scope of my invention. The limits of the invention and the bounds of the patent protection are measured by and defined in the following claims. The restrictive description and drawing of the specific example above do not point out what an infringement of this patent would be, but are to enable the reader to make and use the invention. | A pipe thread connector of resilient deformable material has a sleeve or tubular shape with radial ribs projecting from the sleeve. The protector is driven upon the threads of the pipe and the geometric configuration of the sleeve changes because the sleeve is bent between the ribs. This bending keeps the ribs in tight resilient contact with the threads. | 5 |
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to engine assembly techniques and, more particularly, toward devices and methods for easing installation of a belt around engine pulleys.
2. Description of Related Art
During the assembly of automobile engines, it is necessary to wrap one or more belts around the engine pulleys. Such pulleys include a drive pulley, one or more driven pulleys, and idler pulleys. One or more of the idler pulleys is a tensioning pulley that is adjustable to maintain the belt at a predetermined tension, so as to reduce belt slippage and wear. However, during a belt installation process, the tension placed on the belt by the tensioning assembly makes it difficult or impossible to wrap the belt around the pulleys. Therefore, it is necessary to reduce or relieve the belt tension in order to permit the belt to be wrapped around the pulley.
The belt tensioning devices typically include a spring-biased piston that is disposed within a cylinder. With this arrangement, the cylinder is secured to a pulley mounting plate, while the free end of the piston is secured to a fixed support on the engine. The cylinder and piston are urged away from each other by the spring, and the pulley mounting plate and the pulley disposed thereon are moved, with the cylinder, away from the piston fixed support, so as to place tension on the belt that is disposed around the engine pulley.
However, to permit the belt to be placed around the pulleys, the belt tensioning device must be compressed or otherwise de-activated. When the belt tensioning device is compressed, the associated idler pulley may be moved so as to permit the belt to be placed therearound. Thereafter, the belt tensioning device may be released to return the idler pulley to its normal position and place the desired tension on the belt.
Unfortunately, it is difficult to manually compress or deactivate the belt tensioning device. In the past, compression clips have been used to hold the belt tensioning device in a collapsed or deactivated condition, but such compression clips are not useful in all applications. Also, it is known to use a lever to force the idler pulley mounting bracket to rotate against the spring bias of the belt tensioning device, and thereby move the idler tensioning pulley into a position to permit the belt to be placed therearound. Unfortunately, moving the bracket in this way requires a lot of force, and is a difficult operation for the belt installer. Furthermore, the installer will have to hold the lever with one hand while positioning the belt with the other hand, which is awkward at best.
Therefore, there exists a need in the art for a device and method for releasing or compressing a belt tensioning device so as to ease installation of a belt around the engine pulleys.
SUMMARY OF THE INVENTION
The present invention is directed toward a device and method for compressing an automatic belt tensioning cylinder, and thereby easing installation of a belt around the engine pulleys.
In accordance with the present invention, a tension releasing device includes a double acting pneumatic cylinder having a jig secured thereto. The jig is adapted to receive the tensioning cylinder and to hold the tensioning cylinder during compression thereof by the pneumatic cylinder. The pneumatic cylinder has a piston rod extending therefrom, and is operated to extend/retract the piston rod relative to the pneumatic cylinder. A distal end of the piston rod holds a pusher block. The pusher block cooperates with the jig to receive and hold the tensioning cylinder.
In further accordance with the present invention, the jig includes a sensor that detects whether the tensioning cylinder is received within the jig. Operation of the pneumatic cylinder is prevented when a tensioning cylinder is not detected by the sensor.
BRIEF DESCRIPTION OF THE DRAWINGS
These and further features of the invention will be apparent with reference to the following description and drawings, wherein:
FIG. 1A is a front elevational view of an engine with a belt mounted around a series of drive, driven and idler tensioning pulleys;
FIG. 1B is similar to FIG. 1A , but showing the tension releasing device disposed over an automatic belt tensioning cylinder;
FIG. 2 is a front perspective view of the tension releasing device;
FIG. 3 is a rear perspective view of the tension releasing device;
FIG. 4 is a perspective view of a cylinder weldment;
FIG. 5 is a perspective view of a base weldment;
FIG. 6 is a front perspective view of the tension releasing device according to the present invention with the tensioning cylinder received in the jig and in a normal or extended condition, and with other portions of the engine removed for purposes of clarity;
FIG. 7 is similar to FIG. 6 , but illustrates the tension releasing device in an activated condition and with the tensioning cylinder in a compressed condition to permit placement of the belt around the pulleys;
FIG. 8 schematically illustrates a pneumatic circuit of the tension releasing device of the present invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
With reference to FIGS. 1A and 1B , an engine 10 has a plurality of pulleys extending therefrom that are adapted to receive a belt 11 . These pulleys include a drive pulley 12 , one or more driven pulleys 14 , and one or more idler pulleys 16 . In the illustrated engine 10 , both idler pulleys are tensioning pulleys 16 , although this is not always the case. The tensioning pulleys 16 are mounted upon a mounting plate 18 , and the mounting plate 18 is pivotally moved by an automatic belt tensioning cylinder 20 . Normally, belt tension fluctuates during operation of the engine 10 , and the tensioning cylinder 20 moves the mounting plate in response to these changes in belt tension so as to maintain a fairly constant tension on the belt 11 , as is well known in the art.
The tensioning cylinder 20 has a first end 20 a and a second end 20 b . The tensioning cylinder first end 20 a is attached to the engine 10 and thus is held in a fixed position. The tensioning cylinder second end 20 b is attached to the mounting plate 18 and thus is movable relative to the first end 20 a and the engine 10 . A tension releasing device 22 of the present invention, described hereinafter, is adapted to compress or deactivate the tensioning cylinder 20 so as to ease installation of the belt 11 around the engine pulleys 12 , 14 , 16 .
With particular reference to FIGS. 2-3 , the tension releasing device 22 of the present invention includes a double-acting pneumatic cylinder 24 and a jig 26 , with the jig 26 being adapted to receive the tensioning cylinder 20 . The jig 26 includes a cylinder weldment 28 ( FIG. 4 ), a base weldment 30 ( FIG. 5 ), a pusher block 32 , and a sensor 34 . As will be apparent from the following discussion, the jig 26 is integral with the pneumatic cylinder 24 in that the cylinder weldment 28 and base weldment 30 are secured to the pneumatic cylinder 24 and the pusher block 32 is secured to a free or distal end of a piston rod 36 extending from, and driven by, the pneumatic cylinder 24 .
The pneumatic cylinder 24 includes a framework or body that provides mounting locations for the various handles, guards, and valves, as illustrated and described hereinafter, and to which the jig 26 is secured. More specifically, a hanger member 37 and a first handle 38 are attached to a top of the pneumatic cylinder 24 , with the hanger member 37 extending upwardly from a first side of the pneumatic cylinder 24 and the first handle 38 extending rearwardly from a second side of the pneumatic cylinder 24 . Relatively beneath the first handle 38 , a toggle valve assembly 40 is mounted to a first vertical sidewall of the pneumatic cylinder 24 .
The toggle valve assembly 40 includes a toggle valve body 40 a from which a toggle valve switch 40 b extends. The toggle valve body 40 a includes a plant air input 42 , first and second air outlets 44 , 46 , and a toggle valve (not shown) that is actuated or manipulated by the toggle valve switch 40 b so as to control communication of pressurized air to the pneumatic cylinder 24 so as to control operation (extension/retraction) of the device 22 . More particularly, the toggle valve controls communication of pressurized air from the plant air input 42 to the first and second air outlets 44 , 46 .
As will be appreciated by those skilled in the art, when the toggle valve switch 40 b is moved in a first direction from a neutral position, pressurized air supplied to the toggle valve body 40 a via the plant air input 42 is directed through the first outlet 44 , the plunger valve 34 , and a first flow restrictor 45 , and is introduced into the pneumatic cylinder 24 on a first side of the piston and thereby drives the piston in a first direction (i.e., to extend the piston rod 36 and pusher block 32 ). On the other hand, when the toggle valve switch 40 b is moved in a second direction from the neutral position, pressurized air supplied to the toggle valve body 40 a via the plant air input 42 is directed through the second outlet 46 and a second flow restrictor 47 and is introduced into the pneumatic cylinder 24 on a second side of the piston and thereby drive the piston in a second direction (i.e., to retract the piston rod 36 and pusher block 32 ).
The first handle 38 includes a guard that helps to conceal and protect the toggle valve switch 40 b so as to prevent unintended actuation thereof. A shield 48 is secured to the pneumatic cylinder 24 relatively beneath the first handle 38 and the toggle valve assembly 40 and serves to prevent tampering of the flow controls (i.e., the first and second flow restrictors 45 , 47 ) mounted to the pneumatic cylinder 24 , as described hereinafter.
With reference to FIG. 4 , the cylinder weldment 28 includes an upper plate 50 , a lower plate 52 , a series of supports 54 extending between the upper and lower plates 50 , 52 , and a guide handle 56 extending outwardly from the lower plate 52 . The guide handle 56 is disposed below the shield 48 on the second side of the pneumatic cylinder 24 , and is directed outwardly and upwardly therefrom in spaced relation to the first handle 38 , as illustrated.
The cylinder weldment upper plate 50 has a generally rectangular periphery, and has a circular hole 50 a formed in the center thereof through which the piston rod 36 extends. Fasteners extending through corners of the upper plate 50 connect the upper plate 50 to a lower end of the pneumatic cylinder 24 in a face-to-face fashion, as illustrated in FIGS. 2-3 .
The cylinder weldment lower plate 52 is somewhat u-shaped, having a pair of sides or arms 52 a that are interconnected by a base or leg 52 b so as to define a u-shaped opening 52 c . The pusher block 32 secured to the free or distal end of the piston rod 36 is reciprocally movable within or through the u-shaped opening 52 c , as will be described hereafter.
The base weldment 30 includes a u-shaped upper wall 58 , a u-shaped lower wall 60 , and first and second sidewalls 62 , 64 interconnecting the upper and lower walls 58 , 60 . The base weldment upper wall 58 is mechanically affixed to the cylinder weldment lower plate 52 by a series of screws, as illustrated. It will be appreciated that the dimensions of the base weldment upper wall 58 are slightly smaller than the corresponding dimensions of the cylinder weldment lower plate 52 .
The base weldment's u-shaped upper wall 58 includes a first arm 58 a , a second arm 58 b , and an interconnecting base or leg 58 c . Similarly, the base weldment's u-shaped lower wall 60 has first and second arms 60 a , 60 b and an interconnecting base 60 c . The u-shaped lower wall 60 is slightly smaller than, and offset from, the u-shaped upper wall 58 , but the upper and lower u-shaped openings 58 d , 60 d provided by the u-shaped upper and lower walls 58 , 60 are aligned with one another. The u-shaped lower wall 60 and, more specifically, the space within the base weldment 30 , is adapted to receive the tensioning cylinder 20 and, as such, may be considered a custom part. While the space between the upper and lower u-shaped walls 58 , 60 is important (to permit the tensioning cylinder 20 to be received therebetween), the space between the first and second arms 60 a , 60 b of the u-shaped lower wall 60 is chosen such that a first portion of the tensioning cylinder 20 may extend therethrough while a second portion of the auto tensioning cylinder 20 will rest thereon, as will be apparent from the discussion to follow. As such, the particular size, dimensions, etc. of the base weldment 30 are illustrative of a preferred embodiment adapted to a particular automatic belt tensioning cylinder 20 , and it is contemplated that at least these physical characteristics of the present invention will be modified to accommodate different auto tensioning cylinders.
The first sidewall 62 extends between, and is integrally affixed to, the first arms 58 a , 60 a of the u-shaped upper and lower walls 58 , 60 . The first sidewall 62 includes a pair of lengthwise extending slots that permit adjustable securement of a wear pad 66 to an inner surface thereof. The second sidewall 64 extends between, and is integrally affixed to, the base or interconnecting leg 58 c , 60 c of the upper and lower u-shaped walls 58 , 60 . The second sidewall 64 has a plurality of tapped openings formed therein to which a guide 68 and a guard 70 are attached. More specifically, an upper pair of tapped openings permit an upper L-shaped guide 68 to be secured to the second sidewall 64 , while the lower pair of tapped openings allow a lower L-shaped guard 70 to be secured thereto. It will be appreciated that the guide 68 and guard 70 have slotted openings that permit horizontal adjustment of the guide 68 and guard 70 relative to the base weldment second sidewall 64 . Relatively below the tapped openings, the second sidewall 64 has an enlarged opening 64 a formed therein to which the sensor 34 is mounted.
The sensor 34 , which is sometimes called a plunger sensor or plunger valve, includes a body portion 72 having an air inlet 72 a and an air outlet 72 b . Between the air inlet 72 a and air outlet 72 b , the body 72 holds a valve (not shown) that is opened and closed by a spring-biased plunger 74 extending outwardly from the body portion 72 . The plunger 74 is biased away from the body portion 72 a toward a valve-closed position. The plunger 74 extends through the enlarged opening 64 a in the second sidewall 64 so as to project into the interior of the jig 26 . When a tensioning cylinder 20 is properly received within the interior of the jig 26 , the plunger 74 will be depressed, opening the valve and thereby allowing pressurized air to pass through the sensor body portion 72 (i.e., from the body portion air inlet 72 a to the body portion air outlet 72 b ).
The pneumatic circuit for the tensioning releasing device 22 is fairly simple, and is schematically illustrated in FIG. 8 , and will be discussed hereafter as it relates to operation of the device 22 .
Plant air is introduced into toggle valve body 40 a via the inlet 42 and is directed toward one side or the other of the pneumatic cylinder 24 , depending upon the direction of actuation of the toggle valve switch 40 b , described previously. When the tensioning cylinder 20 is detected in the jig 26 by depression of the plunger sensor 34 , and the toggle valve switch 40 b is moved in the first direction, pressurized air flows through the first flow restrictor 45 and is introduced into the pneumatic cylinder 24 via an extend port 24 a so as to extend the piston rod 36 and the pusher block 32 . The first flow restrictor 45 is adjustable so as to selectively limit or adjust the pressurized air flow into the pneumatic cylinder 24 and thereby permit the cylinder extension speed to be adjusted.
It has been found that, in order to prevent damage to the tensioning cylinder 20 , it is important to not compress the tensioning cylinder too fast. In the present invention, the speed of movement of the pneumatic cylinder 24 is adjusted by the first flow restrictor 45 so that the tensioning cylinder rate of compression is adjusted so as to not damage the tensioning cylinder. In the illustrated embodiment, the maximum stroke of the pneumatic cylinder 24 is about 30 mm, with the maximum compression of the tensioning cylinder 20 being about 16 mm. The tensioning cylinder compression stroke takes at least 3 seconds.
Since the first end 20 a of the tensioning cylinder 20 is immovably fixed to the engine 10 , when the pusher block 32 engages the first end 20 a of the tensioning cylinder 20 , the jig 26 and the second end 20 b of the tensioning cylinder 20 are drawn upwardly or toward the pneumatic cylinder 24 , compressing the tensioning cylinder 20 and pivoting the mounting plate 18 , and the tensioning pulleys 16 disposed thereon, into a position that eases placement of the belt 11 around the engine pulleys. Once the belt 11 is placed around the pulleys 12 , 14 , 16 , the toggle valve switch 40 b is actuated in the opposite direction to direct pressurized air through the second flow restrictor 25 and into the pneumatic cylinder 24 via the retract port 24 b so as to drive the piston rod 36 and pusher block 32 toward the pneumatic cylinder 24 , release the tensioning cylinder 20 from the jig 26 , and permit removal of the tension releasing device 22 from the tensioning cylinder 20 . The second flow restrictor 47 may be considered optional as it may not be necessary or desirable to reduce or limit the speed of decompression of the tensioning cylinder 20 .
The preferred embodiment of the present invention has been described herein, but it is considered apparent that the invention is capable of numerous modifications or rearrangements of parts without departing from the spirit of the invention. Although the invention has been described herein as it relates to a drive device including the preferred pneumatic cylinder, it is considered apparent that the pneumatic (air) cylinder may be replaced by a hydraulic cylinder or an electric drive device (e.g., motor, gear reducer, transmission) without departing from the scope and spirit of the present invention. It is also contemplated that one skilled in the art may modify the pneumatic circuit to replace the flow restrictors with different means to adjust the speed of operation of the pneumatic cylinder, or that a single flow restrictor or means to adjust the speed of operation (i.e., in only the cylinder extension direction) may be desired. It is further considered apparent that the jig described herein is specially adapted to the particular tensioning cylinder used herein, and may be freely modified as necessary to accommodate different tensioning cylinders. Therefore, the present disclosure is not to be interpreted in a limitative fashion as the scope of the present invention is only defined by the claims appended hereto, which are to be given their broadest possible interpretation. | An apparatus for compressing an automatic belt tensioning cylinder to permit a belt to be placed around, the engine pulleys, includes a pneumatic cylinder and a jig, the jib being adapted to hold the tensioning cylinder during compression thereof by the pneumatic cylinder. The jig holds a plunger sensor that is operable to detect the presence of the tensioning cylinder, and to control the flow of pressurizing fluid such that the pneumatic cylinder cannot be operated in an extension direction when the tensioning cylinder is absent from the jig. | 5 |
FIELD OF THE INVENTION
This invention relates to an oven for baking cakes, bread and other articles and, more particularly, to an oven where the articles, once baked, are automatically removed from the baking compartment of the oven for storage.
BACKGROUND OF THE INVENTION
Some ovens are known, such as the one described in U.S. Pat. No. 2,038,361 issued Apr. 21, 1936 to Hawes, where a turning and ejecting device is used so that, after the baking operation has been completed, a pan carrying the article being baked is dumped in a manner to deposit the cake, bread or the like on a support ready for removal.
However, such oven has no use in places, such as restaurants, where articles like bread, muffins or rolls are continuously served to customers. These articles are baked or bought in advance in a quantity corresponding to an expected serving; in some places, where it is wished to serve them warm, or even simply to prevent them from drying, they are stored in a hot plate compartment.
OBJECTS OF THE INVENTION
It is an object of the present invention to provide an oven where such articles may be baked on a continuous basis and according to demand and, once baked, may be automatically dropped in a storage compartment where they are kept warm.
It is also an object of the present invention to provide such an oven with control means for causing the automatic fall of baked articles in the storage compartment after a pre-adjusted baking time has been completed.
It is also an object of the present invention to provide such an oven wherein the control means may be turned off so that it may be used for normal cooking without effecting the dumping of baked articles.
STATEMENT OF THE INVENTION
The present invention therefore relates to an oven for baking articles such as bread, cakes or the like comprising: a housing; a forwardly opening cavity defining a baking compartment; a door closing the cavity; a lower compartment located beneath the baking compartment for storing baked articles therein; the baking compartment having a bottom shelf separating the baking compartment and the lower compartment, the shelf being formed of a series of pivotably mounted plates adapted to hold articles to be baked; and means for pivoting the plates at predetermined time to cause articles baked in the baking compartment to fall under the action of gravity in the lower compartment.
Other objects and further scope of applicability of the present invention will become apparent from the detailed description given hereinafter; it should be understood, however, that the detailed description, while indicating preferred embodiments of the invention, is given by way of illustration only, since various changes and modifications within the spirit and scope of the invention will become apparent to those skilled in the art from reading the detailed description.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a perspective view of an oven constructed in accordance with the present invention;
FIG. 2 is a cross-sectional elevation view taken along lines 2--2 of FIG. 1;
FIG. 3 is a front, partly cross-sectional, elevation veiw as seen from lines 3--3 of FIG. 1;
FIG. 4 is a schematic elevation view as seen from lines 4--4 of FIG. 2 and showing the oven plates in a horizontal position;
FIG. 5 is a view similar to FIG. 4, showing the plates in a pivoting position; and
FIG. 6 is an electrical diagram for the operation of the oven of the present invention.
DESCRIPTION OF PREFERRED EMBODIMENTS
Referring to FIG. 1, there is shown, for illustrative purposes, a free-standing electric oven including a housing, generally denoted 10, with a forwardly opening cavity 12 defining a baking compartment. A door 14 closes the cavity. Housing 10 further includes a pull-out storage drawer 16 located beneath the baking compartment.
Referring to FIGS. 1-3, the baking compartment is defined by a pair of side walls 18 and 20, a rear wall 22 and a top wall 24. Thermal insulation 26 provided on the hidden faces of walls 18, 20, 22, 24 reduces the rate of heat transfer from the baking compartment to the outer walls 28, 30, 32 and 34 of housing 10.
The top wall 24 of the baking compartment is provided with a ventilation duct 36 to allow air to be evacuated through suitable openings 38 on the top outer wall 28 of housing 10. On the front face of housing 10, above door 14, an elongate panel 40 displays a series of manual and visual devices that include: a pair of switches 42 and 44, three lights 46,47 and 48, a temperature selector 50, a time-setting button 52 and a push-button 54; the function of these devices will hereinafter be described.
On side walls 18, 20, there are respectively provided two grill supports 56, 58 and two heating units 60, 62. A third heating unit 64 may be provided on the rear wall 22 or alternatively, there may be provided only one heating unit of sufficient wattage to suit the purpose of the oven. One type of suitable heating unit is the one sold under the trademark Chromatox. A temperature sensing element 66 is mounted to rear wall 22.
The bottom shelf or surface of the baking compartment 12 is formed of a series of plates; in the drawings, four plates of identical shape are shown as 68, 69, 70 and 71. Each plate, at opposite end thereof, is pivotably mounted to a frame 72 fixed to the housing 10. In the embodiment illustrated, each plate includes, centrally thereof, a rod 68a, 69a, 70a, 71a (see FIG. 4) which has its opposite ends mounted in the front and rear channel members 72a, 72b forming the front and rear parts of frame 72.
The rear outer wall 32 of housing 10 is at some distance from rear wall 22 of the baking compartment so as to define a space 74 therebetween in which the rear extremities 68a, 69a, 70a and 71a extend (see FIG. 2). As shown in FIGS. 4 and 5, these extremities are interconnected by a series of linking members 75,76,77,78,79,80,81. These linking members are simultaneously operated by a motor 82 fixedly mounted to frame 72 in space 74 and operatively connected to the linking members via a speed-reducing gear arrangement 84 and further linking members 85 and 86. As can be seen, plates 68,69 and plates 70,71 are arranged in tandem wherein one tandem pivots in a direction opposite to the other tandem. With such arrangement, the space provided between two adjacent pivoted plates for the dropping of the baked articles 88 in the lower compartment 16 is equal to at least the width of a plate.
A counterweight 87 may be provided for balancing the weight of the linking members and for assisting the pivotal movement of the plates.
A small gap 90 should be provided at least between adjacent plates so that, when the plates are in a horizontal shelf position, heat flow from the baking compartment to the lower compartment is permitted through these gaps to maintain the articles in lower compartment warm.
A general description of the oven described above will now be given.
Articles to be baked are placed on the bottom shelf of the baking compartment and door 14 is closed. Switch 44 is pushed to the ON position and light 46 lights. The temperature selector 50 is set at the desired baking temperature and lamp 47 lights. Button 52 is adjusted at the desired baking time. As said above, the present invention is particularly concerned with means for automatically controlling the baking operation and the falling of the baked articles in the lower compartment. Therefore, switch 42 is pushed to the AUTO position whereby light 48 begins to flash, which flashing is stopped, as hereinafter described, as soon as push-button 54 is actuated in operation.
The operation of these control means will now be described with reference to FIG. 6 which shows the ON-OFF switch 44 and its lamp 46, the temperature selector 50 and its lamp 47, and resistance R generally representing the three heating elements 60,62 and 64. The automatic control is on by closing switch 42. Immediate flashing of lamp 48 occurs due to current passing through normally closed contacts TO1 and TO3 (flashing is caused by the opening and closing of TO3 in response to current passing through the heat sensitive lamp TC3). This flashing occurs either at the beginning of the baking operation or after the baked articles have fallen into the lower compartment. Actuating push-button 54 causes the timer relay 96 to operate, which thereby opens contact TO1 (stopping flashing of lamp 48) and closes contact TC1. Once the baking time has been completed, contact TDC1 is closed causing motor 82 to be driven if switch 94 is closed (switch 94 is opened when the storage drawer 16 is in the pull-out position). The motor being driven, the plates pivot. As motor 82 is driven, it closes limit switch 92. TDC2 is a time delay lamp, similar to TC3, which, after a few seconds, causes the opening of TDO2. Thus, current is fed to motor 82 via the circuit that includes switch 92, closed contacts TC1, switch 94, contacts TDC1. After one complete revolution of the motor, the limit switch 92 is again opened cutting the current to the motor and returning the timer relay 96 to zero. Lamp TDC2 cools and TDO2 closes and is ready for the next baking operation. Also, with no current in the control circuit, TC1 and TDC1 open while TO1 closes causing lamp 48 to flash, as described above, indicating that more articles should be placed in the oven cavity for baking.
Although the invention has been described in relation to one specific form of the invention, it will be evident to the persons skilled in the art that it may be modified and refined in various ways. For example, some means may be provided in connection with the drawer to prevent it from being opened when the plates are rotating. Therefore, it should be understood that the present invention is not limited in interpretation except by the scope of the following claims. | The oven includes a baking compartment and a lower compartment located beneath the baking compartment for receiving baked articles therefrom; a horizontal shelf separates the baking compartment from the lower compartment and is formed of a series of pivotable plates; means are provided for pivoting the plates at predetermined time to cause the baked articles in the baking compartment to fall under the action of gravity in the lower compartment. | 5 |
This application claims priority under 35 U.S.C. § 120 of application Ser. No. 09/811,673 filed on Mar. 20, 2001 and issued as U.S. Pat. No. 6,740,746B2 on May 25, 2004, the contents of which are hereby incorporated by reference.
FIELD OF THE INVENTION
The present invention relates to a DNA molecule encoding a variant human paraoxonase (EC 3.1.1.2), and to said variant paraoxonase protein. The present invention also relates to a method for detecting or predicting the risk of, or predisposition to, cancer, coronary and cerebrovascular diseases, type 2 diabetes, hypertension, dementia, arthrosis, cataract and sensitivity to organophosphorus compounds in a subject, as well as to a kit or assay for carrying out the said method. This invention also relates to targeting paraoxonase enhancing treatments and to transgenic animals comprising a human DNA molecule encoding said variant paraoxonase and to a method of mutation search.
BACKGROUND OF THE INVENTION
The publications and other material used herein to illuminate the background of the invention are incorporated by reference.
Oxidative stress and free radicals have been implicated in the etiology of a number of diseases, including cancers, coronary heart disease, cerebrovascular disease, type 2 diabetes, hypertension, dementia and cataract. The human body has a number of endogenous free radicals scavenging systems which have genetic variability. The human serum paraoxonase (PON) is an enzyme carried in the high-density lipoprotein that contributes to the detoxification of organophosphorus compounds but also of toxic products of lipid peroxidation. 1-9 The paraoxonase hydrolyzes the toxic metabolites of several organophosphorus (OP) insecticides, pesticides and nerve agents.
The PON1 gene is polymorphic in human populations and different individuals also express widely different levels and activities of the paraoxonase enzyme, which is the protein product coded by the gene. 3,5-7
Several polymorphisms are currently known in human PON1. The Gln191 Arg poly-morphism was the first mutation of PON1 reported. 3,6 The second one is the Met54Leu. 3 Both these polymorphisms have been shown to affect serum PON activity. 6,10,11
Transgenic animals and with lowered paraoxonase activity can be used e.g. to test the effects of organophosphorus compounds, such as insecticides, pesticides and war agents, drugs that affect paraoxonase activity, other antioxidative compounds and drugs, and liver enzyme activity inducing agents.
A lot of methodological work has been done to locate disease-causing genes or candidate genes. However, there are no previous methodological studies concerning the methods of how to promote the search for mutations in a given or known candidate gene. To facilitate the finding of mutant DNA sequences, we developed a new method of phenotype-targeted gene sequencing.
SUMMARY OF THE INVENTION
One object of this invention is to provide a DNA sequence of a variant human PON1 gene and the amino acid sequence of the corresponding variant paraoxonase protein. Another object of the invention is to provide a method for screening a subject to assess if such subject is at risk of cancer, coronary or cerebrovascular disease, hypertension, type 2 diabetes, dementia, joint arthrosis or eye cataract, or at risk of being sensitive to organophosphate toxicity. The invention is also directed to a kit or an assay for said method, as well as to a probe for use in said method or kit. A further object of the invention is to provide a method for targeting a paraoxonase enhancing treatment for example for the above mentioned diseases and for organophospate poisoning, and/or for assessing the effectiveness of paraoxonase modifying treatments. A fourth object of the invention is to provide a transgenic animal with a gene encoding a variant paraoxonase. A fifth object of the invention is to provide a method for rapid search of gene mutations. These and further objects will be evident from the following description and claims.
According to one aspect, the invention concerns a DNA sequence comprising a nucleotide sequence encoding a variant paraoxonase protein with the Ile102Val mutation. The said mutation can, in the alternative, be named also Ile101Val, if the start codon atg (Met) is not included in the count. In the following description and claims, reference is made to the Ile102Val mutation, but said reference means within the scope of the invention in the alternative the Ile101Val mutation in case the alternative way of counting is used. The invention also concerns a variant paraoxonase protein with the Ile102Val mutation.
According to further aspect, the invention concerns a method for screening a subject to determine if said subject is a carrier of a variant gene encoding a variant paraoxonase, by determining the allelic pattern for the codon 102of the human PON1 gene, i.e. to determine if the said subject is a carrier of the Ile102Val mutation.
Specifically such a method comprises the steps of
a) providing a biological sample of the subject to be screened, and b) providing an assay for detecting in the biological sample the presence of the Ile102Val or Val102Val genotype of the human PON1 gene.
The assay result can be used for assessing the subject's risk to develop a low paraoxonase expression related disease such as cancer, coronary or cerebrovascular disease, type 2 diabetes, hypertension, dementia, arthrosis or cataract or sensitivity to organophosphorus compounds, and/or for assessing the effectiveness of paraoxonase-inducing therapy in a subject, whereby identification of a Ile102Val mutation being indicative of said risk being increased or effectiveness being modulated.
The present invention is thus directed to a method for detecting a risk of cancer, coronary or cerebrovascular disease, type 2 diabetes, hypertension, dementia, arthrosis or cataract in a subject, comprising isolating genomic DNA from said subject, determining the allelic pattern in the exon number 4 in the codon number 102 of the paraoxonase encoding PON1 gene in the genomic DNA, and identification of Ile102Val mutation indicating said risk being increased.
The present invention is also directed to a method for assessing the effectiveness of paraoxonase inducing therapy of a subject, comprising isolating genomic DNA from said subject, determining the allelic pattern in the exon number 4 in the codon number 102 of the paraoxonase encoding PON1 gene in the genomic DNA, and identification of Ile102Val mutation indicating said effectiveness being modulated, e.g. reduced.
The invention is also directed to a method for determining the presence or absence in a biological sample of a DNA sequence comprising a nucleotide sequence encoding a variant paraoxonase protein, the method comprising isolating genomic DNA from said subject, determining the allelic pattern in the exon number 4 in the codon number 102 of the paraoxonase encoding PON1 gene in the genomic DNA, and identification of Ile102Val mutation indicating the presence of said DNA sequence.
The techniques for carrying out such a method and presented here are intended to be non-limiting examples. One skilled in the art will readily appreciate that other methods for detection of the variant DNA sequence can be used, developed or modified.
One detection method is minisequencing which is based on a minisequencing reaction, in which an oligonucleotide that ends one nucleotide upstream the variant nucleotide, is enzymatically elongated by one nucleotide that is complementary to either the variant or the wild type nucleotide in the target sequence, and this added labelled nucleotide is detected. Such label can be, for example, radioactive or fluorescent label.
Another detection method is based on appearance or disappearance of an enzymatic cleavage site by the variant nucleotide. This kind of detection can be performed by first amplificating the target nucleotide sequence by a polymerase chain reaction with primers that flank the variant nucleotide, and then digesting the reaction product with a restriction endonuclease that recognises only the variant or only the wild-type sequence, producing DNA fragments of different length for each. These fragments may be recognised, for example, by gel electroforesis with DNA staining.
Yet another detection method is the oligonucleotide ligation assay, in which two allele specific oligonucleotide probes and one common oligonucleotide probe are used to distinguish between the variant and wild-type nucleotide. In this method, the target sequence is hybridised with the three oligonucleotide probes, and the probe pair that is complementary to the target sequence is joined enzymatically at the site of the variant nucleotide. The detection of the two alleles is based on differing labels, for example fluorescent labels of different colour, of the two allele specific oligonucleotide probes.
Furthermore, a detection method is the single stranded conformational analysis, in which the different alleles of a target sequence are identified on the basis of a difference in the electrophoretic mobility of the two alleles. In this method, the variant and wild-type target sequences that are in single stranded form, migrate with different speed through an electrophoresis matrix. Preferably, the target sequence is first amplified with a polymerase chain reaction, and the product is labelled for detection by radioactive or fluorescent label.
Yet furthermore, a detection method is sequencing, in which each nucleotide of the target sequence is identified. The variant allele is identified by the variant nucleotide.
Another detection method is allele specific hybridisation, in which an oligonucleotide probe is hybridised with the target sequence, and in which the probe is complementary only to the variant or wild-type allele. Preferably, two allele specific probes are used simultaneously to identify both alleles. Detection of a successful hybridisation and the determination of a genotype is based on detection of the probe-target duplex, on a basis of enzymatic colour reaction, or based on a label on the probe or on the target, for example a radioactive or a fluorescent label.
The present invention is also directed to a kit or assay for detecting a risk of cancer, coronary or cerebrovascular disease, type 2 diabetes, hypertension or dementia and sensitivity to organophosphorus compounds, and/or for assessing the need for or effectiveness of paraoxonase inducing therapy in a subject, comprising means for determining the allelic pattern in the exon number 4 in the codon 102 of the paraoxonase encoding PON1 gene in a genomic DNA sample. The assay may be a part of a DNA macroarray or microarray or a DNA chip or a DNA slide, which is intended for the detection of multiple gene mutations.
According to a further aspect, the present invention concerns a transgenic animal which carries a human DNA sequence comprising a nucleotide sequence encoding a variant human paraoxonase protein.
According to a farther aspect, the present invention concerns the method of phenotype-targeted gene sequencing.
DETAILED DESCRIPTION OF THE INVENTION
In order to find new previously unknown functional mutations in the human PON1 gene, phenotype-targeted hierarchial sequencing was used. The serum paraoxonase activity was determined for over 1000 serum samples. DNA samples of 10 persons with the lowest PON activity were first chosen for sequencing and they were sequenced through in all 9 exons with an ABI PRISM 3100 Genetic Analyzer (Applied Biosystems). A new previously unknown human PON1 mutation was found in codon number 102 in exon number 4, called PON Ile102Val, causing the change ATC to GTC; Ile to Val. After the new mutation was found, DNA samples of 100 men with low paraoxonase activities were sequenced, and the mutation was present in 9.0% of the subjects. Finally 1,595 DNA samples available in the KIHD (Kuopio Ischaemic Heart Disease Risk Factor Study) cohort were genotyped and the new mutation was found for 61 persons; 3.8% of the random population sample of men.
A polymerase chain reaction was carried out as follows: the genomic DNA was amplified in eight parts specific for the PON1-gene and for its exons 1 to 9. Eight different amplifications were made, with eight different PCR primer pairs (SEQ ID NO:5–20); one pair for each exon except for the exons 2 and 3 which were amplified together. All 9 exons were sequenced.
The kit or assay for use in the method according to the invention preferably contains the various components needed for carrying out the method packaged in separate containers and/or vials and including instructions for carrying out the method. Thus, for example, some or all of the various reagents and other ingredients needed for carrying out the determination, such as buffers, primers, enzymes, control samples or standards etc can be packaged separately but provided for use in the same box. Instructions for carrying out the method can be included inside the box, as a separate insert, or as a label on the box and/or on the separate vials.
Experimental Section
Polymerase Chain Reaction
The method according to the invention for determining the allelic pattern of the codon in question is preferably carried out as a polymerase chain reaction, in accordance with known techniques. 3 The PCR primer pair for human paraoxonase (PON 1) exon number 4 was as follow: 5′-CTCCTCCATGGTTATAAGGG-3′ (SEQ ID NO:9) and 5′-CCCAGAGTAAGAACATTATTC-3′ (SEQ ID NO: 10) (product size 315 bp). The primers were designed by Marja Marchesani and they were delivered by the AIV Institute, sequencing services (Kuopio, Finland). PCR amplification was conducted in a 25 μl volume containing 150 ng genomic DNA (extracted from peripheral blood), 10×PCR buffer, dNTP (10 mM of each), 20 pmol/μl of each primer, DNA-polymerase (2U/μl) (DyNAzyme™ DNA polymerase kit, Finnzymes, Espoo, Finland). Samples were amplified with a Biometra UNO programmable thermoblock (Biometra, Göttingen, Germany) with PCR programme conditions as follows: 95° C. for 3 minutes, Repeat following for 30 cycles: 95° C. for 30 seconds, 58° C. for 45 seconds, 72° C. for 45 seconds, 72° C. for 5 minutes, 4° C. hold. Amplified PCR-products were purified using the QIAquik PCR purification kit (QIAGEN, Valencia, Calif.).
Sequencing
Sequencing was made using a ABI PRISM® 3100 Genetic Analyzer (Applied Biosystems, Foster City, Calif.). The ABI PRISM® 3100 Genetic Analyzer is a fluorescence-based DNA analysis system of capillary electrophoresis with 16 capillaries operating in parallel, fully automated from sample loading to data analysis.
The sequencing reactions were made by using the DNA Sequencing Kit; Big Dye™ Terminator cycle sequencing v.2.0 ready reactions with ampliTaq® DNA polymerase (Fs ABI PRISM®, PE Biosystems, Foster City, Calif.). The sequencing primers were the same as the PCR primers: 5′ -CTCCTCCATGGTTATAAGGG-3′ (SEQ ID NO:9) or 5′ -CCCAGAGTAAGAACATTATTC-3′ (SEQ ID NO: 10). Cycle sequencing was made in the GeneAmp PCR System 9600 (PE Biosystems) with the programme as follows: Repeat the following for 25 cycles; rapid thermal ramp to 96° C., 96° C. for 10 seconds, rapid thermal ramp to 50° C., 50° C. for 5 seconds, rapid thermal ramp to 60° C., 60° C. for 4 minutes (to perform cycle sequencing under standard conditions, ABI PRISM® 3100 Genetic Analyzer Sequencing Chemistry Guide, Applied Biosystems).
Dye Terminator Removal and sequencing reaction clean-up was made using multiscreen 96-well filtration plates (Multiscreen(® -HV clear plates, Millipore, Bedford, Mass.). After purification the samples were denaturated at 94° C. for 1 min and the sequencing was done using the ABI PRISM® 3100 Genetic Analyzer using MicroAmp optical 96-well reaction plates (Applied Biosystems).
Genotyping
Specifically genotyping was done by extracting DNA from EDTA blood with a salting-out method after lysing red cells with 10 mM NaCl/10 mM EDTA. The 315 bp exon 4 PCR-product of the PON1 gene was digested with Sau 3 AI restriction endonuclease (New England BioLabs, Beverly, Mass.), mixed with 6× loading dye solution and run in 2.0 % agarose gel electroforesis. Identification of normal and mutant forms was based on different electrophoretic migration rates of the restriction fragments, resulting in distinct bands (normal form (Ile102Ile); 196 bp, 100 bp, 19 bp, heterozygote form (Ile102Val); 215 bp, 196 bp, 100 bp, 19 bp and homozygote form (Val102Val); 215 bp, 100 bp).
Determination of Serum PON Activity
Serum paraoxonase activity was measured based on its capacity to hydrolyse paraoxon. 100 μl of diluted serum (25-fold dilution in TRIS-HCl buffer, pH 8.0) was mixed with 100 μl of paraoxon (Paraoxon, Dr. Ehrensdorfer GmbH, Augsburg, Germany) (0.1 g in 66.1 ml of TRIS-HCl buffer, pH 8.0). Formation of p-nitrophenol was monitored photometrically at 405 nm (at 30 C), as previously described. 12
Testing for the Risk of Cancer, Coronary or Cerebrovascular Disease, Type 2 Diabetes or Hypertension
The study subjects were from the “Kuopio Ischaemic Heart Disease Risk Factor Study” (KIHD), a prospective population study to investigate risk factors for cardiovascular diseases, type 2 diabetes, hypertension, dementia and cancers. 13-17,19,20 The KIHD study protocol was approved by the Research Ethics Committee of the University of Kuopio, Finland. The study sample comprised men from Eastern Finland aged 42, 48, 54 or 60 years. A total of 2,682 men were examined during 1984–89. All participants gave a written informed consent. A DNA sample was available for 1595 men.
All cancer cases in the health care have been reported to a national cancer registry in Finland since 1953. 18 Our study cohort was record-linked to this cancer registry data by using the unique personal identification code (social security number) that all Finns have. Deaths in the cohort were obtained by record linkage to the national death certificate registry and hospitalizations by record linkage to the national hospital discharge registry. The history of hypertension and diabetes was assessed at baseline and at a 4-year follow-up by self-administered questionnaire, checked by an interviewer. Both at baseline and at the 4-year follow-up examination, blood pressure and fasting blood glucose were measured using identical methods both at baseline and at the 4-year follow-up. 16,20
The first occurrence of cancer after the KIHD baseline examination was registered in the cancer registry during 1984–97 for 60 cohort members. The primary site was prostate for 15 cancers. There were 1246 men with no prior CHD or cerebrovascular disease. Of these, 342 were smokers and 904 non-smokers. Of the smokers, 21 died of a cardiovascular cause by the end of 1998. Of the 515 men examined at baseline during 1984–86, 36 developed an arthrosis (ICD-10 M15–M19) by the end of 1998. Of the 1107 non-smoking men, 23 developed a cataract (ICD-10 H26–H29) by the end of 1998.
The association of the PON1 Ile102Val genotype with the risk of hypertension and diabetes was studied among 1038 men who were re-examined 4 years after the baseline examination, see references 15,19 for details of the re-examination. For the analysis of the incidence of hypertension, hypertensive (history of hypertension, antihypertensive medication or systolic BP 160 mmHg or more or diastolic BP 95 mmHg or more) and obese (body mass index 29 kg/m 2 or more) men and those with a history of cancer were excluded, leaving 488 men for the analysis. For the analysis of the incidence of type 2 diabetes, men with a history of cancer or prevalent diabetes at baseline (fasting blood glucose 6.7 mmol/l or more or treatment for diabetes) were excluded, after which exclusion there were 967 men for the analysis.
Lipoproteins were separated from fresh serum samples using ultracentrifugation and precipitation. 13,14 Cholesterol and triglyceride concentrations were measured enzymatically, plasma ascorbate and lipid-standardized plasma vitamin E concentration by HPLC methods 16,20 serum ferritin and apolipoproteins with a RIA 12 . The maximal oxygen uptake, a measure of cardiorespiratory capacity, was measured directly during a symptom limited exercise test. 15 Information regarding medical history and medications was obtained by interview. Smoking was recorded using a self-administered questionnaire and the dietary intake of nutrients was estimated by four-day food recording. 17
Risk-factor adjusted relative risks of cancer, prostate cancer and cardiovascular death were estimated by multivariate Cox proportional hazards modelling and those of incident hypertension and incident diabetes by multivariate logistic regression modelling. Covariates were selected by forward step-up modelling, using P-value of 0.10 as entry criterium. Missing values in covariates were replaced by grand means. Tests of statistical significance were one-sided. The statistical analyses were performed with SPSS version 10.0 for Windows.
Of all members of the study cohort, 61 (3.8%) were Val allele carriers of the PON1 gene Ile102Val polymorphism. To ascertain the penetrance of the PON1 102 mutation, serum PON activity was measured at the 11 -year re-examination for 783 cohort members as described above. The mean activity was 168.7 U/l in the wild Ile-Ile homozygotes vs. 70.7 U/l in 102Val carriers (p<0.001). In a 2-way analysis of variance (n=782), the Ile102Val polymorphism (p<0.001) was a stronger predictor of paraoxonase activity than the Leu54Met polymorphism (p=0.016).
In a multivariate Cox model adjusting for the strongest other risk factors in this cohort: maximal oxygen uptake, dietary vitamin C intake, smoking status (current smoker vs. non-smoker), body mass index, serum lipoprotein (a), dietary iron intake and apolipoprotein B, the relative risk of any cancer in the 102Val carriers was 2.4 (90% CI 1.0 to 5.5, p=0.052), compared with 102Ile homozygotes (p<0.001 for the model, Table 1). This association was stronger in 462 smokers with 24 incident cancers (RR 3.2, 90% CI 0.9–10.8, p=0.060) than in 1107 nonsmokers with 36 incident cancers (RR1.5, 90% CI 0.4–4.8, p=0.300).
The risk of prostate cancer was 4.9-fold (90% CI 1.4–17.4, p=0.021) among 102Val carriers compared with the wild homozygotes (Table 1). The model included maximal oxygen uptake, place of residence, serum HDL 2 cholesterol, histories of stroke and any atherosclerosis-related disease, cholesterol lowering medication, dietary iron intake and diastolic blood pressure as covariates.
The risk of cataract was examined in non-smokers, because smoking is an overwhelmingly powerful risk factor for cataracts. Among the 1107 non-smokers, the 102Val carriers had a 3.8-fold (90% CI 1.1–13.0, p=0.038) risk of cataract in a Cox model adjusting for blood glucose, blood leukocyte count, hair mercury content and the examination year 1989 (Table 1).
Smoking men who were PON1 102Val carriers had a 4.9-fold (90% CI 1.3–18.1, p=0.023) risk of cardiovascular death, compared with the 102Ile homozygotes (Table 1). The covariates included in the model were maximal oxygen uptake, history of any atherosclerosis-related disease, place of residence, serum apolipoprotein B level, plasma lipid-standardized vitamin E concentration (protective), examination year 1988 (vs. any other), and the serum fatty acid ratio (saturated/sum of monoenes and polyenes).
Among non-obese men, the PON1 102Val carriers had a 2.9-fold (90% CI 1.3–6.5, p=0.019) risk of hypertension, compared with non-carriers (Table 2), when adjusting for serum triglycerides, CHD in exercise test, dietary vitamin E intake (protective), frequency of hangovers, dietary retinol intake, and PON1 54 polymorphism.
As arthrosis is a chronic, gradually developing disease, only men examined in the first three years (1984–6) were included in a logistic regression analysis (Table 2). The carriers of the 102Val mutation had a 4.0-fold (90% CI 1.3–12.4, p=0.022) risk of developing an arthrosis during the follow-up, when adjusting for waist-to-hip circumference ratio, serum ferritin and dietary intakes of vitamin E and vitamin C.
Men with an 102Val allele had a 3.2-fold (90% CI 1.1–9.3, p=0.039) risk of type 2 diabetes, as compared with 102Ile homozygotes. Covariates in the model were serum fatty acid ratio (defined above), serum ferritin concentration and family history of obesity.
The Mini Mental State Examination was used to assess the presence of cognitive impairment and the degree of dementia of the KIHD participants aged 65–71 during 1998–2000. The test examines orientation (ten items), registration (three items), attention and calculation (five items), recall (three items) and language (nine items). A correct response to each item scores 1 (incorrect 0), which are summed to give a potential maximum score of 30. Higher scores indicate better cognitive function. The mean score was 25.5 (SD 2.5) among the 26 carriers of the PON102 Val allele and 26.4 (SD 2.2) among 338 non-carriers for whom data were available (one-sided p=0.031 in t-test, exact p=0.045). The Mini Mental State examination score was directly associated Pearson's correlation coefficient 0.14, p=0.008, n=359) with serum paraoxonase enzyme activity. This association remained statistically significant (p=0.012) after a statistical adjustment for age and socio-economic status, which were other strongest predictors of the score.
TABLE 1
The association of PON1 102Val carrier status with the
risk of any cancer, prostate cancer and cardiovascular
death in multivariate Cox regression models in healthy men
Number of men free of
disease at entry
At
Who
the start of
developed
Relative
Disease
follow-up
disease
risk (90% CI)*
p-value
Any cancer**
1569
60
2.35 (1.00, 5.54)
0.052
Prostate
1569
15
4.86 (1.36, 17.36)
0.021
cancer**
Cataract**
1107
23
3.79 (1.10, 12.98)
0.038
non-smokers
Cardiovascular
342
21
4.93 (1.34, 18.10)
0.023
death***
smokers
*The step-up models included other strongest risk factors.
**Men with a history of cancer were excluded.
***Men with a history of coronary heart disease or cerebrovascular stroke were excluded.
TABLE 2
The association of PON1 102Val carrier status with the
risk of hypertension and type 2 diabetes in multivariate
logistic regression models in healthy men
Number of men free of
disease at entry
At
Who
the start of
developed
Relative
Disease
follow-up
disease
risk (90% CI)*
p-value
Hypertension**
488 non-
109
2.85 (1.25, 6.51)
0.019
obese men
Arthrosis***
515 men
36
3.99 (1.29, 12.36)
0.022
examined in
1984–6
Type
967 non-
33
3.17 (1.08, 9.28)
0.039
2 diabetes****
diabetic men
*The step-up models included other strongest risk factors.
**Men with a history of cancer or prevalent hypertension were excluded.
***Men with a history of cancer were excluded.
****Men with a history of cancer or prevalent diabetes were excluded.
REFERENCES
1 Mackness M I, Thompson H M, Hardy A R, Walker C H. Distinction between ‘A’-esterases and arylesterases. Implications for esterase classification. Biochem J 1987; 245: 293–6
2 Mackness M I, Arrol S, Durrington P N. Paraoxonase prevents accumulation of lipoperoxides in low-density lipoprotein. FEBS Lett 1991; 286: 152–4.
3 La Du B N, Adkins S, Kuo C L, Lipsig D. Studies on human serum paraoxonase/arylesterase. Chem Biol Interact 1993 June; 87 (1–3):25–34
4 Humbert R, Adler D A, Disteche C M, Hassett C, Omiecinski C J, Furlong C E. The molecular basis of the human serum paraoxonase activity polymorphism. Nature Genet 1993; 3: 73–6.
5 Davies H G, Richter R J, Keifer M, Broomfield C A, Sowalla J, Furlong C E. The effect of the human serum paraoxonase polymorphism is reversed with diazoxon, soman and sarin. Nature Genet 1996; 14: 334.
6 Mackness M I, Mackness B, Durrington P N, Connelly P W, Hegele R A. Paraoxonase: biochemistry, genetics and relationship to plasma lipoproteins. Curr Opin Lipidol 1996; 7: 69–76.
7 Mackness M I, Arrol S, Mackness B, Durrington P N. Alloenzynes of paraoxonase and effectiveness of high-density lipoproteins in protecting low-density lipoprotein against lipid peroxidation. Lancet 1997; 349: 851–2.
8 Mackness B, Durrington P N, Mackness M I. Polymorphisms of paraoxonase genes and low-density lipoprotein peroxidation. Lancet 1999; 353: 468–9.
9 Shih D M, Gu L, Xia Y-R, et al. Mice lacking serum paraoxonase are susceptible to organophosphate toxicity and atherosclerosis. Nature 1998; 394: 284–7.
10 Garin M C, James R W, Dussoix P, et al. Paraoxonase polymorphism Met-Leu54 is associated with modified serum concentrations of the enzyme. A possible link between the paraoxonase gene and increased risk of cardiovascular disease in diabetes. J Clin Invest 1997; 99: 62–6.
11 Mackness B, Mackness M I, Arrol S, Turkie W, Durrington P N. Effect of the molecular polymorphisms of human paraoxonase (PON1) on the rate of hydrolysis of paraoxon. Br J Pharmacol 1997; 122: 265–8.
12 Mackness M I, Harty D, Bhatnagar D, Winocour P H, Arrol S, Ishola M, Durrington P N. Serum paraoxonase activity in hypercholesterolemia and insulin-dependent diabetes mellitus. Atherosclerosis 1991; 86: 193–9.
13 Salonen J T. Is there a continuing need for longitudinal epidemiologic research?—The Kuopio Ischaemic Heart Disease Risk Factor Study. Ann Clin Res 1988; 20: 46–50.
14 Salonen J T, Nyyssönen K, Korpela H, Tuomilehto J, Seppänen R, Salonen R. High stored iron levels are associated with excess risk of myocardial infarction in Eastern Finnish men. Circulation 1992; 86: 803–11.
15 Lakka T A, Venäläinen J M, Rauramaa R, Salonen R, Tuomilehto J, Salonen J T. Relation of leisure-time physical activity and cardiorespiratory fitness to the risk of acute myocardial infarction. N Engl J Med 1994; 330: 1549–54.
16 Salonen J T, Nyyssönen K, Tuomainen T-P, Mäenpää P H, Korpela H. Kaplan G A, Lynch J, Helmrich S P, Salonen R. Increased risk of non-insulin dependent diabetes mellitus at low plasma vitamin E concentrations: a four year follow-up study in men. Brit Med J 1995; 311: 1124–7.
17 Ihanainen M, Salonen R, Seppänen R, Salonen J T. Nutrition data collection in the Kuopio Ischaemic Heart Disease Risk Factor Study: Nutrient intake of middle-aged eastern Finnish men. Nutr Res 1989; 9: 89–95.
18 Teppo L, Pukkala E, Lehtonen M. Data quality and quality control of a population-based cancer registry. Experience in Finland. Acta Oncologica 1994; 33: 365–9.
19 Everson S A, Goldberg D E, Kaplan G A, et al. Hopelessness and risk of mortality and incidence of myocardial infarction and cancer. Psychosom Med 1996; 58: 113–21.
20 Salonen J T, Lakka T A, Lakka H-M, Valkonen V-P, Everson S A, Kaplan G A. Hyperinsulinemia is associated with the Incidence of hypertension and dyslipidemia in middle-aged men. Diabetes 1998; 47: 270–275. | This invention is directed to a DNA sequence comprising a nucleotide sequence encoding a variant paraoxonase protein and to said variant paraoxonase protein as well as a method and a kit for detecting a risk of cancer, coronary or cerebrovascular disease, hypertension, type 2 diabetes, dementia, joint arthrosis, cataract, or sensitivity to organophosphorus compounds in a subject, the method comprising isolating genomic DNA from said subject, determining the allelic pattern for the codon 102 of the paraoxonase encoding PON1 gene in the genomic DNA, identification of Ile101Val mutation indicating said risk being increased and for targeting paraoxonase activity modulating therapies. Further this invention relates to transgenic animals comprising a human DNA molecule encoding said variant paraoxonase and to a method of phenotype-targeted gene sequencing. | 2 |
CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] This application claims priority as a divisional application from U.S. patent application Ser. No. 11/680,303, filed on Feb. 28, 2007, which claims priority from U.S. Provisional Patent Application Ser. No. 60/778,040, filed on Mar. 1, 2006, which are each incorporated by reference herein in their entirety.
FIELD OF THE INVENTION
[0002] The present invention relates to tire inflation valves, and more specifically to a tire inflation valve that is releasably imbedded within a tire rim that forms part of a central tire inflation system of a vehicle.
BACKGROUND OF THE INVENTION
[0003] In order to inflate and deflate the tires forming part of the wheels on a vehicle, valves are located on the rims or hubs of the wheels to be used for selectively inflating and deflating the tires disposed around the wheel rims. Air can be directed through the valves either into or out of the tires to increase or decrease the air pressure in the tires, correspondingly altering the ride characteristics of the individual wheel, and the overall vehicle.
[0004] On most occasions the valves are only accessible from the exterior of the wheel, such that it is necessary to exit the vehicle to use the valve to inflate or deflate the tire. However, various central tire inflation systems have been developed that provide valves on the wheel rims that can be remotely activated from the cab or other driver compartment for the vehicle. These systems enable an individual to control the flow of air into and out of the vehicle tires using the valves to vary the ride characteristics of the tires as necessary. Examples of systems of this type are illustrated in each of Howald et al. U.S. Pat. No. 6,474,383, and Wang et al. U.S. Pat. No. 7,168,468, both of which are incorporated by reference herein. In each of theses patents, the rim of the wheel is formed with internal passages that enable air to be selectively passed from a compressed air supply through the passages to a valve. The valve is selectively operable from within the passenger compartment or cab of the vehicle to enable air to flow through the valve and into the tire through the passages formed in the rim. The passages are formed in either the outer rim (as in the '383 patent) or in the inner rim (as in the '468 patent) and form a flow path from an inlet for the compressed air through the rim and the associated valve to an opening on the exterior surface of the rim component that is located between the opposed sides of the wheel formed by the inner and outer rim sections. This outlet is also located between the beads of a tire mounted to the wheel, such that air exiting the outlet is retained within the tire to increase the air pressure, i.e., inflate the tire as desired.
[0005] Nevertheless, these prior art central tire inflation systems utilize passage designs that require the valves utilized therewith to have designs which require a number of additional components for the incorporation of the valves into tires for use with existing central tire inflation systems. These additional components greatly increase the cost and complexity of the valves, causing the valves to fail on a regular basis, necessitating that the valves be repaired and/or replaced on a consistent basis.
[0006] Additionally, the configuration of the passages in the rim in the prior art systems requires that the valve be positioned in an abutting relationship with the passages on the exterior surface of the rim component, i.e., surface-mounted on the rim. This positioning for the valve on the exterior of the rim in an exposed location where the valve can easily be damaged by debris or other objects striking the valve when the vehicle is in operation. In most instances, a wheel cover is required to protect the valve and other ancillary components for the central tire inflation system, such as hoses and fittings. The wheel cover is formed of steel or a composite material, and can trap rocks within the cover when in use, turning the cover into a rock tumbler that enables the rocks to damage the valve and other components of the CTIS system on the wheel that the cover is meant to protect.
[0007] As a result, it is desirable to develop a valve for use in a central tire inflation system that includes a minimum of parts and that can be incorporated into a number of different types of wheels. Also, it is desirable to develop a valve that can be positioned within a rim of a wheel incorporating a central tire inflation system that in a recessed or imbedded manner to effectively reduce the profile of the valve on the exterior of the wheel, thereby reducing the likelihood of the valve being struck and damaged during operation of the vehicle.
SUMMARY OF THE INVENTION
[0008] According to a first aspect of the present invention, a tire valve is provided that includes a simplified construction that can be seated directly within a tire wheel. The valve includes a main body that is positionable in a sealed configuration within an opening in the wheel rim in communication with the interior of the tire via passages formed within the rim. The body is also positioned within the opening in communication with a pressurized air source that is used to inflate or deflate the tire by passing air through the valve and along the passages to the tire. The main body encloses a valve mechanism that can be selectively operated in response to variations in the air pressure supplied to the valve, such that control of the operation of the valve can be remotely controlled via a controller connected to the pressurized air source. The positioning of the valve within the opening formed in the rim operates to reduce the profile of the valve that is positioned on the exterior of the wheel, to greatly reduce the chance of the valve being struck and damaged when the vehicle is in operation.
[0009] According to another aspect of the present invention, the valve is releasably mounted in the opening, such that the valve can be removed from the opening and replaced without having to remove the wheel, or a component of the wheel from the vehicle. An anchor ring is secured around the valve on the exterior side of the rim, and serves to both protect the valve within the opening and to maintain the valve in position with regard to each of the passages within the wheel and the pressurized air inlet. The valve is releasably secured to the anchor ring, such that the valve can be removed from the rim and the anchor ring without disengaging the anchor ring from the rim, or having to remove the rim from the vehicle.
[0010] According to another aspect of the present invention, the valve mechanism housed in the main body of the valve includes a minimum of moving parts to simplify the construction of the valve and to increase the longevity of the valve. These components are situated in a single, self-contained unit within the main body beneath a removable cap in a manner that also enables the valve mechanism to be easily removed, cleaned and/or replaced if necessary without having to remove the entire valve assembly from the wheel.
[0011] Numerous other aspects, features and advantages of the present invention will be made apparent from the following detailed description taken together with the drawing figures.
BRIEF DESCRIPTION OF THE DRAWINGS
[0012] The drawings illustrate the best mode currently contemplated of practicing the present invention.
[0013] In the drawings:
[0014] FIG. 1 is an isometric view of a wheel assembly constructed according to the present invention;
[0015] FIG. 2 is a front plan view of the wheel assembly of FIG. 1 ;
[0016] FIG. 3 is a cross-sectional view of the wheel assembly along line 3 - 3 of FIG. 2 ;
[0017] FIG. 3A is a circular sectional view along line 3 A- 3 A of FIG. 3 showing a first embodiment of a valve cartridge used in the wheel assembly of the present invention in the open position;
[0018] FIG. 3B is a circular sectional view along line 3 B- 3 B of FIG. 3 showing the valve cartridge in a closed position:
[0019] FIG. 4 is a cross-sectional view of a second embodiment of the valve cartridge utilized in the wheel assembly of FIG. 1 in the closed position;
[0020] FIG. 5 is a cross-sectional view of the valve cartridge of FIG. 4 in the open position;
[0021] FIG. 6 is an isometric view of the main body of the valve cartridge of FIG. 4 ;
[0022] FIG. 7 is a side plan view of the main body of FIG. 6 ;
[0023] FIG. 8 is a top plan view of the main body of FIG. 6 ;
[0024] FIG. 9 is an isometric view of an anchor ring utilized with the valve cartridge of FIG. 4 ;
[0025] FIG. 9A is a cross-sectional view of a securing cup utilized with the valve cartridge of FIG. 4 ;
[0026] FIG. 9B is an exploded, cross-sectional view of the securing cup and valve cartridge of FIG. 9A ;
[0027] FIG. 10 is a bottom isometric view of a valve seat used in the valve cartridge of FIG. 4 ;
[0028] FIG. 11 is a top isometric view of the valve seat of FIG. 10 ;
[0029] FIG. 12 is an isometric view of a disk screen used in the valve cartridge of FIG. 4 ;
[0030] FIG. 13 is an isometric view of a valve bushing of the valve cartridge of FIG. 4 ;
[0031] FIG. 14 is an isometric view of a cap used in the valve cartridge of FIG. 4 ;
[0032] FIG. 15 is a top isometric view of a piston used in the valve cartridge of FIG. 4 ;
[0033] FIG. 16 is a bottom isometric view of the piston of FIG. 15 ;
[0034] FIG. 17 is an isometric view of a ring screen used in the valve cartridge of FIG. 4 ;
[0035] FIG. 18 is an isometric view of a first embodiment of a valve stem utilized with the valve cartridge of FIG. 4 ;
[0036] FIG. 19 is an isometric view of a second embodiment of a valve stem utilized with the valve cartridge of FIG. 4 ;
[0037] FIG. 20 is an isometric view of a third embodiment of the valve stem utilized with the valve cartridge of FIG. 4 ; and
[0038] FIG. 21 is a cross-sectional view of the first embodiment of the valve cartridge in the closed position as shown in FIG. 3B .
DETAILED DESCRIPTION OF THE INVENTION
[0039] With reference now to the drawing figures in which like reference numerals designate like parts throughout the disclosure, a wheel assembly 1000 including an inner rim member 10 and an outer rim member 24 is illustrated in FIGS. 1-3B . The inner rim 10 includes a peripheral wall 12 adapted to support an inflatable tire 200 and an outer flange 14 at one end of the wall 12 . Opposite the outer flange 14 , the inner rim 10 includes a mounting wall 16 extending inwardly from the peripheral wall 12 . The mounting wall 16 defines a central opening 17 that receives a hub (not shown) and includes a number of first openings 18 spaced around the circumference of the mounting wall 16 adjacent the peripheral wall 12 , a number of second openings 19 spaced inwardly from the first openings 18 opposite the peripheral wall 12 , and a valve mounting opening 20 disposed between adjacent second openings 19 .
[0040] Each of the first openings 18 receives a wheel stud 22 therein that extends through the mounting wall 16 for connecting the outer rim 24 to the inner rim 10 . The outer rim 24 and the outer flange 14 on the inner rim 12 define the outer edges of the wheel assembly 1000 within which opposed beads (not shown) of a tire (not shown) are mounted and retained. The second openings 19 are used to mount the wheel assembly 1000 on a number of hub bolts (not shown) that can secure the wheel assembly 1000 and tire to the hub (not shown) of a vehicle (not shown).
[0041] The inner rim 12 also includes an air passage or channel 26 formed in the inner rim 10 that extends from the valve opening 20 through the peripheral wall 12 . The air channel 26 is formed in the inner rim 10 in any suitable manner, such as by drilling, and terminates in a groove 28 formed in the peripheral wall 12 , and that preferably extends radially inwardly from the channel 26 towards the center of the wall 12 . When the outer rim 24 is affixed to the inner rim 10 , the outer rim 24 is positioned over the air channel 26 and a portion of the groove 28 to define an air flow path between the valve opening 20 and the exterior of the peripheral wall 12 , over which the tire is positioned, thereby creating a path for introducing and removing air from the interior of the tire.
[0042] Alternatively, the shape and direction of the groove 28 can be varied as desired, so long as the end of the groove 28 opposite the channel 26 is not completely obscured by the outer rim 24 . Additionally, the groove 28 can be omitted entirely, and the channel 26 can be formed to extend from the opening 20 to a point on the peripheral wall 12 below the outer rim 24 when the outer rim 24 is secured to the inner rim 10 . Also, the outer rim 24 can be formed in a manner that allows communication between the channel 26 and the tire when the wheel assembly 10 is completed, such as by forming the groove 28 in the outer rim 24 . Further, the inner rim 10 and the outer rim 24 can be formed as a single piece rim (not shown), eliminating the need for securing the sections to one another.
[0043] Within the valve opening 20 is mounted a control valve cartridge 30 that is used to control the flow of air into and out of the tire 200 . By mounting the valve cartridge 30 within the opening 20 extending through the inner rim 10 , and located radially inwardly of the outer rim 24 , the valve 30 is protected from being damaged by objects stuck by and striking the inner rim 10 or outer rim 24 . This is because when the valve 30 is disposed within the opening 20 , a much smaller portion of the valve 30 is disposed on the exterior surface of the wheel assembly 1000 . Also, the positioning of the valve opening 20 adjacent to the first openings 18 and second openings 19 positions the wheel studs 22 and the hub mounting bolts close to the portion of the valve 30 outside of the opening 20 . The studs 22 and bolts are longer than the valve 30 , such that they prevent objects and debris from being able to move far enough into the wheel assembly 1000 to contact the valve 30 .
[0044] Referring now to FIGS. 4-20 , in one embodiment, the valve cartridge 30 includes a main body 32 that is positioned within and frictionally or sealingly engaged with the valve opening 20 . The main body 32 , as best shown in FIGS. 4-8 , includes a lower end 34 and an upper end 36 connected to one another. The lower end 34 is preferably cylindrical in shape, and includes a number of air inlet shafts 38 extend through the lower end 34 that are aligned with one or more mating holes (not shown) in the wheel hub (not shown) to provide a connection to the pressurized air supply (not shown) used to inflate or deflate the tire 200 . The lower ends of the inlet shafts 38 are covered by disk screen 40 ( FIG. 12 ) engaged within the lower end of the main body 32 . Between the shafts 38 is disposed a central chamber 42 . The central chamber 42 has a wide upper portion 43 a , and a narrow lower portion 43 a from which extend a number of air outlet shafts 44 which are positioned between and oriented perpendicular to the inlet shafts 38 . The outlet shafts 44 are surrounded on their outer ends on the exterior of the main body 32 by a cylindrical ring screen 46 ( FIG. 17 ) formed similarly to the disk screen 40 . Above and below the screen 46 on the exterior of the main body 32 are disposed channels 48 in which are located sealing members 50 to enable the main body 32 to frictionally and sealingly engage the circumference of the valve opening 20 , securely holding the valve 30 therein.
[0045] The upper end 36 defines a central recess 52 that extends the entire length of the upper end 36 . Opposite the recess 52 , the exterior of the upper end 36 includes a screw thread 54 . To assist the sealing members 48 and 50 in securely holding the valve 30 within the valve opening 20 , an anchor plate or ring 56 , best shown in FIGS. 4 , 5 , and 9 , is threadedly engaged with the thread 54 on the upper end 36 . The anchor plate 56 includes a circular central part 58 that defines a central opening 60 having a threaded interior surface 62 matable with the thread 54 . Extending from the central-part 58 , and preferably from approximately opposite side of the central part 58 , are a pair of securing flanges 64 each having an aperture 66 defined therein. The apertures 66 can receive bolts (not shown) therein that secure the flanges 64 to the inner rim 10 , and the valve 30 within the opening 20 .
[0046] As an alternative to the anchor ring 56 , especially for use in situations where the rim 10 is not sufficiently thick to enclose the valve cartridge 30 , a valve cup 300 is illustrated in FIGS. 9A and 9B . The cup 300 is formed with an open upper end 302 and a closed lower end 304 between which extends a circular wall 306 . The circular wall 306 includes a lower section 310 and an upper section 308 separated by an annular shoulder 312 . The lower section 310 includes a number of apertures 314 formed therein that extend through the lower section 310 generally perpendicular to the wall 306 . The upper section 308 includes a threaded interior surface 316 that extends the length of the upper section 308 . A bottom wall 318 forming the closed lower end 304 includes an air inlet 320 that is in fluid communication with the interior 322 of the cup 300 . The air inlet 320 is positioned within a sleeve 324 that extends outwardly from the bottom wall 318 and includes a threaded exterior surface 326 extending the length of the sleeve 324 .
[0047] The main body 32 of the valve cartridge 30 can be positioned within the cup 300 by inserting the lower end 34 into the lower section 310 , and threadedly engaging the upper section 36 with the interior surface 316 of the upper section 308 . The interior surface 316 allows the upper end 36 to be inserted into the cup 300 until the upper end 36 contacts the annular shoulder 312 . In this position, the upper end 36 of the main body 32 extends outwardly from the upper end 302 of the cup 300 , while the lower end 34 is spaced a short distance above the lower end 304 . Additionally, when the main body 32 is fully inserted within the cup 300 , the air outlet shafts 44 in the lower end 34 are generally aligned with the apertures 314 in the lower section 310 , and are sealed off from the upper end 302 and lower end 304 of the cup 300 by the sealing members 50 located within the channels 48 extending around the lower end 34 . Also, because the upper end 36 is positioned above the upper end 302 of the cup 300 , the cap 70 can be engaged with the main body 32 as discussed previously, to retain the various components of the valve cartridge 30 within the main body 32 .
[0048] Either prior to or after insertion of the main body 32 within the cup 300 , the cup 300 can be secured to a wheel rim 10 such that the apertures 314 are positioned in alignment with the passage 26 to enable air passing through the valve cartridge 30 and out the outlet shafts 44 to enter the passage 26 . Also, the sleeve 324 within which the air inlet 320 is disposed is engageable with a threaded hub air outlet (not shown) to both securely engage the air inlet 320 for the cup 300 with the air outlet on the hub, and to provide added support to the cup and valve cartridge 30 .
[0049] To hold the valve components of an interior valve mechanism 81 within the central recess 52 , a cap 70 is engageable with the thread 54 above the anchor plate 56 . As best shown in FIGS. 4 , 5 and 14 , the valve cap 70 is generally cylindrical in shape, having a top wall 72 from which downwardly extends a circular side wall 74 . The side wall 74 includes a threaded interior surface 76 that is engageable with the thread 54 on the upper end 36 . Immediately adjacent the top wall 72 , the side wall 74 includes a peripheral notch 78 that is co-linear with the threaded interior surface 76 and that encloses a sealing member 80 therein. Thus, when the cap 70 is engaged with the upper end 36 of the main body 32 , the sealing member 80 sealingly engages the upper end 36 above the thread 54 to provide and airtight sea between the upper end 36 and the cap 70 . Being threadedly engaged with the upper end 36 , the cap 70 is also removable from the main body 32 in order to clean or replace the interior components of the valve 30 without also removing the main body 32 from the valve opening 20 . This is due to the ability of the main body 32 to be secured within the valve opening 20 by either or both of the sealing members 48 and 50 and the anchor plate 56 , which are each located below the cap 70 .
[0050] Turning now to FIGS. 4 , 5 , 10 and 11 , the interior valve mechanism 81 includes a valve seat 82 is disposed within the central recess 52 of the upper end 36 of the main body 32 . The valve seat 82 includes a wide upper end 84 and a narrow lower end 86 . The narrow lower end 86 includes a number of air flow tubes 88 formed therein that extend from the exterior of the lower end 86 into fluid communication with a central opening 90 located in the center of the lower end 86 . The lower end 86 also includes an axially extending ring 92 at the lowermost end. The ring 92 provides an alignment and engagement point for the lower end 86 of the valve seat 82 to rest on and sealingly engage a sealing ring 94 located within the wide upper end 43 a of the chamber 42 in the main body 32 . This engagement provides an airtight seal between the lower end 86 of the valve seat 82 and the main body 32 .
[0051] The wide upper end 84 of the valve seat 82 defines an inner chamber 96 that is disposed concentrically with the central opening 90 in the lower end 86 . As best shown in FIGS. 10 and 11 , on the exterior of the upper end 84 opposite the chamber 96 are formed a number of spaced air flow passages 98 that extend the entire length of the upper end 84 to allow air entering through the shafts 38 in the main body 32 to flow upwardly around the valve seat 82 . Immediately below the upper end 84 of the valve seat 82 , the passages 98 extend inwardly into fluid communication with the inner chamber 96 of the valve seat 82 .
[0052] Inside the upper end 84 of the valve seat 82 adjacent the opening 90 , the chamber 96 defines a circular retaining wall 100 having an annular shoulder 102 defined therein. The retaining wall 100 and shoulder 102 are used to receive and engage a valve bushing 104 . As best shown in FIGS. 4 , 5 and 13 , the valve bushing 104 is generally cylindrical in shape and defines a central aperture 106 that, when bushing 104 is disposed on the shoulder 102 within the retaining wall 100 , is positioned concentrically with the chamber 96 and the opening 90 in the valve seat 82 as well as with the central chamber 42 in the lower end 34 of the main body 32 . A sealing member 108 is positioned between the bushing 104 and a peripheral flange 110 separating the opening 90 from the chamber 96 to provide an airtight seal between the bushing 104 and the upper end 86 of the valve seat 82 .
[0053] Referring now to FIGS. 4 , 5 , 15 and 16 , a valve piston 112 is disposed within the chamber 96 above the bushing 104 . The piston 112 is generally cylindrical in shape with a diameter slightly less than that of the interior of the chamber 96 , and including a peripheral recess 114 within which is disposed a sealing member 116 . The piston 112 is slidably movable within the chamber 96 and the sealing member 116 engages the chamber 96 in manner that provides an airtight seal between the piston 112 and the chamber 96 as the piston 112 moves within the chamber 96 .
[0054] The piston 112 also includes a threaded bore 118 extending through the center of the piston 112 in a direction perpendicular to the recess 114 . The bore 118 is threadedly engaged with a threaded end 120 of a valve stem 122 , best shown in FIGS. 4 , 5 and 18 - 20 . The valve stem 122 extends from the threaded end 120 downwardly through the aperture 106 in the bushing 104 . Downwardly from the threaded end 120 , the stem 122 has a diameter slightly less than that of the aperture 106 in the bushing 104 , such that the busing 104 provides a guide for the movement of the valve stem 122 when moved as a result of the movement of the piston 112 . Below the bushing 104 , the stem 122 extends through the opening 90 and into the chamber 42 , where the stem 122 terminates with a radial stem flange 124 positioned below and in sealing engagement with the sealing flange 94 opposite the valve seat 82 . The stem flange 124 includes a number of tines 126 that extend outwardly from the flange 124 and are crimped or bent inwardly to grip one end of a spring 128 . The spring 128 is positioned between the stem flange 124 and the lowermost end of the central chamber 42 , such that the spring 128 urges the valve stem 122 and the piston 112 upwardly, to sealingly engage the flange 124 with the sealing flange 94 , and to position the piston 112 adjacent the upper end 84 of the valve seat 82 . The stem flange 124 can also include various spring-engaging features in different embodiments ( FIGS. 18-20 ) that enhance the ability of the flange 124 to stay in engagement with the spring 128 , such as outwardly extending or angled tabs 129 , a securing ring 130 extending downwardly from the flange 124 and having a diameter larger or smaller than that of the spring 128 for the spring 128 to seat therein or therearound, respectively, or a 130 ring including a slot (not shown) that receives and engages a part of the spring 128 to positively hold the flange 124 on the spring 128 .
[0055] Looking now at FIG. 4 , when the valve 30 is not in operation no air flow is passing through the valve 30 , such that the bias of the spring 128 urges the flange 124 against the sealing flange 94 to prevent any air flow from the inlet shafts 38 in the lower end 34 of the main body 32 , through the air tubes 88 in the lower end 86 of the valve seat 82 and past the sealing flange 94 into the air outlet shafts 44 in the lower end 43 of the main body 32 to the tire 200 . However, upon activation of the central tire inflation system to which the valve 30 is connected, a pressurized air flow is directed from the hub through the air inlet shafts 38 and along the air flow passages 98 in the valve seat 82 into the upper end 36 of the main body 32 above the piston 112 . The pressure of the air flow builds in the upper end 36 until the pressure overcomes the bias of the spring 128 and the air pressure in the tire 200 acting through the valve 30 . Normally, this pressure is selected to be approximately one-third of the pressure in the tire 200 , but the valve 30 can be set to operate at alternative pressures depending upon the particular use to which the valve 30 is put. Once the pressure in the upper end 36 reaches this point, the pressure presses downwardly on the piston 112 , causing the piston 112 and valve stem 122 to move downwardly with respect to the bushing 104 , valve seat 82 and main body 32 . Sufficient movement of the piston 112 due to the air pressure in the upper end 36 above the piston 112 disengages the stem flange 124 from the sealing flange 94 , allowing air to flow around the stem flange 124 and into the tire 200 through the air outlet shafts 44 , as shown in FIG. 5 . Once the desired air pressure for the tire 200 has been reached and sensed by the central tire inflation system, the air flow to the valve 30 through the air inlet shafts 38 is stopped, allowing the spring 128 to re-engage the stem flange 124 with the sealing flange 94 and maintain the desired pressure in the tire 200 . The valve 30 may also include a suitable venting member (not shown) to enable the valve 30 to eliminate any backpressure in the valve 30 that occurs during the operation of the valve 30 .
[0056] Referring now to FIGS. 3A , 3 B and 21 , another embodiment of the valve 230 is illustrated. The valve 230 is formed similarly to the valve 30 illustrated and discussed previously, with the same general configuration as the previous embodiment, including the main body 32 ′, the valve seat 82 ′ and the cap 70 ′.
[0057] However, the valve seat 82 ′ is modified to eliminate the air flow passages 98 and to include a pair of sealing members 232 and 234 disposed on the exterior of the valve seat 82 ′ within grooves 236 . The sealing members 232 and 234 are preferably low friction seals and extend around the valve seat 82 ′ in the grooves 236 generally perpendicular to the longitudinal axis of the valve seat 82 ′ and function to provide an air-tight seal between the valve seat 82 ′ and the upper end 36 ′ of the main body 32 ′. Thus, no air flow occurs between the main body 32 ′ and the valve seat 82 ′ as in the previous embodiment.
[0058] To provide the air flow to the top of the valve body 82 ′ that acts on the piston 112 ′, the valve stem 122 ′ is formed with an internal passage 238 that extends from the end of the stem 122 ′ located within the piston 112 ′ along the center of the stem 122 ′ to a point spaced from the stem flange 124 ′ an generally in at least partial alignment with the air flow tubes 88 ′ in the lower end of the valve seat 82 ′. At this point, the passage 238 communicates with a bore 240 extending into the stem 122 ′ generally perpendicular to the passage 238 , which allows air flow from the tubes 88 ′ to pass through the bore 240 and into the passage 238 . The air then flows up through the passage 238 to the upper end of the stem 122 ′ into the space between the piston 112 ′ and the cap 70 ′ to provide the motive force on the piston 112 ′.
[0059] This air flow through the stem 122 ′ operates to move the piston 112 ′ against the bias of a spring 128 ′, as in the previous embodiment. However, the spring 128 has been moved from the central chamber 42 ′ in the lower end 34 ′ of the main body 32 ′. In this embodiment, the spring 128 ′ is disposed within the chamber 96 ′ of the valve seat 82 ′ between the lower end of the piston 112 ′ and the lower end 86 ′ of the valve seat 82 ′. The spring 128 ′ is positioned around the bushing 104 ′ and urges the piston 112 ′ towards the cap 70 ′. In this location, the spring 128 ′ is positioned within the valve 230 such that the spring 128 ′ can be removed with the other moving parts of the valve 230 disposed within the main body 32 ′ when the components are to be replaced. The removal of the spring 128 ′ from the lower end 34 ′ of the main body 32 ′ also allows for a greater amount of air flow through the lower end 34 ′, because the spring 128 ′ is no longer present to obstruct this air flow.
[0060] In this embodiment, the stem flange 124 ′ on the valve stem 122 ′ is also modified to include an upwardly extending peripheral tab 242 , as opposed to the simple circular flange 124 ′ in the previous embodiment. This tab 242 is pulled into positive sealing engagement with the lower side of the seal 94 ′ by the spring 128 ′, and provides a secure air-tight seal until actuation of the valve 230 .
[0061] Additionally, to address the problem of backpressure within the valve 30 ′, the upper end 36 ′ of the main body 32 ′ includes a bore 244 that is extends through the screw thread 54 ′ on the upper end 36 ′, but that is covered by the cap 70 ′ when the cap 70 ′ is engaged with the thread 54 ′. This bore 244 communicates with an aperture 246 formed in the upper end 86 ′ of the valve seat 82 ′ that communicates with the central chamber 96 ′ in the valve seat 82 ′ and functions as a vent to reduce any back pressure present within the valve 230 during operation, by allowing the pressurized air to escape the valve 230 through the clearance between the threads 54 ′ on the main body 32 ′ and 76 ′ on the cap 70 ′.
[0062] In addition to the description of the previous embodiments, the wheel assembly 1000 and valve 30 of the present invention can also be modified in various manners to provide added functionality to the assembly 1000 and valve 30 . For example, the upper end 36 of the main body 32 and the upper end 86 of the valve seat 82 can be chamfered to enable the components of the valve 30 to be assembled and disassembled more easily. Also, the various structural components of the valve 30 can be formed from any suitable fluid-impervious material, such as a metal or hard plastic, to reduce the overall weight of the valve 30 .
[0063] Various alternatives are contemplated as being within the scope of the following claims, particularly pointing out and distinctly claiming the subject matter regarded as the invention.
[0064] We hereby claim: | The present invention is a wheel assembly having a rim with a valve aperture extending therethrough that is designed to receive a valve having a simplified a construction that can be seated directly within a tire wheel assembly to minimize the number and type of components necessary for the valve. The valve includes a main body that is positionable in a sealed and recessed or embedded configuration within the aperture in the wheel rim in communication with the interior of the tire and with a pressurized air source that is used to inflate or deflate the tire. The main body encloses a valve mechanism that includes a components situated within the main body in a manner that enables the parts to be easily removed, cleaned and/or replaced if necessary without having to remove the entire valve assembly from the wheel. | 8 |
[0001] This application claims priority from a Provisional Application, Serial No. 60/475,062, filed May 30, 2003.
FIELD OF THE INVENTION
[0002] The present invention relates to blood pumping devices, and, more particularly, to ventricular assist devices.
BACKGROUND
[0003] A ventricular assist device (“VAD”) is used to help supplement the heart's pumping action both during and after certain kinds of surgery, in situations where a complete cardiopulmonary bypass (using a heart-lung machine) is neither needed nor advisable in light of the serious side effects associated therewith. Ventricular assist devices typically comprise a pair of cannulae or other tubing and some sort of pump operably connected to the cannulae. In use, the cannulae are attached to either the left side of the heart (a left ventricular assist device) or to the right side of the heart (a right ventricular assist device) “in parallel,” i.e., the pump supplements the heart's pumping action but does not completely bypass it, and the pump is activated. Alternatively, a pump may be directly implanted into the body.
[0004] Originally, ventricular assist devices were air powered, wherein fluctuating air pressure, provided by a simple mechanical air pump machine, was applied to a bladder-like sac. The bladder had input and output valves, so that blood would enter the bladder through the input valve when the pressure on the bladder was low, and exit the bladder through the output valve when the pressure on the bladder was high. Unfortunately, these pneumatic ventricular assist devices were complicated, and used expensive mechanical valves that were prone to failure, subject to “clogging,” and that caused blood trauma or damage because of hard, metal edges and the like.
[0005] To overcome these problems, other types of ventricular assist devices were developed, including axial flow pumps for temporary insertion directly into the heart, and centrifugal pumps. The former are based on the Archymides' Principle, where a rod with helical blades is rotated inside a tube to displace liquid. In use, a catheter-mounted, miniature axial flow pump is appropriately positioned inside the heart, and is caused to operate via some sort of external magnetic drive or other appropriate mechanism. With high enough RPM's, a significant amount of blood can be pumped. In the case of centrifugal pumps, blood is moved by the action of a rapidly rotating impeller (spinning cone or the like), which causes the blood to accelerate out an exit. Both of these categories of ventricular assist devices are generally reliable and implantable, but are very expensive, not particularly durable, and are not useful in situations where a patient needs a true pulsating blood supply. Specifically, axial and centrifugal pumps are typically left on in a continuous operation mode, where a steady stream of blood is supplied on a continuous basis, as opposed to the natural rhythm of the heart, which acts on a periodic, pulse-producing basis. In addition, such pumps are still largely in the developmental or trial phase.
[0006] Accordingly, a primary object of the present invention is to provide a pneumatic ventricular assist device that offers the advantages of pneumatic operation without the drawbacks associated with prior pneumatic devices.
SUMMARY
[0007] A pneumatic ventricular assist device (“VAD”) is for use in any circulatory support application including RVAD, LAVD, or BIVAD, trans-operative, short-term or long-term, tethered implantable or extracorporeal. The VAD comprises a soft-contoured (rounded, low-profile) pumping shell and a disposable pumping unit that includes a blood sac, two one-way valves, and two tubing connectors. The pumping unit is specially designed to allow continuous and fluid movement of blood and to limit blood-contacting surfaces, and is made of a supple and elastic material such as silicone. The components can be inexpensively and reliably manufactured by injection molding. Also, the design of the VAD, according to the present invention, facilitates priming, de-bubbling, and connection to the body.
[0008] For assembly, the pumping shell is opened (it includes two halves in a clam shell-like arrangement), the pumping unit is positioned inside, and the shell is closed. The interior of the shell is complementary in shape to the pumping unit: a pumping chamber portion holds the blood sac, and two pump inlets are shaped to securely hold the valves and tubing connectors. A disposable seal rests between the two clamshell halves for sealing the connection there between.
[0009] In use, the VAD is connected to a patient's heart by way of two cannulae connected to the tubing connectors (the cannulae are connected to the heart at appropriate locations according to standard surgical practices). Then, a pneumatic drive unit is attached to an air inlet in the pumping shell by way of an air line or the like. Subsequently, the drive unit is activated to cause the blood sac to move in and out, in a gentle pumping action, by way of controlled periodic air pressure introduced into the pumping shell through the air inlet.
BRIEF DESCRIPTION OF THE DRAWINGS
[0010] These and other features, aspects, and advantages of the present invention will become better understood with respect to the following description, appended claims, and accompanying drawings, in which:
[0011] [0011]FIG. 1 is a perspective exploded view of a universal pneumatic ventricular assist device according to the present invention;
[0012] [0012]FIG. 2 is a perspective exploded view of the ventricular assist device with an assembled disposable pump assembly;
[0013] [0013]FIG. 3 is a perspective, partially exploded view of the ventricular assist device in place against a lower half of a pumping shell portion of the ventricular assist device;
[0014] [0014]FIG. 4A is a elevation cross-sectional view of a valve portion of the ventricular assist device, taken along line 4 A- 4 A in FIG. 1;
[0015] [0015]FIG. 4B is a perspective cross-sectional view of the valve portion of the ventricular assist device shown in FIG. 4A;
[0016] [0016]FIG. 5A is a plan view of a disposable pump blood sac portion of the ventricular assist device;
[0017] [0017]FIG. 5B is a cross-sectional view of the disposable blood sac taken along line 5 B- 5 B in FIG. 5A;
[0018] [0018]FIGS. 6A-6C show various elevation views of how the ventricular assist device is placed and connected for use with a patient; and
[0019] [0019]FIG. 7 is a perspective view of two of the ventricular assist devices in use extracorporeally with a patient.
DETAILED DESCRIPTION
[0020] With reference to FIGS. 1-7, a ventricular assist device (VAD) 10 includes: a reusable pumping shell 12 having a first or upper “clamshell” half 14 and a second or lower clamshell half 16 removably attachable to the first half 14 ; a disposable seal 18 that fits between the two pumping shell halves 14 , 16 ; and a disposable pumping unit 20 that includes: a disposable blood sac 22 that fits in the pumping shell 12 ; two disposable, one-way injection-molded valves 24 , 26 attached to the blood sac 22 ; and two tubing connectors 28 , 30 attached to the valves. Although the valves 24 , 26 are identical, one valve 26 is positioned to act as an inlet valve, and the other valve 24 is positioned to act as an outlet valve (i.e., blood can only flow through the valves 24 , 26 as indicated by the arrows in FIG. 3).
[0021] For assembly, the disposable pumping unit 20 is placed against the lower pumping shell half 16 , the seal 18 is positioned in place, and the upper pumping shell half 14 is placed against and connected to the lower pumping shell half 16 (by way of screws or other fasteners). In use, the ventricular assist device 10 is appropriately connected to a patient's heart by way of a ventricular (or atrial) cannula 32 and an arterial cannula 34 respectively connected to the tubing connectors 28 , 30 . Then, a pneumatic drive unit 36 is operably attached to an air inlet 38 in the ventricular assist device 10 by a pneumatic line 40 or the like (see FIG. 7). Subsequently, the drive unit 36 is activated to cause a portion of the disposable blood sac 22 to move in and out, in a gentle pumping action, by way of controlled fluctuating air pressure introduced into the pumping shell 12 through the air inlet 38 .
[0022] The pumping shell 12 is either molded or machined from a hard material that may or may not be implantable in the human body, and may or may not be reusable. The pumping shell 12 comprises the two halves 14 , 16 (generally similar to one another), which mate together like a clamshell and together define a rounded pumping chamber 42 and two generally cylindrical pump inlets 44 , 46 into the pumping chamber. As best seen in FIGS. 2 and 3, the pump inlets 44 , 46 are provided with annular contours or shoulders 37 for holding the connectors 28 , 30 (i.e., each pump shell half includes a semi-annular shoulder which, when the two halves are connected, together define an annular shoulder). In addition, the lower shell half 16 includes the air inlet 38 , which is a small hole or channel extending from the outer surface of the shell through the shell wall to the pumping chamber 42 . The outer surfaces of the shell halves 14 , 16 are rounded, while the peripheral inner surfaces are flat so that the shell halves fit snugly against one another. The shape of the pumping shell is generally flat and softly contoured (i.e., rounded, ellipsoidal) so that it may be comfortably implanted.
[0023] As mentioned, the pumping shell pump inlets 44 , 46 are generally cylindrical and dimensioned to hold and support the entireties of the cylindrical valves 24 , 26 therein. As should be appreciated, having the valves enclosed within the confines of the complementary-shaped pump inlets maximizes support of the valves, thereby enhancing their performance and durability. It also reduces the likelihood of the valves becoming dislodged or loose during use.
[0024] The blood sac 22 , valves 24 , 26 , and cannulae 32 , 34 are specially designed to allow continuous and fluid motion of blood and to limit blood contacting surfaces. These components are made of a supple elastomer such as silicone that will stretch and deform to pressure gradients reducing the damage to blood cells. With reference to FIGS. 4A and 4B, the valves 24 , 26 are hinge-less and have valve leaflet portions 50 that are flexible and elastic, simulating the action of natural heart valves, and improving their reliability and durability. The valves are injection molded in four piece molds reducing the manufacturing cost compared to biological or mechanical valves. In use, blood can flow through the valves in one direction only, from the valve inlet 52 to the valve outlet 54 , i.e., in the direction of the arrows in the figures. Specifically, when the pressure is greater on the valve inlet side 52 , the valve leaflets 50 respectively flex upwards and downwards, allowing blood to pass. However, when the pressure is greater on the valve outlet side 54 , the leaflets are gently but forcibly compressed together, preventing blood from flowing back through the valve. Because the valves are each one-piece, are made from silicone (or another suitable material), and have rounded or contoured inner surfaces, they are very reliable, perform well, and minimize damage to blood. For example, as shown in FIG. 4B, note that the valve wall 53 leading up to the leaftlets 50 is rounded/sloped to minimize blood disturbance.
[0025] As indicated in FIG. 4A, the sac 22 and connectors 28 are configured to fit within the entrance and exit ends of the valves 24 , 26 and against interior, circumferential shoulders 55 provided in the valves. This produces a continuous surface between the various elements and eliminates any sharp lips or ridges in the blood flow path, reducing blood damage.
[0026] [0026]FIGS. 5A and 5B (in addition to FIGS. 1-3) show the pumping sac 22 . The pumping sac is bilaterally symmetric and includes circular/tubular inlets 70 , 72 connected to a main pumping chamber 73 . The pumping chamber 73 sports a gently rounded or circular profile, which has been found to maximize pumping effectiveness and to reduce blood trauma during the pumping action. More specifically, the pumping chamber 73 is generally shaped like a semi-flattened ellipsoid, i.e., flat, circular top and bottom walls 74 a , 74 b interconnected by a rounded sidewall 75 .
[0027] The blood sac, valves, and/or cannulae may be coated with lubricant, hydrophobic, antibacterial and/or antithrombotic coatings, including but not limited to PTFE coatings, heparin bonded coatings, fluorinated coatings, treclosan and silver compound coatings, and anti-calcification agent releasing coatings such as previously described to improve blood compatibility and non thrombogenicity.
[0028] The connectors 28 , 30 are made of a hard material (e.g., plastic, stainless steel, titanium), molded or machined, that will secure the connection between the valves 24 , 26 and the cannulae 32 , 34 . The tubing connectors 28 , 30 each include a cylindrical through-bore, a cylindrical fore-portion that fits into the valves 24 , 26 , an annular flange 76 which corresponds in shape to the pump inlet shoulders 37 , and a rear-portion dimensioned to accommodate a cannula. In use, when the pumping unit 20 is placed in the pumping shell 12 , the valves' annular flanges 76 lie against the pump inlet shoulders, securely holding the tubing connectors 28 , 30 in place and preventing their removal from the pumping shell.
[0029] The seal 18 is made of a soft elastomer like the pumping sac and valves, but will not be in contact with blood and is only used to insure an airtight fit of the pumping shell halves 14 , 16 . The disposable pumping unit 20 (blood sac, valves and connectors and seal) may be preassembled and coated as a single disposable part.
[0030] To ensure that the cannulae 32 , 34 remain securely connected to the connectors 28 , 30 , the inlet portions 44 , 46 of each pumping shell half are provided with protruding, semi-annular gripping ridges 60 (see FIG. 2). In use, when the pumping unit 20 is placed in the lower pumping shell half 16 , as shown in FIG. 3, the cannulae 32 , 34 contact the gripping ridges of the lower half 16 . Then, when the upper half 14 is placed against and connected to the lower half 16 , the gripping ridges 60 of both halves bite into and engage the cannulae, securing them in place.
[0031] The whole system has been designed to be used in a wide range of applications of circulatory support, by simply selecting the appropriate cannulae and accessories. Intended applications include short term trans-operative support (a few hours), acute and post-cardiotomy support (up to a couple of weeks), bridge to transplant (˜3-6 months), bridge to recovery (˜several years) and destination therapy (until death). The device is also designed to be used as either a right VAD (FIG. 6B), a left VAD (FIG. 6A), or for bi-ventricular use (FIG. 6C), and to be used as a tethered implant(s), paracorporealy, or extracorporealy (FIG. 7).
[0032] To install the system, first the cannulae are sewn to the atrium, ventricle or outflowing artery of the compromised side of the heart, as applicable. The cannulae are then connected to the disposable pumping unit 20 , while carefully removing any air bubbles in the system. The blood sac assembly is supple and flexible, facilitating its priming and de-bubbling. The connectors 28 , 30 are also made to be easily connected and disconnected, facilitating this procedure. Once the system has been properly purged and connected, the pumping shell 12 is locked closed over the pumping unit. The blood sac assembly is symmetrical so that it can be placed either with the inflow valve on the left or on the right, making its design more adaptable to different applications. The connectors fit inside the pumping shell so that when the latter is closed it will crimp down on the cannulae connections preventing an accidental disconnection, as mentioned above. The device can then be placed in the abdomen or outside the body and the drive unit can be activated to start pumping.
[0033] Although the ventricular assist device of the present invention has been illustrated as having a pumping shell with two separate halves 14 , 16 , the halves could be hinged together or otherwise permanently connected without departing from the spirit and scope of the invention. Also, although the pumping unit has been described as comprising separate components connected together, the pumping unit could be provided as a single unit, i.e., a unitary piece of molded silicone. This also applies to the valves 24 , 26 and connectors 28 , 30 , i.e., the connectors could be provided as part of the valves.
[0034] Although the valves 24 , 26 have been characterized as being identical and each having two leaflets, it should be appreciated that the valves 24 , 26 could have a different number of leaflets, e.g., 1 leaflet, or 3 leaflets, and the two valves 24 , 26 could be different from one another. More specifically, where operating pressures on the two valves may be different (because one is acting as an inlet valve and the other acting as an outlet valve), it may be advantageous to utilize valves with different characteristics.
[0035] Since certain changes may be made in the above-described universal pneumatic ventricular assist device, without departing from the spirit and scope of the invention herein involved, it is intended that all of the subject matter of the above description or shown in the accompanying drawings shall be interpreted merely as examples illustrating the inventive concept herein and shall not be construed as limiting the invention. | A pneumatic ventricular assist device is designed for use in any circulatory support application including RVAD, LAVD, or BIVAD, trans-operative, short-term or long-term, tethered implantable or extracorporeal. It consists of a soft contoured pumping shell and a disposable pumping unit, which includes a pump sac, two one-way valves, and tubing connectors. The pumping unit is specially designed to allow continuous and fluid movement of blood and to limit blood-contacting surfaces, and is made of a supple and elastic material such as silicone. The components can be inexpensively and reliably manufactured by injection molding. Also, the pumping shell and pumping unit include complementary features that quickly and securely hold the pumping unit, and any attached cannulae, in place. | 0 |
BACKGROUND OF THE INVENTION
1. Technical Field
The invention relates to the field of double locking snap hook designs and provides an anchoring device for retaining safety harnesses, load supports, lanyards and the like.
2. Background Information
The double locking snap hook generally consists of a hook portion and an eye to which a rope may be secured. The hook portion includes a latch which is spring loaded, biasing the latch into a closed, latched position. Further, a locking means, also spring loaded, is provided to help prevent the latch from inadvertently becoming opened, thus maximizing the safety factor of the hook. In recent years, several new designs for double locking snap hooks have been introduced. The safety and effectiveness of any snap hook of this variety is directly related to the ease of use and simplicity of operation of the snap hook. Unfortunately, many of these designs are either clumsy to use or too easily unlocked and unlatched. Similarly, some of these designs are not adequately durable, and components of the locking mechanism sometimes break or wear off, rendering the snap hook useless.
Among the more relevant prior art patents are U.S. Pat. Nos. 4,434,536 issued to Schmidt et al. on Mar. 6, 1984, 4,528,728 issued to Schmidt et al. on July 16, 1985, 4,528,729 issued to Schmidt et al. on July 16, 1985, and 4,539,732 issued to Wolner on Sept. 10, 1985. In their commercial embodiments, the locking snap hooks made according to the '536 reference and relevant embodiments of the '728 reference are difficult to use because the locking member is difficult to access, especially by a worker wearing gloves. The safety snap of the '732 reference, while effective and simple to use, is relatively complicated in design, and requires the use of several parts, increasing the likelihood of the hook becoming broken or otherwise disabled due to dirty conditions or heavy wear.
The present invention is directed to solving these problems and provides a workable and economical solution to them.
SUMMARY OF THE INVENTION
As noted in the '732 reference, a double lock snap hook device allows a belt connection, such as a fall protection device, window washer's harness, or the like, to be retained within the double lock snap system. The double lock snap system includes a shank which has a return portion at one end which defines a hook, and a nose spaced from the shank which defines a hook throat. An eyelet is located at the other end of the shank which provides a means for attaching a load support member, such as a lanyard or the like. The double lock snap system further includes a latch member having one end pivotally mounted on the shank and the other end engageable with the hook nose to close the hook throat. The latch member is displaceable between a closed position, wherein the belt connection is retained within the hook by the latch member engaging the hook nose, and an open position, wherein the belt connection may be removed from within the hook throat. A latch member spring aids the latch member in moving between its open and closed positions, biasing the latch member toward the closed, latched position.
An object of the invention is to provide a double lock snap hook which will securely hold that to which it has been attached. When in use, the double locking snap hook latch member is retained in its closed position by a lock member. The lock member also pivots between a first position and a second position, maintaining the latch member in its closed position when the lock member is located in its first position. The lock member also includes a spring which biases the lock member toward the first position.
The lock member is controlled by the user, who displaces the lock member by means of the finger pad found thereon. The finger pad of the lock member is easily distinguised from the latch member by the user because of a finger positioning member protruding from the shank between the lock member and the latch member. An object of the invention is thus to provide a double lock snap hook which is easily operable by the user. A further object of the finger positioning member of the invention is to preclude a semi rigid rod from inadvertently simultaneously opening both the lock member and the latch member.
Other objects and advantages of the invention will become apparent from the following detailed description and from the appended drawings in which like numbers have been used to describe like parts of the several views.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a perspective view of the instant invention illustrating the latch member in its first, latched position and the lock member in its first position.
FIG. 2 is a side elevation view of the instant invention, partially in section, illustrating the lock member in its second position.
FIG. 3 is a side elevation view of the instant invention, partially in section, illustrating the lock member in its second position and the latch member in its second, open position.
FIG. 4 is a side elevation view illustrating the lock member in an intermediate position, having been released by the user, with the latch member in its second, open position.
FIG. 5 is a sectional view taken along line 5--5 of FIG. 1.
DESCRIPTION OF THE PREFERRED EMBODIMENT
With reference to the drawings, and in particular to FIG. 1, the double locking snap hook of the present invention is generally indicated by reference numeral 10. The spring biased latch member 12 and spring biased lock member 14 are both pivotally attached to shank 16.
The shank 16 has a first end 18 and a second end 20. The first end 18 includes a return portion 22 defining a hook, the return portion 22 including a nose 24 spaced from the shank 16 to define a hook throat 26 (FIG. 3). The second end 20 of shank 16 includes a means, such as an eyelet or O-ring 28, for attaining a load support member such as a safety harness, lanyard or the like.
The spring biased latch member 12 includes a bifurcated latch body 30 with opposed side walls which straddle hook shank 16. A biasing spring means such as first spring 32 is contained within latch body 30 for urging latch member 12 into a first, latched position, shown if FIGS. 1 and 2. As shown in FIG. 5, shank 16 is provided with a spring retaining means such as a peg 33 for helping maintain spring 32 in the correct relative position. Latch member 12 further includes a first end 34, pivotally mounted on shank 16 by pivot means such as latch member pin 36, and a second end 38 engageable with hook nose 24 to close hook throat 26. The latch member 12 is movable between the first, latched position, as indicated in FIGS. 1, 2 and 5, and a second, open position, as indicated in FIGS. 3 and 4. When latch member 12 is in its first, latched position, end surface 35 spans hook throat 26, thus closing off the hook defined by shank return portion 22. A thumb actuation means 39, preferably in the form of a knurled pad, is mounted to or otherwise integral with rearwardly extending arms 29 and 31 of latch member 12. Thumb activation means 39 is mounted on the rear side of shank 16 so as to have the shank 16 intermediate thumb activation means 39 and the first and second ends 34, 38, respectively, of latch member 12.
The spring biased locking means 14 is also a bifurcated member comprised of a lock body 42 and legs, 41, 43 extending downwardly and rearwardly therefrom when snap hook 10 is oriented as shown in the accompanying drawings, in straddling relation to hook shank 16. Locking member 14 is pivotally attached to shank 16 by pivot means such as pin 40 extending through the lower end of legs 41, 43. Locking member 14 is attached adjacent hook throat 26 of return portion or hook 22 opposite nose 24, as best illustrated in FIGS. 3 and 5. Legs 41, 43 and lock body 42 of locking means 14 are at least partially received within latch member 12, with legs 41, 43 passing through and extending beyond latch member 12. Locking means 14 releasably locks latch member 12 into its first, latched position, as most clearly indicated in FIG. 1. Locking means 14 includes a spring means such as second spring 44 positioned within lock body 42 for urging locking member 14 into the locking position of FIG. 1 when latch member 12 is located in its first, latched position. Lock member 14 is activated by the user by pressing finger pad 48 in a direction opposing second spring 44, thus displacing the lock member 14 to the position shown in FIG. 2. In the preferred embodiment, spring 44 is retained within locking means 14 between shank 16 and finger pad 48 as illustrated in FIG. 5. In its preferred embodiment, lock body 42 includes two locking ear projections 46, one of which is located on each side of snap hook 10. Ear projections 46 extend laterally outwardly from lock body 42 on opposite sides of shank 16 and engage the top edges of first, upper end 34 of latch member 12 to maintain it in its first, latched position.
As oriented in the accompanying drawings, shank 16 includes a forwardly protruding finger positioning segment or nub 50 projecting therefrom in the plane of the shank 16. Finger positioning segment 50 is positioned adjacent the first end 34 of latch member 12 under lock member 14, opposing nose 24 of return portion 22. The front surface 35 of latch member 12 terminates below the upper edges of its first end 34 in order to provide an opening through which segment 50 extends.
In use, the double locking snap hook 10 may be grapsed in the palm of the user's hand with thumb activations means 39 positioned near the user's thumb. In order to either remove an item already fastened to the snap hook or fasten an item to the snap hook, the user must first displace lock member 14. This may be accomplished by pressing against finger pad surface 48, thus compressing second spring 44, as shown in FIG. 2. The finger pad surface may be easily located by the user by first finding the protruding finger positioning piece 50, which acts as a guide or reference point. The user may then move his or her finger to the appropriate position on the finger pad 48 without fear of inadvertently getting his or her finger caught in the latch member 12. After displacing lock member 14, the user displaces latch member 12 by forcing thumb activation means 39 to the position shown in FIG. 3, compressing first spring 32. Lock member 14 may then be released by removing the finger from the finger pad 48, leaving the various components of snap hook 10 as shown in FIG. 4. The item to be removed from or attached to the snap hook 10 may then be passed through hook throat 26, and thumb activation means 39 may be released.
While the preferred embodiments of the invention have been described, it should be understood that various changes, adaptations, and modifications may be made therein without departing from the spirit of the invention and the scope of the appended claims. | A double locking snap hook comprising a shank, a spring biased latch member and a spring biased locking means, the latch member and locking means being biased by two separate screens. One end of the shank defines a hook portion, and the latch member is biased toward a latched position for restraining straps, ropes, etc. within the hook portion. The locking means is biased toward a position which requires that the locking means be deactivated before the latch member may be unlatched or opened. | 8 |
[0001] This application claims priority to and is a divisional application of U.S. Non-provisional application Ser. No. 10/482,244 filed Aug. 11, 2004, which is a US National Stage Application under 35 U.S.C. §371 claiming priority to PCT/US2002/20599 filed Jun. 28, 2002, which claims priority to U.S. Provisional Application No. 60/302,607 filed on Jul. 2, 2001.
INTRODUCTION
[0002] The present invention relates to preimplantation factor (“PIF”) a very early marker of fertilization and embryo viability, to new methods for detecting PIF activity and to PIF peptides.
BACKGROUND OF THE INVENTION
[0003] Infertility is a major health care concern affecting millions of couples worldwide. Contributing to this problem, early demise of the human conceptus is a common event. Approximately 73% of natural single conceptions are lost before reaching week 6 of gestation (Boklage C E. Survival probability of human conceptions from fertilization to term. Int J Fertil 1990; 35:75). This is mostly due to early embryonic demise prior to implantation or soon after implantation occurs. Data relating to the low fertility rate observed in older women and its improvement by oocyte donation from young women indicate that oocyte quality is an important factor in achieving a successful pregnancy (Navot D, Bergh P A, Williams M A et al. Poor oocyte quality rather than implantation failure as a cause of age-related decline female fertility. Lancet 1991; 337:1375).
[0004] In vitro fertilization (“IVF”) is a technology which has been developed to address the problem of infertility. However, maintaining embryo viability is even more problematic under the artificial conditions used for culturing embryos in vitro for implantation. In vitro, the embryo development rate is lower than in vivo and only 25-65% of embryos typically develop to the blastocyst stage (Gardner D K, Lane M, KOuridakis K, Schoolvcraft W B. Complex physiologically based serum-free culture media increase mammalian embryo development. In:Gomel V, Leung P C K, eds. In vitro fertilization and assisted reproduction. Procc 10th World Congress, 1997:187). The state of the art is not yet able to identifying embryos likely to implant and survive. Human chorionic gonadotrophin (“hCG”), the currently used marker for fertilization in vivo and early embryo implantation, can only be detected several days after implantation. As a result of the lack of a suitable marker for embryo viability, nowadays many embryos incapable of implanting are being transferred, thus lowering the chance for achieving successful pregnancy.
[0005] To address the possibility that embryos may not be viable, a greater number of embryos are simultaneously transferred into a potential mother. The transfer of a high number of embryos may lead to multiple pregnancies, which are inherently risky, while transfer of a small number of embryos carries the risk that none would implant, losing a whole IVF cycle. Clearly, there is a need to improve embryo selection and define accurate markers to determine embryo viability. In addition, using non-invasive methods by testing culture media for products specific to viable, implantation-competent embryos would allow selection of those most likely to result in successful pregnancies, without causing embryo damage.
[0006] Another factor involved in determining whether a pregnancy is successful or not is the interaction between the conceptus and the mother's immune system. Shortly after fertilization a systemic maternal recognition of pregnancy should occur. The mother's immune system modulation triggered by specific early embryo signals could be the key of this process. Once the oocyte is fertilized, the zygote up to hatching blastocyst is surrounded by the zona pellucida, a hard semi permeable membrane. Therefore the embryo-maternal communication must occur simultaneously while the embryo is developing in the oviduct and uterine cavity through compounds that are secreted by the embryo.
[0007] It has been shown that pregnant sera and viable embryo conditioned culture media can produce an increase in rosette formation by platelets and T lymphocytes in the presence of CD2 antibody. As disclosed in U.S. Pat. No. 5,646,003 by Barnea et al., issued Jul. 8, 1997, and in U.S. Pat. No. 5,981,198 by Bamea et al., granted Nov. 9, 1999, the presence of Preimplantation Factor (“PIF”) can be detected by mixing lymphocytes, platelets, heat inactivated serum from a pregnant subject, guinea pig complement, and T11 (anti-CD2) monoclonal antibody (Dakko, Denmark), where rosette formation between platelets and lymphocytes is increased by PIF in pregnant subjects. PIF has been found to be (i) secreted by viable early human and mouse embryos from the two-cell stage onward; detectable in the peripheral circulation 34 days after embryo transfer following IVF; (iii) associated with 73% take home babies vs 3% in early negative PIF results; (iv) detectable 5-6 days after intrauterine insemination; (v) absent in non-pregnant serum, or non-viable embryos; and (vi) present in various pregnant mammals in addition to humans, including mice, horses, cows and pigs. In addition, PIF has been observed to disappear from the circulation two weeks before hCG secretion declines in cases of spontaneous abortion.
[0008] The monoclonal antibody used in the above-mentioned PIF assay is directed toward the lymphocyte associated antigen referred to as CD2. CD2 is present on about 80-90% of human peripheral blood lymphocytes, greater than 95% of thymocytes, all T lymphocytes that form erythrocyte rosettes and a subset of NK cells. Various roles for CD2 in T cell activation have been proposed, including function as an adhesion molecule which reduces the amount of antigen required for T cell activation and as a costimulatory molecule or direct promoter of T cell activation. Moreover, CD2 has been implicated in the induction of anergy, the modulation of cytokine production and the regulation of positive selection of T-cells.
[0009] The natural ligand for CD2 is the structurally related IgSF CAMs CD58 (LFA-3), a cell-surface adhesive ligand with broad tissue distribution. In addition, CD2 can interact with CD48, CD59 and CD15 (Lewis x)-associated carbohydrate structure. CD2 binds CD58 with very low affinity and an extremely fast dissociation constant. The lateral redistribution of CD2 and its ligand CD58 also affect cellular adhesion strength. Regulation of CD2 adhesiveness affects the ability of CD2 to enhance antigen responsiveness. CD2-cell lines incapable of avidity regulation exhibit a marked deficiency in an antigen-specific response. Strength of adhesion resulting from increased CD2 avidity contributes directly to T-cell responsiveness independently of CD2-mediated signal transduction.
SUMMARY OF THE INVENTION
[0010] The present invention relates to assay methods used for detecting the presence of PIF, and to PIF peptides identified using this assay. In particular, the present invention relates to flow cytometry assays for detecting PIF. It is based, at least in part, on the observation that flow cytometry using fluorescently labeled anti-lymphocyte and anti-platelet antibodies demonstrated an increase in rosette formation in the presence of PIF. It is further based on the observation that flow cytometry demonstrated that monoclonal antibody binding to CD2 decreased in the presence of PIF.
[0011] The present invention further relates to PTF peptides which, when added to Jurkat cell cultures, have been observed to either (i) decrease binding of anti-CD2 antibody to Jurkat cells; (ii) increase expression of CD2 in Jurkat cells; or (iii) decrease Jurkat cell viability. In additional embodiments, the present invention provides for ELISA assays which detect PIF by determining the effect of a test sample on the binding of anti-CD2 antibody to a CD2 substrate.
BRIEF DESCRIPTION OF THE DRAWINGS
[0012] FIG. 1A-B . PIF purification from mouse embryo culture conditioned medium (MECCM); (A) shows a high performance liquid chromatography (“HPLC”) profile of MECCM-3 kDA ultra-filtrate previously purified by MabCD2 affinity chromatography; (B) shows the profile following additional HPLC purification of a PIF-active fraction from (A).
[0013] FIG. 2A-C . Western blot analysis of different PIF peptides purified from MECCM; MabCD2 was used as a primary antibody and anti-sense mouse horseradish peroxidase (HRP)-biotin streptavidin complex was used as secondary antibody. Specific PIF bands were identified by the ECL detection reagents (Amersham Pharmacia Biotech).
[0014] FIG. 3A-B . (A) shows flow cytometric determination of lymphocyte-platelet rosette formation (L-P) in the presence of fresh culture medium (CM) and mouse embryo culture conditioned medium (MECCM) and MabCD2. Fluorescent labeled specific antibodies to L (MabCD45-PE) and to P (MabCD42a-FITC) were used to detect the L-P complex. MECCM gave 30-40 percent higher formation of L-P compared to culture medium (CM). (B) shows FC of MECCM effect on MabCD2 binding to Jurkat cells (JC). JC were incubated with samples and further with MabCD2 Cy 5 . Antibody binding to CD2 decreased by PIEF present in MECCM. Arrows indicate PIF activity.
[0015] FIG. 4A-C . Mass spectrum from PIEF peptides purified from MECCM. Molecular weight (MW) of PIF-active fractions from MECCM purified by ultrafiltration, diafiltration, HPLC, MabCD2-affinity chromatography and by additional HPLC was determined by mass spectroscopy. MW of PIF peptides were A) 610-995 Da; B) 963-1848 Da; and C) 1807-1846 Da.
[0016] FIG. 5A-F . Flow cytometric analysis of PIF negative effects on MabCD2 binding (A), fluorescence (B) and viability (C) in Jurkat cells, and of PIF positive effects on MabCD2 binding (D), fluorescence (E) and viability (F). PIF in positive samples competes with CD2 (arrows indicate PIF activity).
[0017] FIG. 6 . Effect of Synthetic PIF peptides on CD2 expression on Jurkat cells.
DETAILED DESCRIPTION OF THE INVENTION
[0018] In a first set of embodiments, the present invention provides for a method for determining the presence of preimplantation factor in a sample, comprising the step of detecting whether the sample contains a component which inhibits the binding of an anti-CD2 antibody to CD2 antigen; wherein the ability to inhibit the binding of anti-CD2 antibody to CD2 has a positive correlation with the presence of preimplantation factor.
[0019] Such a method may, for example, be employed in a flow cytometry method or in an enzyme-linked immunosorbent assay method, using techniques otherwise known in the art. A non-limiting example of a flow cytometry method for detecting anti-CD2 antibody binding to CD2 is presented in Section 7, below. An anti-CD2 antibody, as that term is used herein, may be a monoclonal or polyclonal antibody which specifically binds to CD2. Such a monoclonal antibody is sold by Pharmigen (see below).
[0020] CD2 antigen may be in the form of purified CD2 antigen or may be carried by a cell. In non-limiting embodiments of the invention, the cell is a Jurkat cell. Other CD2-expressing cell lines are known in the art.
[0021] The sample may be a serum sample (for example, serum from a subject to be tested for fertilization/implantation/persistence of embryo), may be a sample of culture fluid (for example, to determine the viability of embryos prior to transfer for IVF), or may be a solution to be tested for the presence of a PIF peptide (for example, during the purification of PIF acting agents; see Section 6, below).
[0022] The subject may be a human subject (for example, a human suspected of being pregnant) or a non-human subject (for example an agricultural animal or a zoo animal).
[0023] In a second set of embodiments the present invention provides for a method for determining the presence of preimplantation factor in a sample, comprising the step of detecting, by flow cytometry, whether the sample contains a component which increases the formation of rosettes between lymphocytes, platelets, and anti-CD2 antibodies, where an increase in rosette formation has a positive correlation with the presence of preimplantation factor. Such an assay may be performed, for example, using fluorescently labeled antibodies directed toward lymphocytes and platelets, where preferably different labels are used for anti-platelet and anti-lymphocyte antibodies.
[0024] The increase is relative to a known negative control.
[0025] The present invention also provides for the following isolated peptides:
[0026] (1) An isolated peptide having a sequence selected from the group consisting of: Met-Val-Arg-Ile-Lys-Pro-Gly-Ser-Ala; Met-Val-Arg-Ile-Lys-Pro-Gly-Ser-Ala-Asn-Lys-Phe-Ser; Met-Val-Arg-Ile-Lys-Pro-Gly-Ser-Ala-Asn-Lys-Phe-Ser-Asp; and Met-Val-Arg-Ile-Lys-Pro-Gly-Ser-Ala-Asn-Lys-Phe-Ser-Asp-Asp, or an isolated peptide comprising said peptide which binds to anti-CD2 antibody and which is not a circumsporooite protein;
[0027] (2) An isolated peptide having a sequence Ser-Gly-Ile-Val-Ile-Tyr-Gln-Tyr-Met-Asp-Asp-Arg-Tyr-Val-Gly-Ser-Asp-Leu, or an isolated peptide comprising said peptide which binds to anti-CD2 antibody and which is not an HIV protein;
[0028] (3) An isolated peptide having a sequence Val-Ile-Ile-Ile-Ala-Gln-Tyr-Met-Asp or an isolated peptide comprising said peptide which binds to anti-CD2 antibody; and
[0029] (4) An isolated peptide having a sequence selected from the group consisting of Ser-Gln-Ala-Val-Gln-Glu-His-Ala-Ser-Thr and Ser-Gln-Ala-Val-Gln-Glu-His-Ala-Ser-Thr-Asn-Xaa-Gly, where Xaa can be any amino acid, or an isolated peptide comprising said peptide which binds to anti-CD2 antibody and which is not a silencing mediator for human retinoid and thyroid hormone.
EXAMPLE
Identification of PIF Peptides
[0030] PIF was isolated from a large volume of MECCM using ultra filtration, lyophilization, high performance chromatography (HPLC), affinity chromatography and western blot. Two-cell-to blastocyst stage mouse embryos were cultured for several days in Ham's F-10 medium with penicillin, streptomycin, MgSO 4 , NaHCO 3 , KHCO 3 , and Ca lactate supplemented with 0.1% BSA. MECCM collected was stored at −80° C. until used.
[0031] One liter of MECCM was purified by ultra filtration through an Amicon membrane (3 kDa cut-off; YM-3 kDa, Amicon. Millipore Co, USA). Concentrated MECCM was further diafiltered using 300 ml of pure water. In addition, fresh culture media (CM, without embryos) was processed in the same way. Only MECCM-3 kDa ultra filtrate and diafiltrated demonstrated PIF activity and then they were pooled and concentrated by lyophilization.
[0032] It was observed that PIF is able to bind to anti-CD2 monoclonal antibody (“MabCD2”). Therefore, PIF-active fractions were purified first by affinity chromatography performed with agarose-hydrazide-MabCD2 activated gels. An antibody affinity matrix was prepared as follows. 1.5 mg of MabCD2 (clone RPA-2.10, Pharmigen, Becton Dickinson) was buffer exchanged with the coupling buffer pH 5.5 using the Econo-Pac IODG desalting column provided and further oxidized with sodium periodate and coupled to 2 ml of agarose-hydrazide activated gel following the manufacturer's indications (Affi-gel Hidrazide immunoaffinity kit, BioRad Laboratories, CA, USA). Then, MECCM-3 kDa ultra filtrate-diafiltrate lyophilized powder was further purified using the MabCD2-affinity chromatography column (10×20 mm). 2 g of MECCM-3 kDa powder were dissolved in 10 ml of pure water, pH neutralized, filter-out through a 0.22 m syringe sterile filter (Corning Inc., NY, USA) and passed 5 times through the affinity chromatography column at gravity flow. The column was washed-out with 5 volume bed of 100 mM phosphate saline buffer, pH 7.2, followed by washing with 5 volume bed of 0.5 M NaCl.
[0033] The bound PIF was eluted with 3 ml of 0.1 M acetic acid. PIF-eluted fractions were pooled, assayed for PIF activity and concentrated by lyophilization.
[0034] A total of 300 mg of MECCM-3 kDa ultra filtrate further purified by affinity chromatography were run in three batches by HPLC on a Clipeus C18 preparative column (Higgins Analytical, Inc., USA). Preparative HPLC running parameters were: flow, 15 ml/min. Buffers: A=0.1% trifluoroacetic acid (TFA); B=0.1% TFA in 99.9% acetonitrile (CH 3 CN). Gradient: 0% B, during 5 min plus 0-60% B for 30 min and 0-100% B for 3 min.
[0035] Fractions from HPLC were further concentrated by evaporation. HPLC concentrated fractions were pH neutralized and re-assayed for PIF-activity. Several fractions showed high PIF-activity (see FIG. 1A ). These fractions were purified by additional HPLC on a Vydac C8 analytical column (4.6×250 mm; Hesperia, Calif., USA). Additional HPLC running parameters: flow, 1 ml/min. Buffers: A=0.1% trifluoroacetic acid (TFA); B=0.1% TFA in 99.9% acetonitrile (CH 3 CN). Gradient: 0% B, during 5 min plus 0-60% B for 30 min and 0-100% B for 3 min. Several eluted fractions showed PIF activity (see FIG. 1B ) and were further sequenced for amino acid composition and their molecular weight (MW) was determined by mass-spectrometry.
[0036] PIF active fractions purified from MECCM gave positive signals in Western blots (“WB”). Solutions from CM ultra filtrate-lyophilize fraction was used as negative control in WB. The WB conditions were as follows. For gels, SDS-PAGE pre-casting gels (BioRad) were used, having a 16.5% agarose resolving gel and a 4% agarose stacking gel. The gels were run in 100 mM Tris, 100 mM Tricine, 0.1% SDS, pH 8.3 (Tris-tricine running buffer). Samples consisting of 30 microliters of PIF-MECCM purified fractions plus 10 microliters of Tricine sample buffer [200 mM Tris (hydroxymethyl) aminomethane (Tris-HCl) pH 6.8, 2% sodium duodecyl sulphate (SDS), 40% glycerol, 0.04% Coomassie blue brilliant (CBB-G250)] (BioRad) were incubated at 95° C. during 5 min. After cooling, the samples were loaded into the wells of the SDS-polyacrylamide gels (PAGE). To determine the molecular weight of low molecular weight (MW) polypeptides, 10 microliters of a 1:20 water dilution of SDS-PAGE standards (BioRad) were loaded into a well of each gel. For electrophoresis, samples and standards were run at 175 v during 5 min plus 60 v for 1 h.
[0037] The resulting gels were then electro-blotted using, as transfer buffer, 100 mM CAPS [3-(cyclohexylamino)-1-propanesulfonic acid) buffer, pH 11. Electro-blotting was performed at 80 mA during 1 h onto a 0.22 μm nitrocellulose membrane (BioRad).
[0038] Then, nitrocellulose membranes were blocked with 5% blocking solutions (Amersham, Pharmacia, Biotech, N.J., USA) at room temperature during 18 h., and then were washed-out 4 times during 20 min with PBS-T [phosphate saline buffe−0.05% polyoxyethylenesorbitan monolaurate (Tween 20)]. For the primary antibody incubation, blocked membranes were incubated with 2 μg/ml MabCD2 (Pharmigen)-PBS-T solutions at room temperature during 2 h, and then washed as above. For the secondary antibody incubation, the membranes were incubated with anti mouse IgG-horse radish peroxidase conjugate (1:1000 in PBS-T) solution at room temperature during 1 h. PIF bands were then visualized using the ECL-chemiluminescent system (Amersham). FIG. 2 shows a typical WB of PIF peptides purified from MECCM.
[0039] A flow cytometric methodology (FC) for measuring PIF was developed to improve the efficiency and reproducibility of methods set forth in U.S. Pat. Nos. 5,646,003 and 5,981,198. In particular, rosette formation was evaluated by FC with pregnant and non-pregnant human and porcine serum, MECCM, CM and isolated PIF-fractions using MabCD2 or MabCD2-Cy5 (Cy-chrome conjugated antibody), MabCD45-PE (phycoerytrhin conjugated antibody) and MabCD41a-FITC (fluorescein isothiocyanate conjugated antibody), all antibodies were from Pharmigen. The ratio of labeled P-L complex was higher by 30-40% with MECCM versus CM ( FIG. 3A ). Further, it was found that pre-incubation of MECCM or pregnant sera with immobilized MabCD2 prevented the P-L formation in the assay. The addition of a MabCD58 (lymphocyte function-associate antigen-3 or LFA-3) antibody to L-P did not prevent totally the rosette formation by effect of PIF-active samples in the assay.
[0000] A FC-PIF quantitative assay using Jurkat cells (JC) and MabCD2-Cy5 was developed ( FIG. 3B ). The use of an immortalized leukemia cell line avoids the need for fresh donor blood to assess the PIF activity by the bioassay. The JC-FC assay was validated with human serum samples (see Table I) and was used to assess PIF activity of fractions during PIF purification.
[0040] MW of purified PIF-active fractions was determined by mass spectral analysis on a Voyager-RP Biospectrometry MALDI-TOF Workstation from Perseptive Biosystems (Cambrigde, Mass., USA). Samples were mixed with a matrix consisting in a 1:2 mixture of acetonitrile:water containing 1% trifluoroacetic acid. Spectra were averages of approximately 200 scans. PIF— peptides from MECCM have MW between 610-1845 Da ( FIG. 4 ).
[0041] Further, it was assessed that pre-incubation of PIF-active fractions with MabCD2 abolished the PIF-activity. These data indicated that PIF could be a portion of CD2 or homologue peptides. However, after the sequencing of purified PIF peptides it was demonstrated that these peptides are not a portion of CD2 and their amino acid sequences are unique.
[0042] Using the JC-FC assay it was demonstrated that MEECM-PIF peptides have three different effects on CD2 expressed by T cells. These effects are related to: decreasing MabCD2 binding to the JC; up-regulating CD2 expression by JC; or decreasing JC viability.
[0043] Purified PIF active fractions from mouse embryos were sequenced by Edman degradation on an Applied Biosystems Pulsed Liquid Sequencer (model 477A). Released amino acids were derivatized with phenylisothiocyanate to give the PTH-amino acids which were detected by reverse phase-HPLC on a HPLC system in line with the sequencer. Several of the PIF fractions yielded unique sequences.
[0044] Several peptides gave sequences whose N-terminal nine and ten residues were identical indicating that the peptides were various truncated forms of common molecules (see Table II). PIF peptides were identified as a least three unique families of embryo-derived and pregnancy-related small peptides. The amino acid sequence sequence of a family of three PIF peptides matches 100% with a region of Circumsporozoite protein (malaria parasite: Plasmodium falciparum ). This family of PIF peptides up regulates the CD2 expression by JC. A PIF peptide (14 amino acids) that shares only the five first amino acid residues with the former described PIF-peptide's family and another PIF peptide (18 amino acids) that matches in 11 amino acids to the sequence of HIV-1 RNA directed DNA polymerase (reverse transcriptase, EC 2.7.7.49) also up regulate the CD2 expression by JC. In addition, another family of two PIF peptides (9 and 13 amino acids) matches in 10 amino acids with the sequence of the human receptor-interacting factor, a silencing mediator for retinoid and thyroid hormone receptor (SMRT) (Chen and Evans, 1995). The shorter member of this PIF-peptide family shows a competitive effect for the binding of MabCD2 to JC and the longer PIF-peptide decrease the viability of JC. It is worth to notice that transcriptional silencing mediated by nuclear receptors is important in development, differentiation and oncogenesis.
[0045] PIF peptides were synthesized by solid-phase peptide synthesis (SPPS) on an Applied Biosystems Peptide Synthesizer employing Fmoc (9-fluorenylmethoxycarbonyl) chemistry in which the amino nitrogen of each amino acid is blocked with Fmoc. Coupling was performed by activation of the carboxyl groups of the N-protected amino acids using 3 mol/ml of 2-(1H-benzotriazol-1-yl)-1,1,3,3-tetramethyluronium tetrafluoroborate/1-hydroxybenzotriazole on the presence of diisopropylethylamine. Activated amino acids were sequentially added to the nascent peptide. Upon completion of the synthesis, final purification was carried out by reversed-phase HPLC and identity was verified by MALDI-TOF mass spectrometry and amino acid analysis. PIF synthetic peptides demonstrated to have similar effect on CD2 phenomenon in Jurkat cells ( FIG. 6 ), and were also immunodetected by the Mab CD2.
Flow Cytometry Assay for PIF Materials
[0046] Materials included Jurkat leukemia cells (JC); cloning medium; Falcon tubes for flow cytometry measurements; Mab CD2-Cy5 (Cy-chrome conjugated antibody, clone RPA-2.10, Pharmigen, Becton Dickinson); the biological sample (which could be a human serum to be assayed for PIF activity, or could be a solution of a putative or synthetic PIF peptide); PBS-2% BSA (100 mM phosphate saline buffer-2% bovine serum albumin; a negative control); trypan-blue dye; a CO 2 -incubator for cell culture; and a flow cytometer.
Method
[0047] To prepare the JC suspension:
[0048] Check the viability of the JC culture using Trypan blue dye exclusion staining. Cell viability should be between 80-90%.
[0049] Wash twice the JC with 10 ml of PBS-2% BSA.
[0050] Prepare a JC suspension in cloning medium or PBS-2% BSA containing 5,000,000 cells/ml.
[0051] Dispense 50 ml of JC suspension into falcon tubes (250,000 cells/tube).
[0052] For the sample incubation:
[0053] Add 200 ul samples, serum from early pregnancy controls (3 positive controls) or PBS-2% BSA (negative control). Mix gently.
[0054] Incubate at room temperature for 20-30 min.
[0055] Add 200 ul of MabCD2-Cy5 diluted 1:200 in PBS-2% BSA. Mix gently.
[0056] Incubate at room temperature for 20-30 min.
[0057] For flow cytometric determination:
[0058] Measure the fluorescence of each tube (488 nm laser excitation wavelength). Compare the fluorescence of alive and total cells and total dead cells (see FIG. 5 ) with controls.
[0059] Calculate PIF activity as follows:
[0060] Fluorescence of total cells/% dead cells×Fluorescence of alive cells
[0061] Interpretation of the results
[0062] PIF negative activity should be in the range of: 130-340
[0063] Positive PIF samples are out side of the negative reference range
[0064] Various publications are cited herein, the contents of which are hereby incorporated by reference in their entireties. | The present invention relates to assay methods used for detecting the presence of PIF, and to PIF peptides identified using this assay. In particular, the present invention relates to flow cytometry assays for detecting PIF. It is based, at least in part, on the observation that flow cytometry using fluorescently labeled anti-lymphocyte and anti-platelet antibodies demonstrated an increase in rosette formation in the presence of PIF. It is further based on the observation that flow cytometry demonstrated that monoclonal antibody binding to CD2 decreased in the presence of PIF. The present invention further relates to PIF peptides which, when added to Jurkat cell cultures, have been observed to either (i) decrease binding of anti-CD2 antibody to Jurkat cells; (ii) increase expression of CD2 in Jurkat cells; or (iii) decrease Jurkat cell viability. In additional embodiments, the present invention provides for ELISA assays which detect PIF by determining the effect of a test sample on the binding of anti-CD2 antibody to a CD2 substrate. | 2 |
BACKGROUND
[0001] A fog machine is a device that emits a stream or puff of visible vapor or fog for theatrical or similar purposes. The effect can be enhanced by projecting light through the emitted fog to provide a dramatic visual effect on stage, in a dance club, etc. A fog machine operates by pumping a non-toxic fog fluid, such as glycol, glycerine, or a water-based mixture thereof, into an airstream and past a heating element. The airstream is typically provided by a fan. The heating element causes the fluid to vaporize, producing a visible vapor or fog.
[0002] Fog machines are typically portable but not especially compact, generally having a boxy shape with a size on the order of that of a small suitcase or briefcase and weighing on the order of 5-10 pounds (2.25-4.5 kilograms) or more. Most fog machines are powered by utility power, i.e., they must be plugged into a wall outlet, portable generator or similar source of utility-level power. Accordingly, fog machines are typically brought to an unobtrusive location in a corner of a theater stage or other location where a performance or other activity is to take place, left in place throughout the activity, and used at times during the activity to produce fog. Compact, battery-powered fog machines have been developed, but remain uneconomical due to complex, specialized parts.
SUMMARY
[0003] Embodiments of the present invention relate to a system for generating fog effects. An exemplary system can include a control system, a fog fluid reservoir, an elongated insulator, an elongated electric heating element, an air supply subsystem, a fog fluid supply subsystem, and a handheld body.
[0004] The control system can include a battery-operated power supply and a user-operable control such as a switch. The control system initiates system operation at least in part in response to the user-operated control. The heating element extends along the insulator and is coupled to the control system. The control system electrically energizes the heating element during system operation. The air supply subsystem is coupled to the control system and directs a flow of air in a direction along the heating element from an intake end toward an exhaust end during system operation. The fog fluid supply subsystem is coupled to the fog fluid reservoir and the control system, and supplies fog fluid to the flow of air during system operation.
[0005] The handheld body has an opening substantially adjacent to the exhaust ends of the heating element and insulator and contains the battery-operated power supply, the fog fluid reservoir, the insulator, the heating element, the air supply subsystem, and the fog fluid supply subsystem. In some embodiments, the body can also be elongated and resemble an object that characteristically bums, such as torch, cigar, etc. In this manner the handheld fog effects system can be used as an acting prop, toy or similar device.
[0006] Other systems, methods, features, and advantages of the invention will be or become apparent to one of skill in the art to which the invention relates upon examination of the following figures and detailed description. All such additional systems, methods, features, and advantages are encompassed by this description and the accompanying claims.
BRIEF DESCRIPTION OF THE FIGURES
[0007] The invention can be better understood with reference to the following figures. The elements shown in the figures are not necessarily to scale, emphasis instead being placed upon clearly illustrating the principles of the invention. Also, in the figures like reference numerals designate corresponding elements throughout the different views.
[0008] FIG. 1 is a block diagram of a fog effects system, in accordance with an exemplary embodiment of the invention.
[0009] FIG. 2 is a side elevation view of a portion of the fog effects system of FIG. 1 .
[0010] FIG. 3 is a sectional view taken on line 3 - 3 of FIG. 2 .
[0011] FIG. 4 is a sectional view taken on line 4 - 4 of FIG. 2 .
[0012] FIG. 5 is a side elevation view of the exemplary fog effects system of FIG. 1 .
[0013] FIG. 6 is a similar to FIG. 5 , showing another side of the exemplary fog effects system.
[0014] FIG. 7 is a side elevation view of the exemplary fog effects system of FIG. 1 , housed in a body resembling a torch.
[0015] FIG. 8 is a side elevation view of the exemplary fog effects system of FIG. 1 , housed in a body resembling a cigar.
DETAILED DESCRIPTION
[0016] As illustrated in FIG. 1 , in an illustrative or exemplary embodiment of the invention, a fog effects system comprises a fog generator system 10 that includes a heating element 12 , an insulator 14 , a fog fluid reservoir 16 , an air pump 18 , and a liquid pump 20 . Fog generator system 10 further includes a battery-operated power supply 22 that includes one or more batteries and associated electrical connectors or other power supply elements. Power supply 22 can employ, for example, four AA-size (1.5 volt) batteries connected in series with each other to produce 6 volts. Fog generator system 10 also includes two user-operable switches 24 and 26 or similar controls. In this exemplary embodiment, power supply 22 , switches 24 and 26 and associated electrical connections can together define a control system. However, in other embodiments control systems can include additional or different electronic or mechanical elements. Similarly, although in the exemplary embodiment air pump 18 and associated electrical, pneumatic and mechanical connections (described below in further detail) can define an air supply subsystem, and liquid pump 20 and associated electrical, fluid and mechanical connections (described below in further detail) can define a fog fluid supply subsystem, in other embodiments air supply subsystems and fog fluid supply subsystems can include additional or different electronic, fluid, pneumatic, mechanical, etc. elements. For example, in an alternative embodiment (not shown) the air supply subsystem can include a controllable valve, vane, flap, etc. for directing the flow of air, instead of or in addition to energizing the air pump. Similarly, the fog fluid supply subsystem can include other such controllable elements. Alternatively to being controllable, in some embodiments such elements can be fixed or otherwise passive. Also, in such other embodiments, the liquid pump, air pump, or both can be operated manually rather than electrically. Indeed, in some embodiments, one of the fog fluid supply subsystem and the air supply subsystem need not include a pump at all. Rather, for example, the fog fluid supply system can produce a stream of fog fluid that is sufficiently atomized without the use of an air pump. Also, in other embodiments, the control system and elements that it controls can be configured to cause the fog to be emitted in a specific pattern or other manner, such as in a puff of predetermined duration, a series of puffs, a continuous stream, a pseudo-random manner, or any other desired manner, to create any desired effect.
[0017] In the illustrated embodiment, when a user closes switch 26 , which can be, for example, a miniature slide switch, heating element 12 is electrically coupled to battery-operated power supply 22 and therefore energized. When energized, heating element 12 , which can be, for example, a nickel-chromium or nichrome resistance wire, quickly becomes hot. Then, when a user closes switch 24 , which can be, for example, a momentary-contact pushbutton switch, air pump 18 and liquid pump 20 are each electrically coupled to battery-operated power supply 22 and therefore energized. Air pump 18 can be any suitable pump that can deliver a flow of air, such as a diaphragm pump. When energized, air pump 18 pumps air into an intake end of insulator 14 , which can be, for example, a hollow tube made of ceramic, glass or similar heat-insulating material. Liquid pump 20 can be any suitable pump that can deliver a liquid in a controlled manner, such as a peristaltic pump. When energized, liquid pump 20 pumps fog fluid from fog fluid reservoir 16 into the flow of air or airstream at the intake end of insulator 14 . Heating element 12 is aligned along insulator 14 and has an intake end corresponding to the intake end of insulator 14 and an exhaust end corresponding to the exhaust end of insulator 14 . At the intake ends of heating element 12 and insulator 14 , the heat emitted by heating element 12 begins to vaporize the fog fluid that is carried in the air stream. The vaporization continues as the fog fluid is conveyed through the airstream along the length of heating element 12 and insulator 14 toward the exhaust ends of heating element 12 and insulator 14 . The vapor or fog is emitted at the exhaust ends of heating element 12 and insulator 14 , as indicated by the arrow 28 .
[0018] The fog effects system can also include an illumination system 30 to illuminate the fog emanating from fog generator system 10 for an added dramatic effect. Illumination system 30 can comprise one or more electrical lighting elements, such as light-emitting diodes (LEDs) 32 (only one of which is shown in FIG. 1 for purposes of clarity, but several are connected together in parallel in the exemplary embodiment), and a lighting controller 34 . Lighting controller 34 controls the operation of LEDs 32 by, for example, causing them to flash in a manner that provides a flickering effect that evokes an appearance of flames or fire. Lighting controller 34 can include, for example, a programmable interface controller (PIC) device, which is a well-known device that is commercially available from a variety of sources. As persons skilled in the art understand how PIC devices are programmed and connected, these aspects are not described herein. The LEDs 32 can include a combination of red, amber and white or other colored LEDs that emit colors resembling those of fire, and lighting controller 34 can cause the various colors to alternately flash in a manner that resembles the changing colors of a flickering fire. Although not shown for purposes of clarity, lighting controller 34 is coupled to an output of the above-described control system of fog generator 10 that includes switch 24 so that when a user presses switch 24 lighting controller 34 activates LEDs 32 to illuminate the emitted fog. Although in the exemplary embodiment lighting controller 34 of illumination system 30 is somewhat separate from the control system of fog generator 10 , in other embodiments the lighting control functions and fog generator control functions can be integrated or combined with each other using, for example, a single PIC device or similar controller to control these functions and others.
[0019] As illustrated in FIGS. 2-4 , an air hose 36 delivers air from air pump 18 to a coupling tube 38 , which is connected to the intake end of the (tubular) insulator 14 . Similarly, a liquid hose 40 delivers fog fluid from liquid pump 20 to coupling tube 38 . In the exemplary embodiment, heating element 12 has a helical shape and is disposed within insulator 14 , as best shown in FIG. 2 . Insulator 14 can be made of a suitable heat-insulating material, such as ceramic. Insulator 14 is, in turn, disposed within an outer tube 42 and held in place by a retaining tube 44 . Retaining tube 44 has a flattened or elliptical cross-sectional shape that squeezes or holds insulator 14 centered within retaining tube 44 . Although in other embodiments (not shown) an insulator can be retained in any other suitable manner, such as by one or more spacers (not shown) extending between the insulator and the outer tube or similar outer structure, the flattened tube of the exemplary embodiment provides the retaining function in a manner that can be economically manufactured from readily available metal tubes. Outer tube 42 and retaining tube 44 can be made of economical but durable materials such as aluminum or brass. The heat-insulating property of insulator 14 and the air gaps between insulator 14 and retaining tube 44 and between retaining tube 44 and outer tube 42 insulate outer tube 42 against becoming unsafely or uncomfortably hot, thereby facilitating use of the fog effects system as part of a toy, prop, costume, etc., worn or held by a person. Although tubes 42 and 44 are metal tubes in the exemplary embodiment, in other embodiments (not shown) analogous structures can have any other suitable shapes and compositions. Although in the exemplary embodiment outer tube 42 serves as one of the electrical conductors for powering heating element 12 (as described below in further detail), in embodiments (not shown) in which the tubes or other structures are made of a non-conductive material, a separate electrical conductor can be included.
[0020] A first clamp-like ring terminal 46 can be attached to coupling tube 38 to electrically couple one side or polarity output, e.g., a positive polarity output, of the above-described control system to heating element 12 . The proximal end (i.e., intake end) of heating element 12 can be electrically coupled to coupling tube 38 by, for example, friction-fitting it within a groove-like indentation 48 in coupling tube 38 between the outer wall of coupling tube 38 and the inner wall of insulator 14 , as best shown in FIG. 3 . A second clamp-like ring terminal 50 can be attached to outer tube 42 to electrically couple the other side or polarity output, e.g., a negative polarity output, of the above-described control system to heating element 12 . The distal end (i.e., exhaust end) of heating element 12 can be electrically coupled to retaining tube 44 by, for example, friction-fitting it within a groove-like indentation 52 in retaining tube 44 between the outer wall of retaining tube 44 and the inner wall of outer tube 42 , as best shown in FIG. 3 .
[0021] In operation, liquid pump 20 pumps fog fluid from fog fluid reservoir 16 into the airstream produced by air pump 18 . The hot heating element 12 vaporizes the fog fluid as the fog fluid suspended in the airstream migrates along the length of heating element 12 from its proximal or intake end toward its distal or exhaust end. The relatively long region in which the fog fluid suspended in the airstream can absorb the heat emitted by heating element 12 promotes complete vaporization despite the relatively low voltage (for example, 6 volts) applied to heating element 12 by battery-operated power supply 22 .
[0022] A frusto-conical nozzle 54 having an exhaust opening 56 is attached to the distal end (i.e., exhaust end) of outer tube 42 , with exhaust opening 56 adjacent to the exhaust ends of heating element 12 and insulator 14 . In operation, the fog effects system emits the vapor or fog through exhaust opening 56 .
[0023] As illustrated in FIGS. 5-6 , fog generator system 10 and illumination system 30 can be mounted within a body 58 . Switches 24 and 26 can be mounted in walls of body 58 to facilitate their operation by a user (not shown). The LEDs 32 of illumination system 30 can be mounted around the periphery of a ring 60 near nozzle 54 . A perforated disk 62 can be mounted adjacent nozzle 54 to aid dispersing or inducing laminar flow of the vapor or fog. Similarly, a grating 64 , which can have hexagonal openings (not shown) arrayed in a honeycomb fashion, can similarly aid dispersing the vapor or fog. A user can fill fog fluid reservoir 16 through a removable cap 59 .
[0024] Body 58 is shown in broken line in FIG. 5 to indicate that it need not have the indicated cylindrical shape. Rather, body 58 can have a shape that resembles an object that characteristically bums, such as the torch shape shown in FIG. 7 or the cigar shape shown in FIG. 8 . An actor, for example, can hold a fog effects system having a torch-shaped body 58 in his hand and use it as a prop to simulate a burning torch. Note that switch 24 is mounted in an orientation in or on body 58 that facilitates button 24 to be actuated by the user's finger in a trigger-like manner when the user (not shown) is gripping body 58 . When the actor or other user presses button 24 , the fog effects system emits a stream of fog and generates flickering light. The simulated smoke and the flickering light combine to create an effect that is evocative of the fire in a torch.
[0025] Similarly, an actor can hold a fog effects system having a cigar-shaped body 60 in his hand and use it as a prop to simulate a burning cigar. When the actor or other user presses switch 24 , the fog effects system emits a puff of fog and generates a glowing light. The simulated smoke and glowing light combine to create an effect that is evocative of a burning cigar. In view of these descriptions, persons skilled in the art can readily provide fog effects systems having bodies with other shapes that simulate or resemble any other such hand-held objects that are characteristically used in a burning state.
[0026] It should be noted that embodiments in which operation is initiated in a trigger-like manner especially lend themselves to the inclusion of a manually operated or otherwise non-electrically-operated fog fluid supply subsystem, air supply subsystem, or both. For example, a manually operated fog fluid pump (not shown) can have a trigger resembling button 24 shown in FIG. 5 . The force that the user's finger applies to the trigger operates the fog fluid pump.
[0027] Furthermore, in other embodiments (not shown) one of the fog fluid supply subsystem and the air supply subsystem can operate more passively than the other. For example, in some embodiments the fog fluid introduced by the fog fluid supply subsystem is flash-vaporized so rapidly that as it changes from a liquid to a gas the expanding gas creates such a sufficient flow of the vapor out of the exhaust end that no air pump is needed. In such embodiments the air supply subsystem serves to passively direct the flow. It should be noted that although in the embodiment described above both the fog fluid supply subsystem and air supply subsystem are electrically operated (i.e., both air pump 18 and a liquid pump 20 are electrically operated), in other embodiments neither the fog fluid supply subsystem nor the air supply subsystem need be electrically operated. For example, the fog fluid pump can be manually operated, and the air supply subsystem can operate passively, directing the expanding vapor out the exhaust end.
[0028] While one or more embodiments of the invention have been described as illustrative of or examples of the invention, it will be apparent to those of ordinary skill in the art that other embodiments are possible that are within the scope of the invention. Accordingly, the scope of the invention is not to be limited by such embodiments but rather is determined by the appended claims. | A fog effects system includes a control system, a fog fluid reservoir, an elongated insulator, an elongated electric heating element, an air supply subsystem, a fog fluid supply subsystem, and a handheld body. The control system can include a battery-operated power supply and a user-operable control. The heating element extends along the insulator. The control system electrically energizes the heating element during system operation. The air supply subsystem directs a flow of air along the heating element during system operation. The fog fluid supply supplies fog fluid to the flow of air. The heating element vaporizes the fog fluid, which is emitted from an end of the system. | 0 |
CROSS REFERENCE TO RELATED APPLICATIONS
[0001] This application claims the benefit and priority of the following applications, each of which is incorporated herein by reference in its entirety: the U.S. Provisional Application bearing Ser. No. 60/189,317, filed Mar. 14, 2000; the U.S. Provisional Application bearing Ser. No. 60/202,721, filed May 8, 2000; and the U.S. Non-Provisional Application bearing Ser. No. 09/805,754, filed Mar. 13, 2001, now U.S. Pat. No. 6,575,066 B2.
FIELD
[0002] The material described herein relates generally to the field of wood and lumber processing and, more particularly, to the efficient reduction or cutting of scrap wood into useable chips.
BACKGROUND
[0003] Lumber mills and other wood processing facilities typically generate wood scraps of various sizes. In plywood processing mills, for example, the wood scraps can be in the form of thin, elongate, veneer-like strips. To be useful in the manufacture of paper, cardboard, and other recyclable materials, wood scraps must be reduced into wood chips having an acceptable size and shape. Mills use screens to separate acceptable wood chips from oversized wood chips. The oversized wood chips are sometimes referred to as overs because they pass over the separating screens.
[0004] Ideally, the overs need to be reduced to wood chips that are relatively uniform in size, having gross dimensions of approximately one inch or less. The desirable chip size may vary, depending upon the intended use. Several different types of machines have been tried for reducing overs, such as disc chippers, drum chippers, chip hogs, and the like. These machines often crush or pulverize the overs into unusable bits that are unacceptable for use in making paper, for example.
[0005] Mills typically generate a nearly steady flow of overs during wood processing, creating a concomitant need for a system capable of processing overs continuously. The flow of incoming overs may vary greatly, from zero to a large batch, depending upon the mill operations. Most available systems are not capable of adapting to changing volumes without interrupting processing or requiring expensive manual labor when a system becomes jammed or overloaded.
[0006] The presence of metal objects in batch wood processing presents an ongoing challenge to facilities where equipment is both expensive and sensitive to damage from metal. The cost and delay of stopping a major piece of equipment to remove metal or repair the damage it caused represents an unacceptable expense for most facilities. Even small metal objects can cause significant damage, especially to grinders and chippers having an array of closely-spaced saw blades. The machinery in use, for example, to reduce overs into small wood chips may be particularly vulnerable to damage from small metal objects.
[0007] Thus, there is a need in the art for improvements for the task of safely reducing overs to an acceptable and useful size, efficiently and steadily, during ongoing mill operations.
SUMMARY
[0008] The following summary is not an extensive overview and is not intended to identify key or critical elements of the systems, methods, apparatuses, processes, and the like or to delineate the scope of such elements. This Summary provides a conceptual introduction in a simplified form as a prelude to the more-detailed description that follows.
[0009] Certain illustrative systems, methods, apparatuses, processes, and the like are described herein as examples in connection with the following description and the accompanying drawing figures. These examples represent but a few of the various ways in which the principles underlying the systems, methods, apparatuses, processes, and the like may be employed and thus are intended to include equivalents. Other advantages and novel features may become apparent from the detailed description presented later, when considered in conjunction with the drawing figures.
[0010] The above and other needs are met by the present invention which, in one embodiment, provides a system, method, and apparatus for reducing a continuous incoming flow of oversized wood chips known as overs by cutting them smoothly, with minor impact, so the resulting chips are suitable for making paper, cardboard, and other recyclable materials.
[0011] The examples described herein include an apparatus for reducing the size of wood chips. The apparatus may include a saw assembly having an array of blades disposed upon a shaft and configured to be driven at a cutting speed in a first rotational direction. The shaft may define a shaft interference zone. The apparatus may also include a feeder assembly configured to direct a flow of the wood chips along a feeder path, the feeder path passing into and through the array of blades. The feeder assembly may define a feeder zone at least partially intersecting the array of blades. The apparatus may also include a topper assembly positioned proximate the feeder path, the topper assembly located upstream of the saw assembly relative to the feeder path. The topper assembly may be configured to reduce the height of the flow of the wood chips such that the flow of wood chips does not tend to extend into the shaft interference zone. The apparatus may reduce the wood chips into a plurality of cut chips.
[0012] The saw assembly may be positioned such that the shaft interference zone nearly intersects tangentially with the feeder zone.
[0013] The topper assembly may be positioned such that the topper zone nearly intersects tangentially with the feeder zone.
[0014] The saw assembly may further include an array of spacers disposed upon the shaft, with the spacers positioned alternately between the array of blades.
[0015] The feeder assembly may include one or more paddle assemblies configured to be driven along the feeder path at a feeder speed in a direction generally opposing the first rotational direction. Each of the paddle assemblies may define an array of slots therethrough, positioned to accept insertion of the array of blades.
[0016] The paddle assemblies may include a series of like paddle members. The paddle assemblies may be disposed upon a drum and the drum may be mounted upon a feeder shaft.
[0017] In one embodiment, the paddle assemblies may be mounted to an endless chain configured to be driven along an endless feeder path about one or more powered rollers, the endless feeder path comprising one or more either straight or curved segments, and the endless path may coincide with the feeder path at least during the flow through the array of blades.
[0018] The paddle assemblies may also include a scoop portion shaped to cradle the wood chips and a fence portion shaped to contain the wood chips during the flow through the array of blades.
[0019] The paddle assemblies may be shaped to align the oblong chips generally transverse to the array of blades in preparation for the flow through the saw assembly.
[0020] The fence may be further shaped to contain the wood chips in opposition generally to the wind force created by the saw assembly.
[0021] The topper assembly may include one or more topper blades disposed upon a shaft and configured to be driven at a topping speed in the first rotational direction.
[0022] The apparatus may further include a conveyor assembly providing an incoming flow of the wood chips.
[0023] The apparatus may also include a chute disposed in an engaged position to guide the flow of the wood chips toward the feeder assembly, the chute having a floor and a lower chute edge.
[0024] The chute may further include a chute actuator configured to move the chute relative to the feeder assembly between the engaged position and a disengaged position, the disengaged position characterized by the chute guiding the wood chips away from the feeder assembly; and a chute controller operably connected to the chute actuator.
[0025] The chute may further include a chute load sensor positioned along the chute near the flow of wood chips; the chute load sensor operably connected to the chute controller, the chute load senior capable of transmitting at least a normal signal and a fault signal.
[0026] The chute load sensor may include a metal detector, and the fault signal indicates a metal object in the flow of wood chips.
[0027] In one embodiment, the chute actuator moves the chute into the disengaged position in response to a fault signal.
[0028] The apparatus may also include a darn positioned between the chute and the feeder assembly, the dam shaped to urge the wood chips toward the feeder assembly. The dam may include an inner face oriented toward the feeder assembly (the inner face shaped to nearly coincide with the feeder zone), a trailing dam edge, and a leading dam edge.
[0029] The dam may be stationary relative to the feeder assembly and the trailing dam edge may nearly meet the lower chute edge when the chute is in the engaged position. Where the paddle assemblies include an outer paddle face and a leading paddle edge, the dam may be positioned such that the outer paddle face nearly meets the inner dam face and the leading paddle edge nearly meets the leading dam edge.
[0030] In another example, an apparatus for reducing the size of wood chips may include a saw assembly having an array of blades disposed in spaced-apart relation upon a shaft and configured to be driven at a cutting speed in a first rotational direction, the shaft defining a shaft interference zone; a feeder assembly configured to direct a flow of the wood chips along a feeder path, the feeder path passing into and through the array of blades, the feeder assembly defining a feeder zone at least partially intersecting the array of blades, wherein the saw assembly is positioned such that the shaft interference zone nearly intersects tangentially with the feeder zone; a topper assembly positioned proximate the feeder path, the topper assembly located upstream of the saw assembly relative to the feeder path, the topper assembly configured to reduce the height of the flow of the wood chips such that the flow of wood chips does not tend to extend into the shaft interference zone, the topper assembly defining a topper zone, the topper assembly positioned such that the topper zone nearly intersects tangentially with the feeder zone; and a chute disposed in an engaged position to guide the flow of the wood chips toward the feeder assembly, the chute comprising a floor and a lower chute edge, the apparatus reducing the wood chips into a plurality of cut chips.
[0031] In another example, an apparatus for reducing the size of wood chips may include the elements described in the immediately-preceding paragraph and, in addition, a dam positioned between the chute and the feeder assembly, the dam shaped to urge the wood chips toward the feeder assembly, the dam comprising an inner face oriented toward the feeder assembly, the inner face shaped to nearly coincide with the feeder zone, a trailing dam edge, and a leading dam edge.
[0032] In another example, an apparatus for reducing the size of wood chips may include a saw assembly having an array of blades disposed in spaced-apart relation upon a shaft and configured to be driven at a cutting speed in a first rotational direction, the shaft defining a shaft interference zone; a feeder assembly configured to direct a flow of the wood chips along an endless feeder path, the endless feeder path comprising one or more either straight or curved segments, the feeder path passing into and through the array of blades, the feeder assembly defining a feeder zone at least partially intersecting the array of blades; a topper assembly positioned proximate the feeder path, the topper assembly located upstream of the saw assembly relative to the feeder path, the topper assembly configured to reduce the height of the flow of the wood chips such that the flow of wood chips does not tend to extend into the shaft interference zone, the topper assembly defining a topper zone, the apparatus reducing the wood chips into a plurality of cut chips.
[0033] In another aspect of the present invention, a control system for wood-reducing apparatus is disclosed. The system may include a saw load sensor operably connected to the saw assembly and configured to sense a saw load; a feeder load sensor operably connected to the feeder assembly and configured to sense a feeder load; a topper load sensor operably connected to the topper assembly and configured to sense a topper load; a chute load sensor operably connected to the chute and configured to sense a chute load; and a master controller operably connected to each of the respective sensors, each of the respective sensors capable of transmitting at least a normal signal and a fault signal.
[0034] In the exemplary control system, the master controller, in response to a fault signal from any of the respective sensors received at a start time, may (a) direct the chute actuator to move the chute into the disengaged position, the disengaged position characterized by the chute guiding the wood chips away from the feeder assembly; and (b) direct the feeder assembly to drive the feeder assembly in the first rotational direction. The master controller, in response to a normal signal from each of the respective sensors received at an end time following the start time, may also (a) direct the chute actuator to move the chute into the engaged position; and (b) direct the feeder assembly to drive the feeder assembly in a direction generally opposing the first rotational direction.
[0035] Also, in the exemplary control system, the master controller, in response to a fault signal from any of the respective sensors received at a first time, may (i) direct the feeder assembly to pause the feeder assembly; (ii) direct the saw assembly to pause the saw assembly; and (iii) direct the topper assembly to pause the topper assembly. The master controller, in response to a normal signal from each of the respective sensors received at a second time following the first time, may also direct the feeder assembly, saw assembly, and topper assembly, respectively, to return to the normal operating condition.
[0036] In another aspect of the present invention, a method of reducing the size of wood chips is disclosed. The method may include directing a flow of the wood chips along a feeder path, the feeder path passing into and through a saw assembly, the saw assembly having an array of blades disposed upon a shaft and configured to be driven at a cutting speed in a first rotational direction, the shaft defining a shaft interference zone; providing a feeder assembly configured to direct the flow of the wood chips along the feeder path, the feeder assembly defining a feeder zone at least partially intersection the array of blades; and positioning a topper assembly proximate the feeder path, the topper assembly located upstream of the saw assembly relative to the feeder path, the topper assembly configured to reduce the height of the flow of the wood chips such that the flow of wood chips does not tend to extend into the shaft interference zone, the topper assembly defining a topper zone.
[0037] The method may also include positioning the saw assembly such that the shaft interference zone nearly intersects tangentially with the feeder zone; and positioning the topper assembly such that the topper zone nearly intersects tangentially with the feeder zone.
[0038] The method may also include equipping the feeder assembly with one or more paddle assemblies configured to be driven along the feeder path at a feeder speed in a direction generally opposing the first rotational direction, each of the one or more paddle assemblies defining an array of slots therethrough; and positioning the slots to accept insertion of the array of blades.
[0039] The method may also include mounting the one or more paddle assemblies to an endless chain configured to be driven along an endless feeder path about one or more powered rollers, the endless feeder path comprising one or more either straight or curved segments, and the endless path coinciding with the feeder path at least during the flow through the array of blades.
[0040] The method may also include shaping the one or more paddle assemblies to align the wood chips generally transverse to the array of blades in preparation for the flow through the saw assembly; providing a scoop portion shaped to cradle the wood chips substantially within each of the one or more paddle assemblies; and providing a fence portion shaped to contain the wood chips substantially within each of the one or more paddle assemblies during the flow through the array of blades.
[0041] The method may also include equipping the topper assembly with one or more topper blades disposed upon a shaft and configured to be driven at a topping speed in the first rotational direction.
[0042] The method may also include providing a chute disposed in an engaged position to guide the flow of the wood chips toward the feeder assembly, the chute comprising a floor and a lower chute edge.
[0043] The method may also include providing a chute actuator configured to move the chute relative to the feeder assembly between the engaged position and a disengaged position, the disengaged position characterized by the chute guiding the wood chips away from the feeder assembly; operably connecting a chute controller to the chute actuator; locating a chute load sensor along the chute near the flow of wood chips, the chute load sensor capable of transmitting at least a normal signal and a fault signal; and operably connecting the chute load sensor to the chute controller.
[0044] The method may also include the chute actuator moving the chute into the disengaged position in response to a fault signal.
[0045] The method may also include positioning a dam between the chute and the feeder assembly, the dam shaped to urge the wood chips toward the feeder assembly; and shaping the dam to include an inner face oriented toward the feeder assembly, the inner face shaped to nearly coincide with the feeder zone, a trailing dam edge, and a leading dam edge.
[0046] The method may also include mounting the dam in a stationary location relative to the feeder assembly; positioning the dam such that the trailing dam edge nearly meets the lower chute edge when the chute is in the engaged position.
[0047] The method may also include, where the one or more paddle assemblies comprises an outer paddle face and a leading paddle edge, positioning the dam such that the outer paddle face nearly meets the inner dam face; and positioning the dam such that the leading paddle edge nearly meets the leading dam edge.
[0048] These and other objects, features, and advantages of the present invention will become apparent upon reading the following detailed description of a preferred embodiment of the invention when taken in conjunction with the drawing and the appended claims.
BRIEF DESCRIPTION OF THE DRAWING
[0049] The invention will be more readily understood by reference to the following description, taken with the accompanying drawing figures, in which:
[0050] FIG. 1 is an illustration of a side elevation of an apparatus, according to one embodiment of the present invention.
[0051] FIG. 2 is a schematic illustration of a side view of an apparatus, according to one embodiment of the present invention.
[0052] FIG. 3 is a cross-sectional illustration of a saw assembly, according to one embodiment of the present invention.
[0053] FIG. 4 is an illustration of a feeder assembly, according to one embodiment of the present invention.
[0054] FIG. 5 is a schematic illustration of a control system, according to one embodiment of the present invention.
[0055] FIG. 6 is an illustration of a side elevation of an apparatus in a disengaged position, according to one embodiment of the present invention.
[0056] FIG. 7 is an illustration of a side elevation of an apparatus, according to one embodiment of the present invention.
[0057] FIG. 8 is an illustration of an array of paddle members, according to one embodiment of the present invention.
[0058] FIG. 9 is an illustration of a side elevation of an apparatus, according to one embodiment of the present invention.
DETAILED DESCRIPTION
[0059] The subject matter of this application is related to that of the following applications, each of which is incorporated herein by reference in its entirety: the U.S. Provisional Application bearing Ser. No. 60/189,317, filed Mar. 14, 2000; the U.S. Provisional Application bearing Ser. No. 60/202,721, filed May 8, 2000; and the U.S. Non-Provisional Application bearing Ser. No. 09/805,754, filed Mar. 13, 2001, now U.S. Pat. No. 6,575,066 B2.
[0000] 1. Introduction
[0060] Exemplary systems, methods, and apparatuses are now described with reference to the drawings, where like reference numerals are used to refer to like elements throughout the several views. In the following description, for purposes of explanation, numerous specific details are set forth in order to facilitate a thorough understanding of the systems, methods, apparatuses, processes, and the like. It may be evident, however, that the systems, methods, apparatuses, processes, and the like can be practiced without these specific details. In other instances, well-known structures and devices are shown in block diagram form in order to simplify the description.
[0061] “Controller,” as used herein, includes but is not limited to hardware, firmware, software and/or combinations of each to perform one or more functions or actions. For example, based upon a desired application or needs, a controller may include a software-controlled microprocessor, a Programmable Logic Controller (PLC), a discrete logic system such as an Application-Specific Integrated Circuit (ASIC), or other programmed logic device. The logic driving a controller may be fully embodied as software.
[0062] “Signal,” as used herein, includes but is not limited to one or more electrical or optical signals, analog or digital, one or more computer instructions, a bit or bit stream, or the like.
[0063] “Sensor,” as used herein, includes but is not limited to one or more elements capable of sensing or otherwise receiving current data or status information from a particular location. A sensor may be used, for example, to indicate equipment status such as feed rate, tool wear, loss of prime on pumps, motor load or amperage, mixer viscosity, the presence of metal objects, or any type of overload or under-load condition. A sensor may also include equipment for staging or timing the operation pump motors, conveyors, hoppers, and other machinery. A sensor may include a current transformer, transducer, relays, alarm circuits, contactors, and auxiliary contacts.
[0064] “Software,” as used herein, includes but is not limited to, one or more computer readable and/or executable instructions that cause a computer, computer component, a controller such as a Programmable Logic Controller (PLC), and/or any other electronic device to perform functions, execute actions, receive and/or send signals, and/or behave in a desired manner. The instructions may be embodied in various forms like routines, algorithms, modules, methods, threads, ladder logic configurations, and/or programs. Software may also be implemented in a variety of executable and/or loadable forms including, but not limited to, a stand-alone program, a function call (local and/or remote), a servelet, an applet, instructions stored in a memory, part of an operating system or browser, and the like. It is to be appreciated that the computer readable and/or executable instructions can be located in one computer component and/or distributed between two or more communicating, co-operating, and/or parallel-processing computer components and thus can be loaded and/or executed in serial, parallel, massively parallel and other manners. It will be appreciated by one of ordinary skill in the art that the form of software may be dependent on, for example, requirements of a desired application, the environment in which it runs, and/or the desires of a designer or programmer or the like.
[0065] An “operable connection” (or a connection by which entities are “operably connected”) is one in which signals, physical communication flow and/or logical communication flow may be sent and/or received. Usually, an operable connection includes a physical interface, an electrical interface, and/or a data interface, but it is to be noted that an operable connection may consist of differing combinations of these or other types of connections sufficient to allow operable control.
[0066] “Data store,” as used herein, refers to a physical and/or logical entity that can store data. A data store may be, for example, a database, a table, a file, a list, a queue, a heap, a sequential function table, structured text, a ladder logic list, and so on. A data store may reside in one logical and/or physical entity and/or may be distributed between two or more logical and/or physical entities.
[0067] Furthermore, to the extent that the term “includes” is employed in the detailed description or the claims, it is intended to be inclusive in a manner similar to the term “comprising” as that term is interpreted when employed as a transitional word in a claim. Further still, to the extent that the term “or” is employed in the claims (for example, A or B) it is intended to mean “A or B or both.” When the author intends to indicate “only A or B but not both,” the author will employ the phrase “A or B but not both.” Thus, use of the term “or” herein is inclusive, not exclusive. See Garner, A Dictionary Of Modem Legal Usage 624 (2d ed. 1995).
[0068] It will be appreciated that some or all of the processes and methods of the system involve electronic and/or software applications that may be dynamic and flexible processes so that they may be performed in other sequences different than those described herein. It will also be appreciated by one of ordinary skill in the art that elements embodied as software may be implemented using various programming approaches such as machine language, procedural, ladder logic, structured text, and object-oriented and/or artificial intelligence techniques.
[0069] The processing, analyses, and/or other functions described herein may also be implemented by functionally equivalent circuits like a digital signal processor circuit, a software-controlled microprocessor, a Programmable Logic Controller (PLC), or an application-specific integrated circuit. Components implemented as software are not limited to any particular programming language. Rather, the description herein provides the information one skilled in the art may use to fabricate circuits or to generate computer software to perform the processing of the system. It will be appreciated that some or all of the functions and/or behaviors of the present system and method may be implemented as logic as defined above.
[0070] Many modifications and other embodiments may come to mind to one skilled in the art who has the benefit of the teachings presented in the description and drawings. It should be understood, therefore, that the invention is not be limited to the specific embodiments disclosed and that modifications and alternative embodiments are intended to be included within the scope of the disclosure and the exemplary inventive concepts. Although specific terms may be used herein, they are used in a generic and descriptive sense only and not for purposes of limitation.
[0000] 2. A Wood-Reducing Apparatus
[0071] FIG. 1 illustrates an apparatus 10 having a saw assembly 80 , a feeder assembly 20 , and a topper assembly 70 . Generally described, the apparatus 10 according to the present invention may be configured to reduce wood chips known as overs 11 by cutting them into smaller chips for use in making paper, cardboard, and other recyclable materials. The overs 11 may take different shapes, including thin strips, generally-prismatic oblong segments, or any irregular shapes.
[0072] The apparatus 10 of the present invention may include a reciprocating or endless feeder path, meaning the apparatus 10 may process a continual flow of incoming overs 11 . The term continual is used herein because it implies a recurring event, as opposed to the term continuous, which implies an uninterrupted occurrence. The overs 11 may be supplied from the lumber mill or other wood processing facility in a generally continual flow, including periods where no overs 11 are incoming. The flow of incoming overs 11 may vary greatly in volume and duration, depending upon mill operations. The overs 11 in FIG. 1 are shown entering from above, generally, although the apparatus 10 may be configured to accept an incoming flow of overs 11 from any direction.
[0073] The apparatus 10 of the present invention provides the components and a control system capable of processing an incoming flow of overs 11 on a continual basis or on a batch basis. The apparatus 10 directs a flow of overs 11 through a saw assembly 80 , where the overs 11 are reduced into cut chips 13 . As used herein, the phrase “directs a flow” of overs 11 is meant to include receiving an incoming flow, re-directing an existing flow, or creating a new flow from a static collection of chips. FIG. 9 illustrates a flow of wood chips 11 through an apparatus 10 .
[0074] Beginning with entry of overs 11 into the area of the apparatus 10 , and referring to FIG. 1 , in one embodiment, the apparatus 10 may include a chute 60 to guide the overs 11 toward the feeder assembly 20 . The chute 60 may be moveable, to allow the apparatus 10 to direct the overs 11 away from the feeder assembly 20 if and when a fault condition develops. The apparatus 10 may also include a dam 50 to urge the overs 11 into the feeder assembly 20 . The dam 50 may be moveable or stationary, or it may be an integral part of the chute 60 .
[0075] The feeder assembly 20 directs the overs 11 along a feeder path toward and through the saw assembly 80 . The feeder path may be generally circular, as shown in FIG. 1 , or it may take different forms, as shown in FIG. 7 . The feeder assembly 20 may be configured to rotate counter-clockwise with respect to the side view illustrated in FIG. 1 . The feeder assembly 20 traces an imaginary feeder zone 320 (shown in FIG. 2 ) as it guides the overs 11 toward the saw assembly 80 .
[0076] In one embodiment, the feeder assembly 20 may include one or more paddle assemblies 40 disposed upon a rotating drum 30 . A paddle assembly 40 may include a series of discrete paddle members 440 , as shown in FIG. 8 . In this embodiment, the outermost surface of the paddle assemblies 40 trace the feeder zone 320 . Also, in this embodiment, each paddle assembly 40 may include an array of slots 45 such that the saw blades 83 extend into and pass through the slots 45 as the feeder assembly 20 moves past the saw assembly 80 . In one embodiment, the paddle members 440 are spaced apart, thereby forming the slots 45 , as shown in FIG. 8 . In one embodiment, the paddle members 440 are constructed of steel and machined to precise tolerances to create uniform slots 45 of a desired width (to produce a desired chip size).
[0077] In an alternative embodiment, the paddle assemblies 40 may be constructed of a high-density plastic material. In one embodiment, a method of preparing the paddles for use may include installing blank (un-slotted) paddles and moving the feeder assembly 20 slowly toward and through the saw assembly 80 such that the saw blades 83 themselves cut the paddle slots 45 . Allowing the saw blades 83 to cut their own corresponding slots 45 assures a good fit that is tailored to match the precise orientation of the saw blades 83 , without requiring precise attachment of the paddle assemblies 40 to the drum 30 .
[0078] Following the feeder path, as the feeder assembly 20 rotates, the overs 11 are directed first to the topper assembly 70 . In this aspect, the topper assembly 70 is generally upstream from the saw assembly 80 . The topper assembly 70 may be configured to rotate clockwise (opposing the rotation of the feeder assembly 20 ) with respect to the side view illustrated in FIG. 1 . The topper assembly 70 traces an imaginary topper zone 370 (illustrated in FIG. 2 ) as it rotates. The topper assembly 70 may include one or more topper blades disposed upon a topper shaft and driven at a topping speed. The topper blades may be disposed in a spiral about a topper drum or in any other configuration suitable for cutting. In an embodiment with topper blades, the outermost surface of the topper blades would trace the topper zone 370 .
[0079] Generally described, the topper assembly 70 removes excess overs 11 and/or cuts any portion of the overs 11 which may be extending beyond the feeder zone 320 (in other words, any overs 11 or any portion of the overs 11 extending to a height above the paddle assemblies 40 of the feeder assembly 20 ). In this aspect, the topper assembly 70 may strike and remove entire wood chips out of a paddle assembly 40 as it passes. Those portions of the overs 11 which are cut and removed by the topper assembly 70 may be referred to as tops 12 . The excess overs 11 and tops 12 are removed at this point so they will not encroach upon or otherwise interfere with the shaft of the saw assembly 80 . The tops 12 , as shown, generally fall under the force due to gravity back toward the feeder assembly 20 to be captured and again directed toward the saw assembly 80 .
[0080] After a particular paddle assembly 40 passes near the topper assembly 70 and the excess overs 11 and/or tops 12 are removed, the feeder assembly 20 continues to guide the overs 11 toward and into the saw assembly 80 . In one embodiment, the saw assembly 80 may include a plurality of spaced-apart high-speed circular saw blades 83 mounted on a horizontal blade shaft 82 driven by a saw drive assembly. The saw assembly 80 may be configured to rotate clockwise (opposing the rotation of the feeder assembly 20 ) with respect to the side view illustrated in FIG. 1 . The saw assembly 80 traces an imaginary sawing zone 380 (shown in FIG. 2 ) as the blades 83 rotate. Similarly, the saw blade shaft 82 traces an imaginary shaft interference zone 382 as it rotates. As mentioned above, the excess overs 11 and/or tops 12 are removed so they will not strike or otherwise interfere with the shaft 82 ; in other words, so no portion of the overs 11 will enter the shaft interference zone 382 . In one embodiment, the saw blades 83 may be spaced apart by a plurality of saw blade spacers 84 .
[0081] FIG. 3 is a cross-sectional illustration of a saw assembly 80 in one embodiment. The saw blades 83 may be horizontally stacked on a shaft 82 along with spacers 84 of appropriate thickness to produce a desired wood chip size. The saw blades 83 may be substantially planar and circular, and may include opposing saw blade keys cut into their center holes to provide an interlocking relationship with a pair of opposed blade shaft key slots on the blade shaft 82 . The interlocking keys and key slots may be provided to prevent the saw blades 83 from rotating relative to the blade shaft 82 .
[0082] In one aspect of the present invention, blades 83 and spacers 84 of various sizes may be provided and installed, to produce the desired chip size according to the intended use. The apparatus 10 may be configured with saws other than circular saws, including but not limited to band saws, jigsaws, chain saws, or other power saws. Saw blades 83 of any type may be used, without departing from the scope of the invention, to produce a desired chip size. Moreover, it should be understood that the saw blades 83 may be powered by devices other than the saw motor 830 , depending upon the particular saw type selected for the application.
[0083] The blade shaft 82 may include a solid shoulder 142 proximate one end with threads on the opposite end. The threaded end of the shaft may allow a large shoulder nut 143 to be tightened against an adjacent spacer 84 , causing the stacked spacers 84 and the saw blades 83 to be sandwiched together between the shoulder nut 143 and the shoulder 142 , and holding the saw blades 83 in place on the blade shaft 82 to be rotated therewith. The shoulder nut 143 not only provides a stop for the endmost spacer 84 , but also includes a pair of opposing flats which allow a wrench to grip the shaft 82 to control rotation thereof during assembly or disassembly. Journals near the ends of the blade shaft 82 for blade shaft bearings 420 with tapered bushings allow for easy removal of the bearings 420 (shown without frame supports for purposes of simplicity). A saw motor coupling 820 with a quick disconnect sleeve such as known in the art can be used.
[0084] FIG. 7 illustrates another embodiment of an apparatus 10 having a saw assembly 80 , a feeder assembly 20 , and a topper assembly 70 , according to the present invention. The feeder assembly 20 may direct the overs through an irregular feeder path and, in turn, trace a feeder zone 320 such as the one shown in FIG. 7 . The embodiment shown also includes a chute 60 and a dam 50 . The feeder assembly 20 generally moves in a clockwise direction with respect to the view shown.
[0000] 3. Zones of Interference
[0085] FIG. 2 is a side view illustration of several three-dimensional reference zones traced by elements of an apparatus 10 according to one embodiment of the present invention. The zones traced are three-dimensional. A generally cylindrical element, for example, will trace a three-dimensional zone shaped like a cylinder. A generally planar body rotating on a lengthwise hinge, for example, may trace a zone in the shape of a sector of a cylinder, somewhat resembling the shape of a pie slice.
[0086] Generally, as mentioned above, the feeder assembly 20 traces an imaginary feeder zone 320 as it moves. A feeder zone 320 is illustrated in FIG. 2 . The saw assembly 80 traces a sawing zone 380 . The saw blade shaft 82 traces a shaft interference zone 382 . The topper assembly 70 traces a topper zone 370 .
[0087] In one embodiment, the topper assembly 70 is positioned relative to the other elements such that the topper zone 370 nearly intersects tangentially the feeder zone 320 . In so doing, the topper assembly 70 is positioned so it will not interfere with the moving parts of the feeder assembly 20 . Also, the topper assembly 70 is positioned to remove any material that may tend to extend beyond the imaginary boundary created by the feeder zone 320 . Keeping material within the feeder zone 320 is a goal for this embodiment because the saw blade shaft 82 may be damaged by excess material.
[0088] The saw assembly 80 in one embodiment is also positioned relative to the feeder zone 320 . As shown, the shaft interference zone 382 also nearly intersects tangentially the feeder zone 320 . Also, as shown, for an embodiment where the feeder assembly 20 includes one or more paddle assemblies 40 , the sawing zone 380 may extend through nearly the full height of the paddle assemblies 40 . By positioning the saw assembly 80 in this location, the apparatus 10 takes advantage of the full cutting width of the saw blades 83 . Also, in this position, the saw assembly 80 will not interfere with the moving parts of the feeder assembly 20 .
[0089] The dam 50 in one embodiment may be positioned so that it nearly coincides with the feeder zone 320 . One of the roles of the dam 50 is to urge the overs 11 toward the feeder assembly so the overs 11 are nearly contained within the feeder zone 320 when they first enter the feeder assembly 20 . In this aspect, the dam 50 may reduce the burden on the topper assembly 70 . In an embodiment where the dam 50 may be part of the chute 60 , the chute 60 may be positioned such that the lower, dam portion of the chute 60 nearly coincides with the feeder zone 320 .
[0090] The chute 60 in one embodiment may be positioned so that its lower edge nearly intersects tangentially the feeder zone 320 . By positioning the chute 60 as shown, the lower edge guides overs into the space between the dam 50 and the feeder assembly 20 , such that the space lies generally within the feeder zone 320 . In this aspect, the chute position also contributes to keeping the overs within the feeder zone 320 .
[0091] The various positions are described as nearly tangential and nearly coinciding because a degree of separation or tolerance may exist between the elements of the apparatus 10 to allow relative movement and to prevent binding.
[0000] 4. Guiding Overs into a Feeder Assembly
[0092] FIG. 4 is a side view illustrating a portion of an apparatus 10 , according to one embodiment. A portion of a feeder assembly 20 is shown; in particular, the embodiment that includes one or more paddle assemblies 40 disposed on a drum 30 . In one embodiment, as shown the apparatus 10 may include a chute 60 and a dam 50 , which may be an integral part of the chute 60 or a separate element.
[0093] Each paddle assembly 40 , in one embodiment, includes a scoop portion 44 and a fence portion 344 , as shown in FIG. 4 . Recall the paddle assembly 40 may include a series of paddle members 440 , as shown in FIG. 8 , wherein each paddle member 440 has the same shape such that, together, the series of paddle members 440 forms a paddle assembly 40 like the one shown in FIG. 1 . The scoop portion 44 generally holds a quantity of overs 11 , conveying them along the feeder path. The scoop portion 44 is shaped to contain the overs 11 ; in three dimensions, the scoop portion 44 may be shaped like a trough. In one aspect, particularly for oblong overs, the scoop portion 44 may be shaped to align to the oblong overs in an orientation generally perpendicular to the blades 83 in the saw assembly 80 . In this aspect, the scoop portion 44 is shaped to align the oblong overs in preparation for cutting in a direction generally transverse to the longer lengthwise dimension of each wood chip.
[0094] The fence portion 344 extends away from the drum 30 , generally, on the open side of the scoop portion 44 . Referring again to FIG. 1 , the paddle assembly 40 that is passing through the saw assembly 80 shows one function of the fence portion 344 of each paddle assembly 40 . The fence portion 344 holds the overs 11 in place during the cutting process. As shown in FIG. 1 , the fence portion 344 is nearly radial with respect to the saw assembly. The nearly radial orientation of the fence portion 344 effectively holds the overs during cutting and helps resists the force imparted to the overs 11 by the rotating blades of the saw assembly 80 . The force imparted may include not only the force exerted by the blades themselves, but also the wind or airflow creating by the saw assembly 80 . The fence portion 344 also resists the wind force, which may be particularly helpful when processing small or lightweight overs 11 .
[0095] Each paddle assembly 40 may also include an outer paddle face 43 and a leading paddle edge 42 , as shown in FIG. 4 , in one embodiment. The outer paddle face 43 may act as the surface which traces and nearly coincides with the feeder zone 320 . The outer paddle face 43 may also nearly coincide with the inner face 53 of the dam 50 as the paddle assemblies 40 moves along the feeder path. In conjunction with the leading paddle edge 42 , each paddle assembly 40 fits closely against the dam 50 .
[0096] The dam 50 in one embodiment may include an inner face 53 positioned toward the feeder assembly 20 and shaped to nearly match the feeder zone 320 . The dam 50 may have a leading edge 52 and a trailing edge 54 . The leading edge 52 is described as leading in reference to the direction of rotation of the feeder assembly 20 . In other words, the first edge met by the approaching paddle assembly 40 is the leading edge 52 of the dam 50 . Accordingly, the last edge is referred to as the trailing edge 54 .
[0097] The outer paddle face 43 and the leading paddle edge 42 may also pass very close to the lower edge 64 of the chute 60 in one embodiment. The lower chute edge 64 may nearly coincide with the trailing dam edge 54 so that, for example, none of the overs 11 pass between the chute 60 and the dam 50 . In one embodiment where the dam 50 is stationary and the chute 60 may be moved with respect to the feeder assembly 20 , the geometry of the lower chute edge 64 and the trailing dam edge 54 may be coordinated to avoid any interference between the dam 50 and the chute 60 when the chute 60 is in motion.
[0000] 5. Automatic Redirection of Overs
[0098] Referring still to FIG. 4 , in one embodiment where the chute 60 may be moved with respect to the feeder assembly 20 , the position of the lower chute edge 64 nearly intersecting tangentially the feeder zone 320 represents one indication that the chute 60 is in the engaged position.
[0099] In one embodiment where the dam 50 is stationary and the chute 60 may be moved with respect to the feeder assembly 20 , the position of the lower chute edge 64 near the trailing dam edge 54 represents another indication that the chute 60 is in the engaged position.
[0100] The apparatus 10 of the present invention, in one embodiment, includes a chute 60 that may be placed in at least two positions: an engaged position 67 (as shown in FIG. 1 ) and a disengaged position 68 (as shown in FIG. 6 ). Generally, from the engaged position 67 , overs 11 are being guided into the feeder assembly 20 . From the disengaged position 68 , overs 11 are being guided away from the feeder assembly 20 .
[0101] FIG. 6 shows the chute 60 in a disengaged position 68 . In the embodiment shown, the chute 60 is articulated about a hinge 62 , although other types of connections are contemplated. A chute actuator 65 may be provided to move the chute 60 to a desired position. In use, a chute actuator 65 may be a pneumatic or hydraulic cylinder, a chain drive, or any other motive means.
[0102] Moving the chute 60 to a disengaged position 68 ends the guidance of overs 11 toward the feeder assembly 20 and/or actively re-directs the flow of overs 11 away from the feeder assembly 20 . In one embodiment, the overs 11 may be collected and re-cycled back to a position before the apparatus 10 , where the overs 11 may re-enter the flow and eventually re-enter the apparatus 10 .
[0103] The chute 60 may be disengaged for any of a variety of conditions. In one embodiment, the apparatus 10 of the present invention includes a master controller 200 and a plurality of sensors, as shown schematically in FIG. 5 . The master controller 200 may be an analog or digital Programmable Logic Controller (PLC), a discrete logic system such as an Application-Specific Integrated Circuit (ASIC), or other programmed logic device. The master controller 200 may be used to receive sensor data and send signals to other controllers and assemblies, including on/off signals, timed notifications, and logic results. A master controller 200 in general may be programmed for on/off control, timing, logic, counting, and sequencing between and among multiple machines and elements in a system. A master controller 20 may use ladder logic, sequential function tables, software, databases, structured text, and/or any other type of programming capable of executing the desired instructions.
[0104] The master controller 200 may include one or more separate controllers for different elements, such as the ones shown in FIG. 5 : a chute controller 260 , a topper controller 270 , a saw controller 280 , and a feeder controller 220 . Also, the apparatus 10 of the present invention may include a chute actuator 65 , a topper drive assembly 75 , a saw drive assembly 85 , and a feeder drive assembly 25 .
[0105] The master controller 200 may receive input signals from one or more discrete sensors, including a feeder load sensor 26 , a saw load sensor 86 , a topper load sensor 76 . For an element driven by a motor, a load sensor may be installed such that it senses the amperage on the motor. A higher amperage may indicate an excessive drain on the motor, which in turn may indicate an excessive load. Similarly, a lower amperage may indicate a reduced or minimum load on the motor. In one embodiment of the present invention, the feeder load sensor 26 , saw load sensor 86 , and topper load sensor 76 are connected to the feeder drive assembly 25 , saw drive assembly 85 , and topper drive assembly 75 , respectively, and configured to sense the load on the respective motors. If the load sensed exceeds a set maximum, the load sensor sends a fault signal to the master controller 200 .
[0106] A master controller 200 may be programmed with rules to execute in response to any variety of conditions or modes, including normal, fault, emergency, slow, pause, or any combination of such modes. Also, for example, any variety of situations may represent a fault condition. Different situations may be programmed in the master controller 200 by writing instructions according to the logic rules governing the controller. Fault conditions may include jammed equipment, an undesirable object such as metal in the incoming flow, an overloaded motor or drive assembly, an under-loaded motor or drive indicating equipment is empty, or any combination of these factors on different elements or machines. A fault condition may also occur in response to a human input, such as pressing a fault button. The timing element in the master controller 200 allows a system to update its status based upon signals received when conditions change.
[0107] The master controller 200 may also receive input signals from a chute load sensor 66 . In one embodiment, the chute load sensor 66 may be a metal detector. If metal is detected anywhere in the incoming flow of overs 11 , the chute load sensor 66 may send a fault signal to the master controller 200 .
[0108] In response to a fault signal from any load sensor 26 , 86 , 76 , 66 , the master controller 200 may be programmed to send a signal directing the chute actuator 65 to move the chute 60 to a disengaged position. With the chute disengaged, as shown in FIG. 6 , the overs 11 may be allowed to fall outside the feeder assembly 20 . The master controller 200 may also be programmed to reverse the direction of rotation of the feeder assembly 20 , in order to unload all the overs 11 .
[0109] Disengaging the chute 60 in response to a fault condition prevents the introduction of additional overs 11 into the apparatus 10 . Reversal of the feeder assembly 20 in response to a fault condition unloads the current overs 11 from the apparatus 10 .
[0110] In a fault condition, the feeder assembly 20 may rotate in this reversed direction until the feeder load sensor 26 reading indicates an empty condition, whereupon the master controller 200 may be programmed to return the apparatus 10 to normal operating mode.
[0000] 6. Rest Mode
[0111] In one embodiment, the master controller 200 may be programmed to halt or pause the apparatus 10 when sensors indicate the incoming flow of overs 11 has stopped. In one embodiment of the present invention, the feeder load sensor 26 , saw load sensor 86 , and topper load sensor 76 are connected to the feeder drive assembly 25 , saw drive assembly 85 , and topper drive assembly 75 , respectively, and configured to sense the load on the respective motors. A low amperage on a motor may indicate a reduced or minimum load on the motor. If the load sensed is less than a set minimum, indicating the apparatus 10 is empty of overs, the load sensor sends a fault signal to the master controller 200 . In response, the master controller 200 may be programmed to stop driving and/or brake the active elements of the apparatus 10 .
[0112] The master controller 200 may be programmed to return the apparatus 10 to normal operating mode if and when a signal from any load sensor indicates the presence of overs 11 to be processed.
[0000] 7. A Method
[0113] The present invention also provides a method of processing wood chips. In one embodiment, a method generally includes directing a flow of overs 11 along a feeder path and into and a saw assembly 80 . The method may include providing a feeder assembly to direct the overs 11 along the feeder path. The method may further include positioning a topper assembly 70 within the feeder path but in advance of the saw assembly 80 , such that the topper assembly 70 removes complete overs 11 or otherwise reduces any portion of the overs 11 that may tend to extend into a shaft interference zone 382 .
[0114] The method of the present invention may also include positioning the saw assembly 80 such that the shaft interference zone 382 nearly intersects tangentially with a feeder zone 320 . The method may further include positioning the topper assembly 70 such that the topper zone 370 nearly intersects tangentially with the feeder zone 320 .
[0115] An additional step may include equipping the feeder assembly 20 with one or more paddle assemblies 40 , each having an array of slots 45 therethrough positioned to accept insertion of the array of blades 83 . In another aspect of this step, the method may include shaping each paddle assembly 40 such that it aligns the overs 112 generally transverse to the array of blades 83 in preparation for cutting. Shaping each paddle assembly 40 may include providing a scoop portion shaped to cradle the overs 11 substantially within each paddle assembly and providing a fence portion shaped to contain the overs 11 substantially within each paddle assembly during cutting.
[0116] In one embodiment, the method may include mounting the paddle assemblies 40 to an endless chain driven along an endless feeder path about one or more powered rollers. The endless feeder path may include one or more either straight or curved segments.
[0000] 8. Conclusion
[0117] The described embodiments of the invention are intended to be merely exemplary. Numerous variations and modifications will be apparent to those skilled in the art. All such variations and modifications are intended to fall within the scope of the present invention as defined in the appended claims.
[0118] What has been described above includes several examples. It is, of course, not possible to describe every conceivable combination of components or methodologies for purposes of describing the systems, methods, computer readable media and so on employed in planning routes. However, one of ordinary skill in the art may recognize that further combinations and permutations are possible. Accordingly, this application is intended to embrace alterations, modifications, and variations that fall within the scope of the appended claims. Furthermore, the preceding description is not meant to limit the scope of the invention. Rather, the scope of the invention is to be determined only by the appended claims and their equivalents.
[0119] While the systems, methods, and apparatuses herein have been illustrated by describing examples, and while the examples have been described in considerable detail, it is not the intention of the applicants to restrict or in any way limit the scope of the appended claims to such detail. Additional advantages and modifications will be readily apparent to those skilled in the art. Therefore, the invention, in its broader aspects, is not limited to the specific details, the representative systems and methods, or illustrative examples shown and described. Accordingly, departures may be made from such details without departing from the spirit or scope of the applicant's general inventive concepts. | Apparatuses, methods, and systems for producing wood chips are disclosed. The disclosure in one embodiment produces smooth wood chips of generally uniform size and shape, suited for use in making paper, cardboard, and other recyclable materials. In one embodiment, an apparatus is disclosed for collecting, aligning and guiding wood scraps through an array of spaced-apart saw blades using a feeder assembly operating on a continual basis. The feeder assembly in one embodiment includes one or more paddle assemblies shaped to align and guide the wood scraps along a feeder path toward the saw blades. A system for controlling an apparatus is also disclosed. A method for reducing wood scraps into cut chips is also disclosed. This Abstract is provided to comply with the rules, which require an abstract to quickly inform a searcher or other reader about the subject matter of the application. This Abstract is submitted with the understanding that it will not be used to interpret or limit the scope or meaning of the claims. | 3 |
CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] This application claims priority under 35 U.S.C. §119 to European Patent Application No. 13159415.2, filed Mar. 15, 2013.
BACKGROUND
[0002] The present invention relates to transporting goods. In particular, the invention relates to dollies, on which parceled goods are transported and stored temporarily. To be precise, the invention relates to a dolly according to the preamble portion of claims.
[0003] There is known a vast variety of different devices used for transporting parceled goods. Typically pieces or stacks thereof are loaded onto a wheeled platform, on which they are conveyed to shop floor or storage. These wheeled platforms are called dollies. Some dollies are equipped with a tow bar and a corresponding hitch for transporting a plurality of dollies in a chained fashion. When the tow bar for pulling the dolly is temporarily not used, it is typically pivoted in an upright position for saving space. U.S. Pat. No. 4,856,810 proposes one solution to providing a space saving tow bar for a dolly.
[0004] Conventional pivoting tow bars, however, occupy valuable space, when the dolly is in transit, for example. When the dolly is loaded onto a trailer such that the tow bar is not used for a long period of time, the folded tow bar uses excess space. This problem has previously been solved by providing couplings between the dolly and the tow bar, whereby the tow bar may be detached for transit. Detachable tow bars, on the other hand, are un-ideal for the reason that the detached tow bars must be handled separately and the coupling typically increases the complexity of the device and therefore reduces its robustness and user-friendliness required for logistics equipment.
[0005] It is therefore an aim of the present invention to provide an improved dolly which is not only effective in terms of return logistics but also simple in design and easy to use.
SUMMARY
[0006] The aim of the present invention is achieved with aid of a novel dolly for transporting items loaded thereon. The dolly includes a chassis which has an upper side with a load carrying surface, and an opposing underside. The dolly also includes a tow bar which is arranged slidably to the underside of the chassis via a pivoting mechanism which is configured to pivot the tow bar about a horizontal axis. The chassis of the dolly includes a corresponding hitch, which allows pivoting action about a vertical axis between the tow bar and the hitch.
[0007] Considerable benefits are gained with aid of the present invention.
[0008] By virtue of the slidable and pivotable connection between the tow bar and the chassis of the dolly, the tow bar may not only be guided to a towing and parking positions, the tow bar may also be guided to a retracted position. In the retracted position the tow bar is completely retracted under the load carrying surface of the dolly, wherein the external dimensions of the dolly are minimized for individual transport and storage of the dolly.
[0009] Other objects and features of the invention will become apparent from the following detailed description considered in conjunction with the accompanying drawings. It is to be understood, however, that the drawings are intended solely for purposes of illustration and not as a definition of the limits of the invention, for which reference should be made to the appended claims.
BRIEF DESCRIPTION OF THE SEVERAL VIEWS OF THE DRAWINGS
[0010] In the following, exemplary embodiments of the invention are described in greater detail with reference to the accompanying drawings in which:
[0011] FIG. 1 presents an upper isometric view of a dolly with a tow bar in a towing position according to one embodiment.
[0012] FIG. 2 presents an upper isometric view of the dolly of FIG. 1 with the tow bar in a retracted position.
[0013] FIG. 3 presents a lower isometric view of the dolly of FIG. 1 .
[0014] FIG. 4 presents a lower isometric view of the dolly of FIG. 2 .
[0015] FIG. 5 presents a lower isometric view of the dolly of FIG. 1 with the tow bar raised to an upright position.
[0016] FIG. 6 presents a top elevation view of the dolly of FIG. 1 .
[0017] FIG. 7 presents a cross-sectional view taken along the line B-B of FIG. 6 .
[0018] FIG. 8 presents a detail view of area C of FIG. 7 .
[0019] FIG. 9 presents an elevated frontal view of the dolly of FIG. 1 .
[0020] FIG. 10 presents a detail view of the pivoting mechanism denoted A in FIG. 9 .
[0021] FIG. 11 presents a rear bottom isometric view of the dolly of FIG. 5 .
[0022] FIG. 12 presents a detail view of the pivoting mechanism denoted A in FIG. 11 .
[0023] FIG. 13 presents an upper isometric view of two dollies as shown in FIG. 1 being hitched to a dolly as shown in FIG. 5 .
DETAILED DESCRIPTION
[0024] The tow bar 120 of the dolly 100 according to the illustrated example may be guided into three main attitudes. In this context the term dolly is meant to refer to a cart-like dolly as described in engineering standard EN 12674-1. FIGS. 1 , 3 and 6 to 10 show the tow bar 120 in a substantially horizontal towing position, where the tow bar 120 is arranged to the first end 101 of the dolly 100 to be engaged with a hitch 190 of a towing dolly or tractor (cf. FIG. 13 ). The dolly 100 as shown in the Figures may be an intermediate link in a chain of dollies 100 , but it may also serve as a tractor, wherein the handle 180 may be used to haul the combination of dollies. The handle 180 has substantially the shape of the letter A, wherein joints has been provided in the top region of the handle 180 for turning the top end of the handle 180 horizontally thus creating a gripping clearance for hands.
[0025] FIGS. 5 , 11 and 12 show the tow bar 120 in a substantially vertical position, where the tow bar 120 is arranged to the same first end of the dolly 100 but pivoted in an upright parking position. The parking position is used for short-term storage of the dolly 100 , whereby the tow bar 120 is turned into the vertical orientation for mainly safety purposes but also to save space.
[0026] FIGS. 2 and 4 show the tow bar 120 in a retracted position, where the tow bar 120 is retracted from the first end 101 towards the opposing second end 102 . When in the retracted position, the tow bar 120 does not occupy the space in front of the first end 101 of the dolly 100 thereby saving crucial centimeters in the external dimensions of the dolly 100 . The retracted position is especially advantageous when dollies 100 are transported individually, i.e. not coupled to each other, in a trailer for example. As compared to the parking position, the tow bar 120 and the pivoting mechanism 130 are completely removed from the first end 101 of the dolly 100 resulting in the desired saving in the outer dimensions of the dolly 100 .
[0027] Next, the construction according to one embodiment which enables this function is discussed in greater detail.
[0028] As is the case with conventional dollies, the dolly 100 according the illustrated embodiment features a chassis 100 with a load carrying surface 113 for receiving said items. The load carrying surface 113 is considered to define the upper side 111 of the chassis 100 , whereas the castors and such are arranged to the opposing underside 112 of the chassis 100 . In the illustrated example, the load carrying surface 113 is uncovered, but according to an alternative embodiment, the load carrying surface 113 may have a veneer cover, a crate or similar tray for the loaded items. When the tow bar 120 is in the retracted position, it is covered by said load carrying surface 113 .
[0029] As best shown in FIGS. 3 to 5 and 11 , the dolly 100 includes a guide track 140 which is provided to the underside 112 of the dolly 100 . The guide track 140 runs in the main traveling direction of the dolly 100 , i.e. between the first and second end 101 , 102 of the dolly thus connecting the front and rear of the dolly 100 . In the illustrated example, the guide track 140 is formed of two opposing profiles which are arranged at a distance from one another. The profiles of the guide track 140 are therefore separated by a distance which extends in the orthogonal horizontal direction in respect to the main traveling direction of the dolly 100 . The profiles of the guide track 140 exhibit a cross-section which have substantially the shape of the letter C. A portion of the guide track 140 nearest to the second end 102 of the dolly 100 is protected by a shield 160 , which is fixed to the underside 112 of the chassis 100 .
[0030] The guide track 140 provides a running path for a tow bar assembly including the tow bar 120 as well as a guide block 150 , which is arranged to run in the guide track 140 , and a pivoting mechanism 130 which connects the tow bar 120 to the guide block 150 in a pivoting manner. Generally speaking, tow bar 120 is arranged slidably to the underside 112 of the chassis 110 via the pivoting mechanism 130 which, on the other hand, is configured to pivot the tow bar 120 about a horizontal axis. More precisely, the pivoting mechanism 130 is configured to be moved along the guide track 140 via the guide block 150 which is arranged slidably to the guide track 140 , namely between the two opposing profiles of the guide track 140 . The guide block 150 extends along the main traveling direction of the dolly 100 , i.e. along the guide track 140 , which has a stabilizing effect on the movement of the tow bar assembly. The guide block 150 according to the illustrated embodiment has been lightened to resemble the letter H for weight saving reasons. The function of the cooperation of the guide block 150 and guide track 140 is therefore to provide a stabile sliding connection between the tow bar 120 and the chassis 110 of the dolly 100 . While the guide block 150 is designed to remain in a fixed angular position in respect to the vertical axis, the angular movement between consecutive dollies 100 is provided between rotation between the hitch coupling 121 of the tow bar and the cooperating hitch 190 .
[0031] According to an alternative embodiment (not shown), the guide is formed by means of a unitary profile shaped such as to receive the tow bar 120 in a similar sliding manner as the illustrated embodiment. In said alternative embodiment, the top of the profile is shaped to be attached to the underside of the dolly, wherein the inner surface of the profile is shaped to receive the guide block. Therefore the inner surface of the profile is adapted to receive the guide block in a sliding manner and the outer surface of the profile is adapted to provide a protective enclosure for the tow bar assembly including the tow bar, pivoting mechanism and the guide block.
[0032] Turning now to FIGS. 3 , 5 and 7 to 12 which illustrate the construction and function of pivoting mechanism 130 connecting the tow bar 120 to the guide block 150 in a hinge-like manner. Fixed to the under surface of the guide block 150 are two distanced axle brackets 135 having aligned openings through which an axle 131 has been arranged to connect the brackets 135 in a horizontal direction transversal to the main traveling direction of the dolly 100 . The axle 131 therefore forms the axis of revolution of the tow bar 120 . A protective profile 161 is provided to the first end 101 of the dolly 100 to cover the pivoting mechanism 130 and to act as a fixing point for a hitch 190 .
[0033] On the axle 131 a swing member 136 has been provided in a rotatable manner. The swing member 136 is connected to the tow bar 120 such that the tow bar 120 extends from the swing member 136 so as to allow the tow bar 120 to be pivoted about the axle 131 . The swing member 136 has a shape resembling the letter C, wherein the distal ends of the member feature male locking pieces 132 which are adapted to lock into to receptive openings 171 of a locking plate 170 which is provided to the first end 101 of the dolly 100 on top of the guide track 140 . Alternatively, the receptive openings 171 may be provided to beams or other structures making up the chassis 110 of the dolly 100 . The male locking pieces 132 are protuberances extending from the swing member 136 and form the male pieces of the locking interface between the swing member 136 and the locking plate 170 whose receptive openings 171 form the female counterpart in the locking interface. The swing member 136 is shown in the vertical position in FIGS. 11 and 12 , wherein the tow bar 120 is in a vertical, i.e. upright position. When the tow bar 120 is pivoted into the horizontal towing position, the swing bar 136 is similarly rotated about the axle 131 into the horizontal position, wherein the male pieces 132 engage with the openings 171 of the locking plate 170 . In this configuration, the locking interface 132 , 171 between the swing member 136 and the locking plate 170 ensure that the tow bar 120 does not slide backwards into the retracted position (cf. FIG. 4 ).
[0034] Referring now specifically to FIGS. 10 and 12 which show that the pivoting mechanism 130 is configured to bias the tow bar 120 to an upright position about a horizontal axis transversal to the main traveling direction of the dolly 100 . More specifically, the swing member 136 is biased toward the horizontal position by means of a biasing spring 134 arranged around the axle 131 between the swing member 136 and the guide block 150 . With aid of the biasing spring the tow bar 120 is suspended such to create a tendency to pivot to the vertical position in order to aid the hitch coupling 121 at the distal end of the tow bar 120 to remain in contact with the cooperating hitch 190 ( FIG. 13 ). It is to be noted that the additional hitch seen in FIG. 10 , for example, is not intended to couple to a hitch coupling 121 as seen on the tow bar 120 but to another coupling outside the scope of the present invention.
[0035] The biasing spring 134 has an additional function. Once the tow bar 120 has been slid into the retracted position (cf. FIGS. 2 and 4 ), the tow bar is biased upward, wherein the opening, i.e. the hitch coupling 121 , in the distal end of the tow bar 120 engages with a corresponding locking means 114 of the chassis 100 . The locking means 114 may, for example, be a protruding screw head of a screw used in the assembly of the chassis. The cooperation between the locking means 114 and the hitch coupling 121 is best shown in FIG. 4 .
[0036] The pivoting mechanism 130 further includes an angle limiting spring 133 which takes the form of an elastic conical stopper which protrudes orthogonally from the swing member 136 toward the second end 102 or guide block 150 of the dolly 100 depending on the angular position of the swing member 136 . The angle limiting spring 133 is configured to engage with the guide block 150 when the swing member 136 and particularly the tow bar 120 is pivoted into the horizontal position (cf. FIG. 8 ). Once the angle limiting spring 133 has made contact with the guide block 150 , the angle of the tow bar 120 around the axle 131 and in respect to the chassis 100 is limited. Due to the compression elasticity of the angle limiting spring 133 , the terminal end of the tow bar 120 may be pressed downwards in order to fit the hitch coupling 121 to the cooperating hitch 190 ( FIG. 13 ). This downward orienting force on the tow bar side of the axle 131 is inverted into an upward orienting force at the angle limiting spring 133 on the opposite side of the axle 131 , wherein the angle limiting spring 133 compresses elastically thus providing suspended angular latitude for the tow bar 120 . The same function is used in on the one hand locking the hitch coupling 121 to the locking means 114 of the chassis 100 and on the other hand for releasing the hitch coupling 121 from the locking means 114 (cf. FIG. 4 ).
[0037] Thus, while there have been shown and described and pointed out fundamental novel features of the invention as applied to a preferred embodiment thereof, it will be understood that various omissions and substitutions and changes in the form and details of the method and device may be made by those skilled in the art without departing from the spirit of the invention. For example, it is expressly intended that all combinations of those elements which perform substantially the same results are within the scope of the invention. Substitutions of the elements from one described embodiment to another are also fully intended and contemplated. It is also to be understood that the drawings are not necessarily drawn to scale but they are merely conceptual in nature. It is the intention, therefore, to be limited only as indicated by the scope of the claims appended hereto. | The present invention provides an improved dolly which is not only effective in terms of return logistics but also simple in design and easy to use. The novel dolly includes a chassis, which has an upper side with a load carrying surface, and an opposing underside. The dolly also includes a tow bar, which is arranged slidably to the underside of the chassis via a pivoting mechanism, which is configured to pivot the tow bar about a horizontal axis. The chassis of the dolly includes a corresponding hitch, which allows pivoting action about a vertical axis between the tow bar and the hitch. | 1 |
FIELD OF THE INVENTION
This invention relates to the structure of a cylinder head assembly, and more particularly to the structure of a cylinder head assembly in which air generated in an oil passageway is prevented from being supplied to those parts which require lubrication, and in which a lubrication oil is effectively utilized, machining efficiency is good, the number of parts is prevented from being increased, and a camshaft housing is improved in rigidity.
BACKGROUND OF THE INVENTION
In an engine, lubrication is applied to those parts of a cylinder block and a cylinder head, which require lubrication, in order to maintain the functions of such parts. Specifically, as shown in FIG. 13, an engine 102 comprises a cylinder block 104, a crank lower case 106, an oil pan 108, a cylinder head 110, and a cylinder head cover (not shown) for defining a cam chamber when placed on the cylinder head 110. Between the cylinder block 104 and the crank lower case 106, a crankshaft 112 is axially supported. On an upper part of the cylinder head 110, an inlet side and an outlet side are coacted with a camshaft housing (not shown) having an integral structure therewith, and a first-side camshaft 114 located on one side, as well as a second-side camshaft (not shown) located on the other side, is axially supported. The rotations of the first-side camshaft 114 and the second-side camshaft (not shown) actuate a first-side hydraulic adjuster (HLA) 116 located on one side of the cylinder head 110 and a second-side hydraulic adjuster (not shown) located on the other side to cause an inlet valve 118 and an outlet valve (not shown) to move reciprocally. The first-side hydraulic adjuster 116 is provided with a high pressure chamber 116a.
In order to feed lubrication oil to the engine 102, an oil pump 120 is mounted on the crank lower case 106. The oil pump 120 draws the lubrication oil in the oil pan 108 from an inlet tube 124 though a strainer 122, and feeds it, under pressure, to those parts which require lubrication, such as the first-side hydraulic adjuster 116, the second-side hydraulic adjuster, a cam journal (not shown) of the camshaft housing via first and second block side oil passageways 126 and 128 which are formed in the cylinder block 104 and first and second head side oil passageways 130 and 132 which are formed in the cylinder head 110. By this, lubrication is applied to various parts of the engine 102.
A structure of a cylinder head of this type is disclosed, for example, in Japanese Laid-Open Patent Application No. Hei 1-253552. As shown in FIG. 14, the structure described in this official publication has an oil feed passageway 204 formed in a generally central part of a cylinder head 202 of an engine, the oil feed passageway 204 being in communication with a reserve chamber 206 formed in an upper part of the cylinder head 202, the reserve chamber 206 being, in turn, communicated with an adjuster oil passageway 210 which is in communication with an adjuster guide portion 208 and a second-side adjuster oil passageway 214 which is in communication with a second-side adjuster guide portion 212. A plug 216 for sealing the reserve chamber 206 is formed with an air removing hole 218 for discharging air (air bubble) generated in the oil passageways.
Incidentally, in the structure of a cylinder head according to the prior art, if air (air bubble) is contained in the lubrication oil in the oil passageways, which is fed under pressure by an oil pump, the lubrication oil is supplied to those parts which require lubrication such as a hydraulic adjuster, etc., together with this air. In this way, when the air-containing lubrication oil is supplied, for example, to the hydraulic adjuster, the air enters the high pressure chamber of the hydraulic adjuster to create a sponge-like condition. As a result, a foreign sound is generated in the engine due to poor operation of the hydraulic adjuster. When the engine is operated for a long time or at a high speed in such a condition as just mentioned, the hydraulic adjuster, the inlet valve, etc. are damaged.
Therefore, in order to obviate the above inconveniences, according to the present invention there is firstly provided a structure of a cylinder head assembly having a camshaft axially supported by a cylinder head through a camshaft housing and a head oil passageway for guiding a lubrication oil to those parts of the cylinder head which require lubrication, the structure of the cylinder head assembly being characterized in that the camshaft housing is provided with an oil reserve chamber communicating with the head oil passageway.
Secondly, there is provided a structure of a cylinder head assembly having a camshaft axially supported by a cylinder head through a camshaft housing and a head oil passageway for guiding a lubrication oil to those parts of the cylinder head which require lubrication, the structure of the cylinder head assembly being characterized in that the camshaft housing is provided with an oil reserve chamber communicating with the head oil passageway, one end of a through-passageway being communicated with an upper part of the oil reserve chamber and the other end thereof being communicated with a camshaft journal of the camshaft housing.
According to the construction of the present invention, firstly, since the oil reserve chamber is formed in the camshaft housing, the number of parts can be avoided from increasing, the camshaft housing can be improved in rigidity, and machinability can be improved.
Secondly, the air, which remains in an upper part of the oil reserve chamber due to stopping of the engine, is supplied to the camshaft journal side via the through-passageway when the engine is driven. As a result, the air is not supplied to such parts as the hydraulic adjuster, etc., and therefore the functions of the parts such as the hydraulic adjuster, etc. are maintained in a favorable condition to ensure a favorable operation of the engine. Furthermore, since the through-passageway acts as means for removing the air in the oil reserve chamber and feeding the lubrication to the camshaft journal, the lubrication oil can be effectively utilized.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is an enlarged cross-sectional view taken on line 1--1 of FIG. 3.
FIG. 2 is a schematic end elevational view of a construction of an engine.
FIG. 3 is a side view of a cylinder head.
FIG. 4 is a plan view of a cylinder head.
FIG. 5 is a cross-sectional view taken on line 5--5 of FIG. 3.
FIG. 6 is a right end view of the cylinder head when viewed in a direction as indicated by an arrow 4 of FIG. 4.
FIG. 7 is a plan view of a camshaft housing.
FIG. 8 is a cross-sectional view taken on line 8--8 of FIG. 7.
FIG. 9 is a cross-sectional view taken on line 9--9 of FIG. 7.
FIG. 10 is a right side view of the camshaft housing of FIG. 7.
FIG. 11 is a bottom view of the camshaft housing of FIG. 7.
FIG. 12 is a left side view of the camshaft housing of FIG. 11.
FIG. 13 is a schematic view of a construction of an engine according to the prior art.
FIG. 14 is a cross-sectional view of a cylinder block according to the prior art.
DETAILED DESCRIPTION
FIGS. 1 through 12 show one embodiment of the present invention. In FIG. 2, reference numeral 2 denotes an engine; 4 a cylinder block; 6 a crank lower case; 8 an oil pan; and 10 a cylinder head. As shown in FIG. 1, the cylinder head 10 is tightly secured to the cylinder block 4 by head tightening bolts 12. Between the cylinder block 4 and the crank lower case 6, a crankshaft 14 is axially supported. A cylinder head cover (not shown) is placed on the cylinder head 10.
The crank lower case 6 is provided with an oil pump 16. This oil pump 16 has a pump shaft 18 and a pump sprocket 20 mounted on the pump shaft 18. The pump sprocket 20 is engaged with a pump driving chain 22, which drives a pump driving sprocket (not shown) which is mounted on the crankshaft 14.
As shown in FIGS. 2-6, first-side and second-side camshaft bearing portions 24 and 26, which are directed in a longitudinal direction X (FIGS. 3 and 4) and spaced apart a predetermined distance from each other in a width direction Y, are formed on an upper part of the cylinder head 10. Between the first-side and second-side camshaft bearing portions 24 and 26, a plurality of spark plug holes 28 are formed in such a manner as to be spaced apart a predetermined distance in the longitudinal direction X as shown in FIG. 4.
As shown in FIG. 5, a plurality of chambers 30 are formed in a lower part of the cylinder head 10 in such a manner as to correspond to the respective spark plug holes 28.
First-side and second-side camshafts 32 and 34 are placed respectively on the first-side and second-side camshaft bearing portions 24 and 26. These camshafts 32 and 34 are axially supported by a camshaft housing 36 from above.
As shown in FIGS. 1 and 2, the camshaft housing 36 is formed with first-side and second-side camshaft journals 38 and 40 adapted to axially support the first-side and second-side camshafts 32 and 34, respectively, and an inlet side and an outlet side are of an integral structure.
As shown in FIGS. 9 and 10, the camshaft housing 36 is further formed with an oil reserve chamber 42 generally at a central part thereof which is open to a housing bottom face 36d. As seen, this oil reserve chamber 42 is of the type which is not open to the camshaft chambers.
As shown in FIG. 9, the camshaft housing 36 is proved with one end of a first-side through-passageway 44 which is in communication with an upper part 42a of the oil reserve chamber 42. The other end of the first-side through-passageway 44 is formed obliquely below in such a manner as to be directed toward the first-side camshaft journal 38. The first-side through-passageway 44 is formed by drilling or the like from the first-side camshaft journal 38 side. The camshaft housing 36 is provided with one end of a second-side through-passageway 46 which is in communication with the other side of the upper part 42a of the oil reserve chamber 42. The other end of the second-side through-passageway 46 is formed obliquely below in such a manner as to be directed toward the second-side camshaft journal 40. This second-side through-passageway 46 is formed by drilling or the like from the second-side camshaft journal 40 side.
The cylinder head 10 as shown in FIG. 1 is formed with a first-side hydraulic adjuster (HLA) (not shown), one side of a second-side hydraulic adjuster (HLA) 48 and adjuster guide portions 50 and 52 in such a manner as to correspond to the first-side and second-side camshaft bearing portions 24 and 26, respectively. The hydraulic adjusters 48 such as are operated to convert the rotational motions of the first-side and second-side camshafts 32 and 34 to linear motions to respectively activate an inlet valve (not shown) and an outlet valve 54. A high pressure chamber 48a is formed within the hydraulic adjuster 48.
As shown in FIG. 1, the cylinder head 10 is provided with an oil tube 58 which extends longitudinally and forms a head main oil passageway 56. In order to communicate this head main oil passageway 56 with the oil reserve chamber 42, an upper part of the cylinder head 10 is formed with a head oil chamber 60 which is in direct communication with the oil reserve chamber 42. Formed in the oil tube 58 is a tube penetration hole 62 which is in communication with a lower part of the head oil chamber 60 and also with the head main oil passageway 56.
First-side and second-side adjuster oil passageways 64 and 66 are at one end in communication with the first-side and second-side adjuster guide portions 50 and 52 respectively, and at the other end are in communication with the head main oil passageway 56.
The cylinder head 10 is formed with a head oil passageway system 68 (FIG. 1) to guide the lubrication oil from the oil pump 16 to the oil reserve chamber 42 formed in the camshaft housing 36. The head oil passageway system 68 comprises an upper head oil passageway 70 communicating with the oil reserve chamber 42 and directed downwardly therefrom, an intermediate head oil passageway 72 communicating with the lower end of upper head oil passageway 70, the passageway 72 being directed in the width direction Y and formed obliquely below the passageway 70, and a lower head oil passageway 74 communicating with the intermediate head oil passageway 72 and directed downwardly. The upper head oil passageway 70 is formed by drilling or the like from above the cylinder head 10. The intermediate head oil passageway 72 is formed by drilling or the like from one lower side in the width direction Y.
As shown in FIG. 2, the cylinder block 4 is formed with a block oil passageway system 78 which is in communication with passageway 74 of the head oil passageway system 68. The block oil passageway system 78 comprises an upper block oil passageway 80 which is in communication with the lower side head oil passageway 74 and a lower block oil passageway 82 communicating with the upper block oil passageway 80 and directed toward the crankshaft 14 side.
Owing to the above arrangement, the lubrication oil from the oil pump 16 is supplied to the oil reserve chamber 42 via the block oil passageway system 78 and head oil passageway system 68, and fed, under pressure, to the head main oil passageway 56, etc.
Next, the operation of the above embodiment will be described.
When the oil pump 16 is driven, the lubrication oil is fed to the oil reserve chamber 42 in the camshaft housing 36 via the block oil passageway system 78 and head oil passageway system 68.
In a normal time, the lubrication oil is fed from the oil reserve chamber 42 to the first-side and second-side camshaft journals 38 and 40 via the first-side and second-side through-passageways 44 and 46 to apply lubrication to the first-side and second-side camshaft journals 38 and 40.
In case air such as an air bubble enters the lubrication oil in the oil passageways such as the block oil passageway system 78 and head oil passageway system 68, etc., if the engine 2 is maintained in its stopping condition, the air stays in the upper part of the oil reserve chamber 42.
When the engine 2 is driven, the air at the upper part 42a of the oil reserve chamber 42 is supplied from the first-side and second-side through-passageways 44 and 46 to the first-side and second-side camshafts 38 and 40 together with the lubrication oil, and therefore, never flows toward the head main oil passageway 56 side.
As a result, since the air-contained lubrication oil is not supplied to the first-side and second-side adjuster guide portions 50 and 52, air does not enter the high pressure chambers 48a in the hydraulic adjusters 48. Accordingly, a favorable operation of the hydraulic adjusters 48 is available, the engine 2 is prevented from becoming abnormal, and the hydraulic adjusters 48, and the inlet valves and the outlet valves 54 are not broken even in the engine 2 is operated for a long time or at a high speed.
Since the first-side and second-side through-passageways 44 and 46 can be used both as air-removing passageways and lubrication oil passageways, the lubrication oil can be effectively utilized.
In case the through-passageways 44 and 46 are formed only for the purpose of removing air, it is usually necessary to set the diameter of these passageways small in order to avoid the lowering of hydraulic pressure. In this embodiment, machining efficiency of the camshaft housing 36 is favorable and a low cost is attainable.
Furthermore, since the oil reserve chamber 42 is formed generally in an intermediate part of the camshaft housing 36 with the inlet side and the outlet side being of an integral structure therewith, the number of parts can be avoided from increasing and the camshaft housing 36 can be improved in rigidity.
As apparent from the foregoing detailed description, according to the present invention, firstly owing to the arrangement in that the camshaft housing for axially supporting the camshaft is provided with the oil reserve chamber which is in communication with the head oil passageway, the number of parts can be avoided from increasing, the camshaft housing can be improved in rigidity, and machining efficiency can be improved.
Secondly, owing to the arrangement in that one end of the through-passageway is in communication with an upper part of the oil reserve chamber and the other end thereof is in communication with the camshaft journal of the camshaft housing, the air generated in the various oil passageways is not supplied to such parts as the hydraulic adjuster, etc., and the functions of the parts such as the hydraulic adjuster, etc. can be maintained in a favorable condition to ensure a favorable operation of the engine. Furthermore, since the through-passageway acts as a means for removing the air in the oil reserve chamber and feeding the lubrication oil to the cam journal, the lubrication oil can be effectively utilized.
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. | A cylinder head assembly having a camshaft axially supported by a cylinder head through a camshaft housing having a head oil passageway for guiding lubricating oil to those parts of the cylinder head which require lubrication. The camshaft housing is provided with an oil reserve chamber communicating with the oil head passageway. One end of a through-passageway communicates with an upper part of the oil reserve chamber, and the other end of this through-passageway communicates with a camshaft journal of the camshaft housing. | 5 |
BACKGROUND OF THE INVENTION
This invention relates to the production of levulinic acid.
Many common materials consist partially or fully of carbohydrates. For example, cellulose and starch are polymers made of carbohydrate molecules, predominantly glucose, galactose, or similar hexoses. When subjected to acid treatment, cellulose and starch split into hexose monomers. On continued reaction the hexose monomers then further degrade to hydroxymethylfurfural, and other reaction intermediates, which then further degrade to levulinic acid and formic acid. Levulinic acid can be used to make resins, plasticizers, specialty chemicals, herbicides and a fuel extender, methyltetrahydrofuran.
Many common waste materials include cellulose or starch. For example, primary sludges from paper manufacture, waste paper, waste wood (e.g., sawdust), as well as agricultural residues such as corn husks, corn cobs, rice hulls, straw, and bagasse, include high percentages of cellulose. Starch can be found in food processing waste derived, for example, from corn, wheat oats, and barley.
SUMMARY OF THE INVENTION
The invention features a process for producing levulinic acid from carbohydrate-containing materials in high yields using two reactors in which the temperature, reaction time, and acid content are closely controlled. According to the preferred process, a carbohydrate-containing material is supplied continuously to a first reactor and hydrolyzed at between 210° C. and 230° C. for between 13 seconds and 25 seconds in the presence of between 1% and 5% by weight mineral acid. The hydrolysis produces hydroxymethylfurfural, which is removed continuously from the first reactor and supplied continuously to a second reactor. In the second reactor, the hydroxymethylfurfural is hydrolyzed further at between 195° C. and 215° C. for between 15 minutes and 30 minutes to produce levulinic acid, which is continuously removed from the second reactor. The levulinic acid preferably is produced in at least 60%, and more preferably at least 70%, of the theoretical yield based on the approximate hexose content of the carbohydrate-containing material.
The levulinic acid preferably is removed from the second reactor as it is generated by drawing off liquid containing the levulinic acid from the reactor. Solid by-products can be removed from the levulinic acid-containing liquid by filtration or centrifugation.
In preferred embodiments, the first reactor is a tubular reactor that includes an entrance and an exit between which the reactor mixture passes without significant axial mixing.
The contents of the second reactor are mixed either by an agitator or by allowing the outflow from the first reactor to enter the second reactor below the level of the liquid in the second reactor. This provides excellent mixing in the second reactor without the need for an agitator.
Preferably the flow of the intermediate sample is controlled by a flow valve that maintains steady conditions in the first reactor, and the volume of reactants in the second reactor is controlled by removing a volume corresponding to the volume fed to the second reactor. The latter may be accomplished by an outflow control valve which acts to maintain steady conditions such as mass level in the second reactor. The temperature in the second reactor preferably also is maintained constant, for example, by the injection of steam into the reactor, or by using a vapour outflow throttling valve which maintains a constant pressure in the second reactor.
Using a continuous two-stage reactor system in which the products are continuously collected provides an efficient use of equipment and space since large quantities of the sample can be run through a relatively small system and conditions in each stage of reaction can be precisely controlled. The lack of axial mixing in the first reactor ensures that a given portion of the sample does not spend too much time in the first reactor. The hydrolysis conditions--temperature, reaction time, and acid content--provide a surprisingly high yield of levulinic acid. In addition, the continuous nature of the second stage allows good control of conditions in the second stage.
Other features and advantages of the invention will be apparent from the description of the preferred embodiment thereof, and from the claims.
BRIEF DESCRIPTION OF THE DRAWING
The FIGURE is a flow diagram illustrating the steps of a preferred process.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
Referring to the FIGURE, an aqueous acidified slurry 10 consisting of wastepaper fibers, paper sludge, sawdust, ground wood, ground corn, starch solution, or other carbohydrate feedstock in dilute mineral acid (e.g., sulfuric acid or hydrochloric acid) is pumped by a high pressure pump 12 into the entrance 14 of a tubular reactor 16. The acid may be premixed with the feed or injected by metering pump into the feedstream as it enters the first stage reactor. The temperature is maintained in the reactor at an elevated level by the injection of high pressure steam 18. The pressure in the reactor is maintained at a sufficient level to give rapid condensation of the steam and to prevent the reactor contents from vaporizing. The carbohydrate is degraded by the acid as the mixture passes through the reactor 16. The mixture flows in the axial direction along the reactor 16 such that the radial mixing is substantially greater than the axial mixing. The mixture flows out of the reactor through a variable orifice exit valve 21. The slurry may consist of 2% to 40% feed solids by weight; the quantity is limited only by the ability of the pump to feed the slurry.
While in the reactor 16 the carbohydrate material is degraded by the acid. Cellulose or starch, for example, in the feed degrade to hexose monomers and oligomers. Hemicellulose in the feed degrades to both hexose and pentose monomers and oligomers. The pentose monomers and oligomers are further degraded to furfural and the hexose monomers are further degraded to hydroxymethylfurfural.
The temperature in the first reactor preferably is 210° C. to 235° C. (more preferably 215° C. to °230 C.). If the temperature is too low, the acid degradation will not proceed at a fast enough rate. If the temperature is too high, too much pressure may be generate in the reactor and also, the first stage degradation may proceed too quickly.
The slurry preferably includes 1% to 5% (more preferably 1.5% to 3.5%) mineral acid by weight of the aqueous portion of the slurry. If too much acid is used, there may be corrosion problems with the equipment and the first stage degradation may proceed too quickly. If too little acid is used, the degradation may not proceed at a fast enough rate.
The amount of time the carbohydrate material spends in the reactor 16 should be about 13 seconds to 25 seconds (more preferably 13.5 seconds to 16 seconds). The material needs to have sufficient time to degrade, but the degradation products should not be exposed to elevated temperatures for an extended period or substantial unwanted decomposition of the products may occur.
The reaction mixture flows from reactor 16, through a pressure control valve 21, and into a tank-type reactor 22, which can be equipped with a stirrer to improve mixing. The temperature, mineral acid concentration, and average residence time of a volume of the mixture in the second reactor are selected so that the remaining hexose monomers, if any, are converted to hydroxymethylfurfural, and the hydroxymethylfurfural is further degraded to levulinic acid and any unreacted feed is converted to hexose which is then converted to levulinic acid. In addition, the conditions are adjusted so that any furfural and formic acid present vaporize quickly. The vapor 24 produced exits the reactor 22 and is externally condensed. The levulinic acid settles to the bottom of the reactor 22 with other liquids, and is continuously drawn off in liquid stream 26. For a given time period the volume removed from the reactor 22 should equal the volume of the reaction mixture added to the reactor 22 from the first reactor 16. Lignin or other solids leave the second reactor 22 in stream 26 and can be removed by filtration. Pressure control valve 28 and liquid pressure control valve 30 control the pressure in the reactor.
The temperature in the reactor 22 preferably should be 195° C. to 215° C. (more preferably 200° C. to 210° C.). If the temperature is too high substantial, unwanted, decomposition of the components of the mixture may occur and the reactor pressure may be too high. If the temperature is too low the conversion of hydroxymethylfurfural to levulinic acid may be too slow. The average residence time a given volume of the intermediate mixture from the first reactor remains in the reactor 22 should be 15 minutes to 30 minutes (more preferably 20 minutes to 30 minutes). Average residence time, as used herein, refers to the time it takes to remove from the reactor (by the draining of the liquid components such as levulinic acid) a volume of components of the mixture equal to the average volume of the mixture in the reactor 22. If the average residence time is too short, the degradation to the desired products may not be complete. If the average residence time is too long, the efficiency of the system may diminish.
The mineral acid concentration of the aqueous portion of the mixture in the reactor 22 preferably is 2% to 7.5%, preferably 3% to 7%, by weight. The mineral acid concentration can be adjusted upward at this stage, if desired, by adding acid to the mixture entering the reactor.
EXAMPLES
Examples 1-3 pertain to the conversion of a bleached kraft paper waste sludge to levulinic acid. The cellulose content of this sludge has been measured to be consistently in the range 42% to 50% by "Quansac" analysis (digestion by concentrated sulfuric acid). The average analysis is 44% by weight. That is, 100 lbs of bone dry sludge contains 44 lbs of cellulose which is available for conversion to levulinic acid.
Examples 4 and 5 pertain to conversion of a partially or non-bleached kraft paper sludge. The cellulose content of this sludge has been measured to be 80% by weight on average. That is, 100 lbs of bone dry sludge contains 80 lbs of cellulose which is available for conversion to levulinic acid. Example 6 pertains to conversion of raw wood flour. The cellulose content of this has been measured to be, on average, 42% by weight. That is, 100 lbs of bone dry sludge contains 42 lbs of cellulose which is available for conversion to levulinic acid.
Example 1
0.945 liters per minute of a 4.0% by weight slurry of paper sludge originating from a fully bleached Kraft pulping process containing 3.5% by weight of the aqueous portion sulfuric acid is fed to the reactor system. The first stage tubular reactor is fifteen feet in length and 0.41 inches in inside diameter. High pressure steam is injected into the process stream at an average rate of 0.47 liters per minute (condensed volume) as it passes into the tubular reactor. The residence time of the reaction mixture in the first stage tubular reactor is 14 seconds. The mixture passes through the pressure let-down valve and flashes directly into the second stage reactor vessel via the dip tube. The second stage reactor is a 10 inch I.D. (Schedule 20 pipe section) vessel of overall length 27 inches. The liquid level in the second stage is set by means of a load switch to give a second stage residence time of 30.0 minutes. The temperature in the first stage reactor was controlled at 232° C. by injection of high pressure steam. The pressure in the first stage reactor was controlled at between 450 and 476 pounds per square inch gauge by means of the pressure let-down valve at the end of the first stage reactor. The temperature in the second stage reactor was controlled at 196° C. and the pressure was controlled at between 207 and 210 psig by means of a vent throttle valve.
The liquid product outflow containing levulinic acid was measured at 1.276 liters per minute and the vent outflow was measured at 0.208 liters per minute after condensation. The levulinic acid concentration in the liquid outflow was measured by analysis to be 0.68% at steady state after four hours of operation. The product outflow from the reactor system was therefore calculated to be 0.0088 kg per minute representing a yield of levulinic acid of 76% of theoretical. A trace quantity (0.0001 kg per min) of levulinic acid was measured in the vent stream this was accounted for as additional yield.
Example 2
0.96 liters per minute of a 2.0% by weight slurry of paper sludge originating from a fully bleached Kraft pulping process containing 1.90% by weight of the aqueous portion sulfuric acid is fed to the reactor system. The first stage tubular reactor is fifteen feet in length and 0.41 inches in inside diameter. High pressure steam is injected into the process stream at an average rate of 0.47 liters per minute (condensed volume) as it passes into the tubular reactor. The residence time of the reaction mixture in the first stage tubular reactor is 14 seconds. The mixture passes through the pressure let-down valve and flashes directly into the second stage reactor vessel via the dip tube. The second stage reactor is a 10 inch I.D. (Schedule 20 pipe section) vessel of overall length 27 inches. The liquid level in the second stage is set by means of a load switch to give a second stage residence time of 20.0 minutes. The temperature in the first stage reactor was controlled at 215° C. by injection of high pressure steam. The pressure in the first stage reactor was controlled between 440 and 460 pounds per square inch gauge by means of the pressure let-down valve at the end of the first stage reactor. The temperature in the second stage reactor was controlled at between 200° and 205° C. and the pressure was controlled at between 230 and 255 psig by means of a vent throttle valve.
The liquid product outflow containing levulinic acid was measured at 1.28 liters per minute and the vent outflow was measured at 0.15 liters per minute after condensation. The levulinic acid concentration in the liquid outflow was measured by analysis to be 0.48% at steady state after four hours of operation. The product outflow from the reactor system was therefore calculated to be 0.0061 kg per minute representing a yield of levulinic acid of 86.7% of theoretical. No levulinic acid was measured in the vent stream.
Example 3
0.32 liters per minute of a 10% by weight slurry of paper sludge containing 3% by weight of the aqueous portion sulfuric acid is fed to the reactor system. The first stage tubular reactor is thirteen feet in length and 0.41 inches in inside diameter. High pressure steam is injected into the process stream at an average rate of 0.55 liters per minute (condensed volume) as it passes into the tubular reactor. The residence time of the reaction mixture in the first stage tubular reactor is 23.3 seconds. The mixture passes through the pressure let-down valve and flashes directly into the second stage reactor vessel via the dip tube. The second stage reactor is a 10 inch I.D. (Schedule 20 pipe section) vessel of overall length 27 inches. The liquid level in the second stage is set by means of a load switch to give a second stage residence time of 29.8 minutes. The temperature in the first stage reactor was controlled at 230° C. by injection of high pressure steam. The pressure in the first stage reactor was controlled between 440 and 460 pounds per square inch gauge by means of the pressure let-down valve at the end of the first stage reactor. The temperature in the second stage reactor was controlled between 206° and 210° C. and the pressure was controlled at between 230 and 255 psig by means of a vent throttle valve.
The liquid product outflow containing levulinic acid was measured at 0.530 liters per minute and the vent outflow was measured at 0.34 liters per minute after condensation. The levulinic acid concentration in the liquid outflow was measured by analysis to be 0.91% at steady state after two and a half hours of operation. The product outflow from the reactor system was therefore calculated to be 0.00482 kg per minute levulinic acid representing a yield of levulinic acid of 48.3% of theoretical. No levulinic acid was measured in the vent stream.
Example 4
1.02 liters per minute of a 1.0% by weight slurry of paper sludge originating from a non-bleached Kraft pulping process containing 1.15% by weight of the aqueous portion sulfuric acid is fed to the reactor system. The first stage tubular reaction is fifteen feet in length and 0.41 inches in inside diameter. High pressure steam is injected into the process stream at an average rate of 0.476 liters per minute (condensed volume) as it passes into the tubular reactor. The residence time of the reaction mixture in the first stage tubular reactor is 14 seconds. The mixture passes through the pressure let-down valve and flashes directly into the second stage reactor vessel via the dip tube. The second stage reactor is a 10 inch I.D. (Schedule 20 pipe section) vessel of overall length 27 inches. The liquid level in the second stage is set by means of a load switch to give a second stage residence time of 20.0 minutes. The temperature in the first stage reactor was controlled at 220° C. by injection of high pressure steam. The pressure in the first stage reactor was controlled at between 450 and 476 pounds per square inch gauge by means of the pressure let-down valve at the end of the first stage reactor. The temperature in the second stage reactor was controlled at 200° C. and the pressure was controlled at between 207 and 215 psig by means of a vent throttle valve.
The liquid product outflow containing levulinic acid was measured at 1.42 liters per minute and the vent outflow was measured at 0.076 liters per minute after condensation. The levulinic acid concentration in the liquid outflow was measured by analysis to be 0.36% at steady state after two hours of operation. The product outflow from the reactor system was therefore calculated to be 0.0073 kg per minute representing a yield of levulinic acid of 68% of theoretical. No levulinic acid was measured in the vent stream.
Example 5
1.04 liters per minute of 2.0% by weight slurry of paper sludge originating from a non-bleached Kraft pulping process containing 1.5% by weight of the aqueous portion sulfuric acid is fed to the reactor system. The first stage tubular reactor is fifteen feet in length and 0.41 inches in inside diameter. High pressure steam in injected into the process stream at an average rate of 0.32 liters per minute (condensed volume) as it passes into the tubular reactor. The residence time of the reaction mixture in the first stage tubular reactor is 14 seconds. The mixture passes through the pressure let-down valve and flashes directly into the second stage reactor vessel via the dip tube. The second stage reactor is a 10 I.D. (Schedule 20 pipe section) vessel of overall length 27 inches. The liquid level in the second stage is set by means of a load switch to give a second stage residence time of 25.0 minutes. The temperature in the first stage reactor was controlled at 215° C. by injection of high pressure steam. The pressure in the first stage reactor was controlled at between 450 and 476 pounds per square inch gauge by means of the pressure let-down valve at the end of the first stage reactor. The temperature in the second stage reactor was controlled at 200° C. and the pressure was controlled at between 207 and 215 psig by means of a vent throttle valve.
The liquid product outflow containing levulinic acid was measured at 1.34 liters per minute and the vent outflow was measured at 0.02 liters per minute after condensation. The levulinic acid and glucose concentration in the liquid outflow was measured at steady state after three and a half hours of operation. The yield of levulinic acid was calculated to be 71% of theoretical. No levulinic acid was measured in the vent stream.
After five hours of operation the feed to the system was reduced to 0.43 liters per minute and the second stage reactor allowed to react further with the reduced inflow and the temperature being maintained by injection of 0.22 liters per minute steam to the first stage. The yield of levulinic acid was found to increase to 92% of theoretical.
Example 6
0.70 liters per minute of a 10% by weight slurry of hardwood flour containing 5.0% by weight of the aqueous portion sulfuric acid is fed to the reactor system. The first stage tubular reactor is fifteen feet in length and 0.41 inches in inside diameter. High pressure steam is injected into the process stream at an average rate of 0.65 liters per minute (condensed volume) as it passes into the tubular reactor. The residence time of the reaction mixture in the first stage tubular reactor is 15.7 seconds. The mixture passes through the pressure let-down valve and flashes directly into the second stage reactor vessel via the dip tube. The second stage reactor is a 10 inch I.D. (Schedule 20 pipe section) vessel of overall length 27 inches. The liquid level in the second stage is set by means of a load switch to give a second stage residence time of 20.0 minutes. The temperature in the first stage reactor was controlled at 220° C. by injection of high pressure steam. The pressure in the first stage reactor was controlled by means of an orifice at the end of the first stage reactor. The temperature in the second stage reactor was controlled at 210° C. and the pressure was controlled by means of a vent throttle valve.
The liquid product outflow containing levulinic acid was measured at 1.15 liters per minute and the vent outflow was measured at 0.23 liters per minute after condensation. The levulinic acid concentration in the liquid outflow was measured by analysis to be 1.05% at steady state. The product outflow from the reactor system was therefore calculated to be 0.0121 kg per minute representing a yield of levulinic acid of 62% of theoretical. A small quantity (0.000069 Kg per min) of levulinic acid was measured in the vent stream this was accounted for as additional yield.
Other embodiments are within the claims. For example, other carbohydrate-containing materials like ground wood paper sludge and recycled paper sludge can be used in the process. Moreover, under some circumstances, such as in example 5, it may be improve yield if the second reactor is run as a batch process, instead of as a continuous process. | A continuous process for producing levulinic acid from carbohydrate-containing materials in high yields is described. According to the process, a carbohydrate-containing material is supplied continuously to a first reactor and hydrolyzed at between 210° C. and 230° C. for between 13 seconds and 25 seconds in the presence of between 1% and 5% by weight mineral acid. The hydrolysis produces hydroxymethylfurfural, which is removed continuously from the first reactor and supplied continuously to a second reactor. In the second reactor, the hydroxymethylfurfural is hydrolyzed further at between 195° C. and 215° C. for between 15 minutes and 30 minutes to produce levulinic acid, which is continuously removed from the second reactor. The levulinic acid preferably is produced in at least 60%, and more preferably at least 70%, of the theoretical yield based on the hexose content of the carbohydrate-containing material. | 2 |
BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention relates to building structures and is directed more particularly to a wall assembly by which there may be constructed a wall structure without benefit of mortar, or the like.
2. Description of the Prior Art
A combination of building blocks and lattice structures is generally known. For example, U.S. Pat. No. 791,291, issued May 30, 1905 to G. J. Roberts, relates to blocks having edge configurations for interlocking engagement and also having grooves therein for receiving wires or rods which operate to retain the blocks in their desired positions. The wires or rods are preferably held by a metal frame which constitutes the outer limits of the wall, the blocks being mounted within the frame.
In U.S. Pat. No. 2,228,363, issued Jan. 14, 1941, to R. L. Pinney, there is disclosed a wall structure of pre-formed blocks with means for connecting the blocks together without mortar. The connecting means comprises key members of generally H-shaped cross section which operate to connect the edge of a first block to a mating edge of a second block.
U.S. Pat. No. 2,294,051, issued Aug. 25, 1942 to N. P. Sjobring shows a wall construction utilizing blocks having tongues extending therefrom, the tongues being provided with notches for receiving locking tie rods.
A. Penton, in U.S. Pat. No. 3,546,833, issued Dec. 15, 1970, discloses a wall construction assembly including a building block, an insulating insert, and a ladder-like metal reinforcing member. U.S. Pat. No. 2,929,238, issued Mar. 22, 1960 to K. H. Kaye also shows a ladder-like "joint mesh strip" for use in building block construction. In the Peneton and Kaye disclosures, it is intended that the reinforcing member be used in conjunction with mortar, cement, or the like.
There exists a need for an assembly by which wall structures, and the like, may be quickly and easily erected, without use of mortar, allowing a reduction in expense of skilled labor.
SUMMARY OF THE INVENTION
An object of the present invention is to provide a wall assembly which can be easily and quickly assembled without use of mortar, cement, or the like.
A further object of the invention is to provide such a wall assembly including preformed building blocks and a lattice member for interconnecting and locking in place such building blocks.
With the above and other objects in view, as will hereinafter appear, a feature of the present invention is the provision of a wall assembly comprising a plurality of building blocks, each of the building blocks having a first upstanding, rectangularly-shaped wall portion, a second upstanding, rectangularly-shaped wall portion parallel to and coextensive with the first wall portion, and a third upstanding wall portion interconnecting the first and second wall portions, the first wall portion having first goove means on an interior surface thereof opposed to the second wall portion, the first groove means extending from an upper edge of the first wall portion toward a lower edge of the first wall portion the second wall portion having second groove means on an interior surface opposed to the first wall portion, the second groove means extending from an upper edge of the second wall portion toward a lower edge of the second wall portion, the third wall portion having third groove means in an upper edge thereof, the third groove means extending width-wise of the third wall portion upper edge, and a lattice member comprising first and second elongated runner members disposed parallel to each other and co-extensive with each other, and spreader members, each spreader member interconnecting the runner members, the ends of the spreader members extending beyond the runner member, the spreader members being upturned at their ends to provided end portions extending substantially normal to the spreader member and extending upwardly above the runner members, the first groove means being adapted to receive the spreader end portions and the third groove means being adapted to receive the runner members, whereby the lattice member is adapted to interconnect and lock together the pluality of building blocks to form a wall structure.
The above and other features of the invention, including various novel details of construction and combinations of parts, will now be more particularly described with reference to the accompanying drawings and pointed out in the claims. It will be understood that the particular devices embodying the invention are shown by way of illustration only and not as a limitation of the invention. The principles and features of this invention may be employed in various and numerous embodiments without departing from the scope of the invention.
BRIEF DESCRIPTION OF THE DRAWINGS
Reference is made to the accompanying drawings in which is shown an illustrative embodiment of the invention from which its novel features and advantages will be apparent.
In the drawings:
FIG. 1 is a perspective view of one form of building block suitable for the illustrative assembly;
FIG. 2 is a top plan view of the block of FIG. 1;
FIG. 3 is an elevational section view, taken along line III--III of FIG. 2;
FIG. 4 is a perspective view of another form of building block;
FIG. 5 is a top plan view of the block of FIG. 4;
FIG. 6 is an elevational sectional view, taken along line VI--VI of FIG. 5;
FIG. 7 is a perspective view of antoerh form of building blocks;
FIG. 8 is a top plan view of the block of FIG. 7;
FIG. 9 is an elevational sectional view, taken along line IX--IX of FIG. 8;
FIG. 10 is a perspective view of one form of lattice member suitable for the illustrative assembly;
FIG. 11 is a top plan view of an illustrative assembly in accordance with the invention;
FIG. 12 is an elevational sectional view of the assembly; and
FIG. 13 is an enlarged detailed elevational view of a building block and a portion of the lattice member.
DESCRIPTION OF THE PREFERRED EMBODIMENT
Referring to the drawings, and particularly FIGS. 1-3, it will be seen that an illustrative building block comprises a preferred block 2 of concrete, cinder block, plastic, wood, or other suitable material. The block 2 is provided with a first upstanding rectangularly-shaped wall portion 4, a second upstanding rectangularly-shaped wall portion 6 disposed parallel to, and coextensive with, the first wall portion 4, and a third upstanding wall portion, or web, 8 interconnecting the first and second wall portions. In the block 2, there are provided two webs 8 interconnecting the wall portions 4, 6.
The first wall portion 4 is provided with first groove means 10 on an interior surface thereof 12 opposed to the second wall portion 6. The first groove means in the block 2 includes two grooves 10 extending from an upper edge 14 of the first wall portion 4 to a lower edge 16 of the first wall portion. In like manner, the second wall portion 6 is provided with second groove means 18 on an interior surface thereof 20, opposed to the first wall portion. The second groove means comprises a pair of grooves 18 opposed to the grooves 10 and extending from an upper edge 22 of the second wall portion to a lower edge 24 of the second wall portion.
The third wall portions, or webs, 9 are provided with third groove means 26 in an upper edge thereof 28, the third groove means including pairs of grooves 26 extending width-wise of the third wall portion upper edge 28.
In a preferred embodiment, the block 2 would have a length of sixteen inches, a width of eight inches and a height of eight inches or, alternatively, four inches.
In FIGS. 4-6, there is shown an end block 30 having first, second and third wall portions 32, 34, 36 arranged substantially as described relative to the block 2 of FIG. 1. The end block 30 is preferably half the length of the block 2 and therefore is provided with a single web 36. First, second and third groove means 38, 40, 42 are provided in substantially the same fashion as the groove means of the block 2, except that with the shorter length, the block 30 is provided with a first groove means comprising a single groove 38, a second groove means comprising a single groove 40, and a third groove means comprising a pair of grooves 42. The block 30 is provided with an end wall 44 interconnecting ends of the first and second wall portions.
In FIGS. 7-9, there is shown an end, or corner, block 50 having first, second, third and end wall portions 52, 54, 56, 58, substantially as described hereinabove with respect to the end block 30. The first and second wall portions 52, 54 are respectively provided with first and second groove means 60, 62 disposed similarly to the first and second groove means of the block 2. The third wall portion 56 is similar to the third wall portion 36 of the end block 30 and is provided with third groove means 42. The end wall 58 of the block 50 is disposed similarly to the end wall 44 of the end block 30.
However, in addition to the features previously discussed with respect to the blocks 2 and 30, the corner block 50 is provided with a fourth groove means 66. The fourth groove means 66 includes a pair of grooves 66 on an upper edge 68 of the first wall portion 52 and an aligned pair of grooves 66 on an upper edge 70 of the second wall portion 54. The corner block 50 is further provided with a fifth groove means 72 comprising a single groove on an interior surface 74 of the end wall portion 58 and extending from an upper edge 76 of the end wall portion to a lower edge 78 thereof. The corner block 50 is preferably of outside dimensions substantially equal to those of the block 2.
Referring to FIG. 10, there is shown an illustrative lattice member 80, including first and second elongated runner members 82, 84 disposed parallel to each other and coextensive with each other. Spreader members 86 are fixed to and interconnect the funner members 82, 84 at spaced intervals. Ends of the spreader members 86 extend beyond the runner members and are upturned to provide end portions 88 extending substantially normal to the spreader members. The spreader members are connected to the runner members at the underside of the runner members, as viewed in FIG. 10, and the end portions 88 of the spreader members extend upwardly above the runner members. The lattice member is preferably constructed of steel rods.
Referring to FIG. 13, it will be seen that the first and second groove means 10, 18 are adapted to receive the spreader end portions 88, and the third groove means 26 are adapted to receive the runner members 82, 84. The end portions 88 project upwardly beyond the upper edges 14, 22, 28 of the wall portions of the block and are adapted to engage the first and second groove means of a block (now shown) on top of the block shown in FIG. 13.
The corner block 50 fourth groove means 66 are adapted to receive the lattice member runner members 80, 82 width-wise of the block, and the fifth groove means 72 are adapted to receive spreader member end portions 88. Thus, the corner block 50 is adapted to receive lattice members lengthwise and width-wise.
The use of the assembly is best illustrated in FIGS. 11 and 12. Referring particularly to FIG. 11, an illustrative wall section 90 includes a corner block 50, a regular or line block 2, and an end block 30. A lattice member 80 locks the blocks together, the runner members 82, 84 of the lattice member being received in the groove means 26, 42 and 64, and the spreader member end portions 88 being received in the groove means 10 and 18, 38 and 40, and 60 and 62. As shown in FIG. 12, the upstanding end portions 88 additionally engage the groove means 10, 18, 38, 40, 60 and 62 of the line of blocks above the line in which rests the lattice member.
Turning again to FIG. 11, a second wall section 92 comprises a series of line blocks 2, an end line block abutting the corner block 50. A second lattice member 80 1 is disposed width-wise of the corner block 50, runner members 82 1 , 84 1 being accepted in the groove means 66 and an end portion 88 1 of a spreader member 86 1 being accepted by the groove means 72.
In practice, the corner block 50 may be used as an ordinary end block, taking the place of the block 30 if the additional length of the block 50 is desired.
Thus, without use of mortar, cement, or the like, wall sections may be erected and subsequently dismounted. The assembly is particularly useful in the construction of temporary quarters, garden walls, decorative walls, traffic detour walls, and like walls or partitions which might be subject to dismantlement or movement.
It is to be understood that the present invention is by no means limited to the particular construction herein disclosed and/or shown in the drawings, but also comprises any modifications or equivalents within the scope of the disclosure.
For example, it will be apparent that the vertical grooves, such as grooves 10, 18 need not extend from top to bottom of the block, inasmuch as only a portion of the grooves receive the lattice member. However, for ease of manufacture, the grooves may extend, as shown, from the upper edge to the lower edge of the block. | A wall assembly comprising a plurality of building blocks, each of the building blocks have first and second coextensive and parallel wall portions interconnected by a third wall portion, each of the wall portions being provided with grooves therein, and a lattice member comprising parallel and coextensive runner members interconnected by spreader members, the grooves being adapted to receive the lattice member, the lattice member being operative to interconnect and lock together the building blocks to form a wall structure. | 4 |
BACKGROUND OF THE INVENTION
[0001] This invention relates generally to ejectors, and, more particularly, to an ejector motive nozzle that may be used in pumping, compression, or mixing applications.
[0002] At least some known ejectors mix two flow streams, a high-pressure (“motive”) stream and a low-pressure (“suction”) stream, so as to produce a discharge flow with pressure intermediate to or lower than the two input flows. The ejector motive nozzle facilitates this mixing process by accelerating the high-pressure motive flow, thereby creating a high speed jet that is channeled through a mixing tube or chamber to entrain the low pressure suction flow. The two mixed flows are then discharged, typically through a diffuser.
[0003] Some known ejectors use a motive nozzle that is surrounded by a casing and includes a nozzle tip having a round or rectangular cross-section oriented about an axis of the ejector. At least some known nozzles may create a motive jet that oscillates in a bending mode, producing coherent flow disturbances such as partial ring vortex structures at an edge of the jet. When these coherent flow disturbances strike a downstream wall of the casing, reflected acoustic waves may be produced and feedback towards the nozzle. The feedback waves may reinforce the jet bending oscillations and result in a fluid dynamic resonance that may produce damaging structural loads and/or high noise levels within the ejector. Over time, fluctuating loads produced by this fluid dynamic resonance may decrease the lifespan of the ejector or other hardware, add to maintenance costs, and/or create objectionable levels of environmental noise.
BRIEF DESCRIPTION OF THE INVENTION
[0004] In one aspect, a method of assembling an ejector is provided, wherein the method includes providing a motive nozzle tip having a centerline axis and including a nozzle tip edge having at least one protrusion extending through a plane normal to the centerline axis. The method also includes coupling the motive nozzle tip to the ejector.
[0005] In another aspect, an ejector is provided, wherein the ejector includes a motive nozzle tip having a centerline axis and including a nozzle tip edge having at least one protrusion extending through a plane normal to the centerline axis.
[0006] In a further aspect, a gas turbine engine is provided, wherein the gas turbine engine includes a compressor and an ejector coupled in flow communication with and configured to receive air bled from the compressor. The ejector includes a motive nozzle tip having a centerline axis and including a nozzle tip edge having at least one protrusion extending through a plane normal to the centerline axis.
BRIEF DESCRIPTION OF THE DRAWINGS
[0007] FIG. 1 is a cross-sectional schematic illustration of an exemplary gas turbine engine;
[0008] FIG. 2 is a schematic block diagram of the engine shown in FIG. 1 and including a turbine cooling ejector;
[0009] FIG. 3 is an enlarged schematic illustration of the turbine cooling ejector shown in FIG. 2 ;
[0010] FIG. 4 is a perspective view of an exemplary nozzle tip that may be used with the turbine cooling ejector shown in FIG. 3 ; and
[0011] FIG. 5 is a perspective view of an exemplary cooling jet stream discharged from the nozzle tip shown in FIG. 4 .
DETAILED DESCRIPTION OF THE INVENTION
[0012] FIG. 1 is a schematic illustration of an exemplary gas turbine engine 100 . Engine 100 includes a compressor 102 and a combustor assembly 104 . Combustor assembly 104 includes a combustor assembly inner wall 105 that at least partially defines a combustion chamber 106 . Combustion chamber 106 has a centerline 107 that extends therethrough. In the exemplary embodiment, engine 100 includes a plurality of combustor assemblies 104 . Combustor assembly 104 , and, more specifically, combustion chamber 106 is coupled downstream from and in flow communication with compressor 102 . Engine 100 also includes a turbine 108 and a compressor/turbine shaft 110 (sometimes referred to as rotor 110 ). In the exemplary embodiment, combustion chamber 106 is substantially cylindrical and is coupled in flow communication with turbine 108 . Turbine 108 is rotatably coupled to, and drives, rotor 110 . Compressor 102 is also rotatably coupled to shaft 1 10 . The present invention is not limited to any one particular engine and may be implanted in connection with other engines or other devices which employ ejectors in any part of the processes by which they operate. For example, the present invention may be used with, but is not limited to use with oil refinery devices, chemical plant devices, and electric cars.
[0013] In operation, air flows through compressor 102 and a substantial amount of compressed air is supplied to combustor assembly 104 . Assembly 104 is also in flow communication with a fuel source (not shown in FIG. 1 ) and channels fuel and air to combustion chamber 106 . In the exemplary embodiment, combustor assembly 104 ignites and combusts fuel, for example, synthetic gas (syngas) within combustion chamber 106 that generates a high temperature combustion gas stream (not shown in FIG. 1 ). Alternatively, assembly 104 combusts fuels that include, but are not limited to natural gas and/or fuel oil. Combustor assembly 104 channels the combustion gas stream to turbine 108 wherein gas stream thermal energy is converted to mechanical rotational energy.
[0014] FIG. 2 is a schematic block diagram of engine 100 including a turbine cooling ejector 150 coupled in flow communication between compressor 102 and turbine 108 . Low-pressure air is extracted from compressor 102 from a plurality of outlets 152 and high-pressure air is extracted from a plurality of outlets 154 . In the exemplary embodiment, low-pressure air is extracted from the ninth stage of compressor 102 and high-pressure air is extracted from the thirteenth stage of compressor 102 . In alternative embodiments, low-pressure air may be extracted at any compressor low-pressure stage and high-pressure air may be extracted from any compressor high-pressure stage.
[0015] The high-pressure and low-pressure air is channeled to ejector 150 . Specifically, high-pressure air is channeled axially through a motive nozzle (not shown) within ejector 150 , and low-pressure air is channeled to a chamber (not shown) surrounding the motive nozzle. As high-pressure air is discharged from the motive nozzle, it entrains the low-pressure air, to facilitate mixing between the two air flows. The mixed air flow is discharged to turbine 108 wherein the air facilitates cooling turbine 108 . As such, ejector 150 facilitates cooling turbine 108 using low-pressure air, such that the efficiency of engine 100 is improved as compared to systems using high-pressure cooling air.
[0016] FIG. 3 is an enlarged schematic illustration of ejector 150 . FIG. 4 is a perspective view of an exemplary motive nozzle tip 200 that may be used with ejector 150 . FIG. 5 is a perspective view of an exemplary cooling jet 202 discharged from nozzle tip 200 . Ejector 150 includes a motive nozzle 204 and a casing 206 that extends radially outward from a downstream end 208 of motive nozzle 204 . Motive nozzle 204 includes a substantially annular body portion 210 and a tapered conical portion 212 extending from downstream end 208 . Nozzle tip 200 extends from downstream end 208 with a frusto-conical cross-sectional shape, such that motive nozzle body portion 210 has a larger radius R 1 than a radius R 2 of nozzle tip 200 . Body portion 210 also includes a high-pressure inlet 214 .
[0017] Casing 206 includes a substantially annular body portion 216 that is spaced radially outward from motive nozzle downstream end 208 , such that a low-pressure chamber 218 is defined therebetween. A frusto-conical portion 220 extends downstream from casing body portion 216 . Portion 220 is positioned such that low-pressure chamber 218 is coupled in flow communication with a chamber 222 defined by conical portion 220 . Furthermore, a substantially annular mixing channel 224 is coupled in flow communication with, and downstream from, conical portion 220 . Mixing channel 224 has a radius R 3 that is smaller than a radius R 4 of casing body portion 216 . An ejection end 226 of ejector 150 is defined at a downstream end 228 of casing 206 . Furthermore, casing body 216 includes a low-pressure inlet 230 .
[0018] The cross sectional area of nozzle tip 200 is convergent in the direction of flow and, in the exemplary embodiment, includes a plurality of protrusions 232 that extend substantially axially therefrom to define a nozzle lip 234 . In the exemplary embodiment, protrusions 232 are identical and each has a substantially triangular shape. Protrusions 232 extend circumferentially about nozzle tip 200 , such that a plurality of triangular recesses 236 are defined between each pair of circumferentially-adjacent protrusions 232 . Specifically, protrusions 232 define a chevron-shaped nozzle lip 234 at an end of nozzle tip 200 . In an alternative embodiment, nozzle tip 200 is slotted and includes a plurality of protrusions extending from a nozzle lip defined at an edge of the slotted nozzle tip. Protrusions 232 may be rounded such that nozzle tip 200 includes a plurality of round-edged cutouts. Moreover, although only seven protrusions 232 are illustrated, it should be noted that nozzle tip 200 may include more or less protrusions 232 . In addition, the size, shape, number, and relative orientation of protrusions 232 is variably selected depending on the use of nozzle tip 200 to facilitate optimizing jet flow 238 discharged therefrom. More specifically, protrusions 232 and, more particularly, nozzle lip 234 facilitate creating a jet flow discharged therefrom with lobed-shaped vortices 240 , for example, a lobed-shaped jet 202 .
[0019] During operation, high-pressure air is channeled to ejector 150 and is discharged through inlet 214 into motive nozzle 204 . Air at relatively low pressure is discharged through low pressure inlet 230 into low pressure chamber 218 . The high-pressure air flows substantially axially through motive nozzle 204 and is accelerated to high speed prior to being discharged through nozzle tip 200 . The orientation of protrusions 232 facilitates discharged air from nozzle tip 200 creating lobed-shaped jet 202 . The shape, velocity, and pressure of lobed-shaped jet 202 facilitates jet 202 entraining the low-pressure air in low-pressure chamber 218 causing the high-pressure and low-pressure air to mix in mixing channel 224 . The mixed air is then discharged through ejector end 226 , such that the mixture of high-pressure and low-pressure air is utilized to facilitate cooling turbine 108 . In alternative embodiments, the mixed air may be used to cool other components of engine 100 .
[0020] The nozzle tip is configured to facilitate the formation of longitudinal flow structures (such as lobes or counter-rotating vortices) that stabilize the jet. Furthermore, the nozzle tip is configured to resist formation of other destabilizing flow structures (such as ring vortices) when the jet is perturbed by noise or other flow disturbances. Specifically, during engine operations, the lobed-shaped jet 202 created by protrusions 232 facilitates increasing the life-span of ejector 150 . Specifically, the protrusions 232 facilitate reducing the intensity and symmetry of flow disturbances produced by or associated with jet bending oscillations, such as coherent ring vortices. Typically, jet bending oscillations in an ejector cause acoustic waves to reflect off a casing wall and back towards the motive nozzle. The lobes created in jet 202 by protrusions 232 reduce the coherency of circumferential turbulent flow structure produced by jet bending, interfering with reinforcement of such flow structures by acoustic waves reflected from casing 206 . Furthermore, because the nozzle interior trailing edges produced by protrusions 232 lie outside of a plane normal to the nozzle, the ability of reflected acoustic waves to excite further jet bending oscillation is reduced. Specifically, protrusions 232 facilitate preventing a reflected wave from oscillating in phase with oscillations of jet 202 , such that the oscillations are disrupted and not enhanced. As such, protrusions 232 facilitate disrupting both the formation and excitation of jet bending oscillations, and thereby, facilitate reducing the effects that jet bending oscillations may have on ejector 150 .
[0021] As a result of protrusions 232 , less vibration is induced to ejector 150 by jet bending oscillations as flow is discharged from nozzle tip 200 . Furthermore, nozzle tip 200 and, more particularly, protrusions 232 , facilitate reducing the excitation of any resonance and vibrations induced to ejector 150 . Accordingly, ejector 150 generates substantially less noise, and experiences substantially reduced fluctuating structural loads than other known ejectors. As such, a useful life of ejector 150 and other connected devices is facilitated to be enhanced, and environmental noise produced by the ejector is reduced.
[0022] The above-described methods and apparatus facilitate increasing the life span of an ejector and reducing environmental noise produced by its operation. Specifically, the chevron-shaped nozzle tip produces a lobed-shape jet that facilitates reducing jet bending oscillations which may occur in an ejector motive nozzle. Furthermore, the lobed-shaped jet facilitates reducing the excitation of jet bending oscillations, such that vibrations induced to the ejector motive nozzle are reduced. Subsequently, less noise and fewer structural loads are generated within the ejector. Moreover, the chevron-shaped nozzle tip also increases entrainment of the low-pressure air, allowing the ejector to operate more efficiently. Ultimately, the above-described methods and apparatus facilitate providing a more efficient and more stable ejector, such that system engine efficiency may increase, costs associated with maintenance of the ejector and devices in flow communication with the ejector may decrease, and the life-span of the system may increase.
[0023] As used herein, an element or step recited in the singular and proceeded with the word “a” or “an” should be understood as not excluding plural said elements or steps, unless such exclusion is explicitly recited. Furthermore, references to “one embodiment” of the present invention are not intended to be interpreted as excluding the existence of additional embodiments that also incorporate the recited features.
[0024] Although the apparatus and methods described herein are described in the context of an ejector motive nozzle for a gas turbine engine, it is understood that the apparatus and methods are not limited to ejector motive nozzles or gas turbine engines. Likewise, the ejector motive nozzle components illustrated are not limited to the specific embodiments described herein, but rather, components of the ejector motive nozzle can be utilized independently and separately from other components described herein.
[0025] While the invention has been described in terms of various specific embodiments, those skilled in the art will recognize that the invention can be practiced with modification within the spirit and scope of the claims. | A method of assembling an ejector is provided, wherein the method includes providing a motive nozzle tip having a centerline axis and including a nozzle tip edge having at least one protrusion extending through a plane substantially normal to the centerline axis. The method also includes coupling the motive nozzle tip to the ejector. | 5 |
BACKGROUND OF THE INVENTION
Fuel waste and generation of pollutants are problems experienced in present day automobile internal combustion engines as a result of the conventional choke mechanism, which is a fuel enriching device used to start a cold engine. The choke apparatus is either manually operated from a dashboard control or is thermostatically operated in response to the temperature of the engine via throttle linkages or electronic spray nozzle injectors.
In every instance these systems put raw fuel into the intake manifold of the cold engine and, while these devices serve the purpose of starting a cold engine, they cause excessive fuel waste and resulting high emissions that pollute the atomosphere as well as cause excessive engine wear. It is known that approximately 25 to 30% of the emissions produced during a so-called CVS "cold start" EPA emission test result from the operation of the choke apparatus.
The reason for this is that in an internal combustion engine system vacuum and air flow are at their lowest during engine startup. The gasoline and air are both generally cold and this makes it virtually impossible to produce a volatile and highly combustible atomized, efficiently mixed, air-fuel mixture during the engine startup cycle. Even when raw fuel is atomized into the engine with fuel injectors there is poor mixing of the fuel with the available air supply and this results in the very rich burn which causes air pollution and significant energy waste in starting present engine systems.
The injection type choke in conventional use is superior to the conventional carburetor type choke but the injection type system uses raw fuel and requires a high presure fuel pump employing a complex drive system to operate the injector valve and is still far from an efficient system. It can only spray raw fuel into the intake manifold or combustion chambers and efficient mixing with the available air supply is virtually impossible. With either the carburetion or injection type choking system, a major portion of the fuel condenses in the intake manifold and on the walls of the combustion chambers rather than mixing with the available air supply whereupon the condensed, unmixed fuel contributes virtually no engine startup energy, and furthermore converts to carbon and enriches the engine exhaust with significant amounts of carbon monoxide.
Thus, even the relatively high degree of atomization realized with the conventional cold start injector, which sprays straight fuel, does not provide the complete air mixing necessary for good combustion and does not significantly improve engine startup efficiency.
A further problem experienced with conventional enriching devices, where improper air-fuel mixing takes place, is the pronounced cooling effect which can lead to ice clogging of the carburetor when the atmosphere is cold and humid. Further, automatic chokes often stick or stay on longer than necessary causing undue fuel waste and air pollution. Hand operated chokes are especially troublesome because operators forget to move them to the off position when their operation is no longer needed.
OBJECTS AND SUMMARY OF THE INVENTION
Accordingly it is a principal object of my invention to provide an improved internal combustion engine fuel injection system and method.
A further object is to provide an improved startup system and method for an internal combustion engine wherein a thoroughly mixed quantity of air and highly atomized fuel is injected into the engine during startup to minimize fuel waste and produce minimum pollutants during the startup cycle.
Still another object is to provide a fuel injection system and method for an internal combustion engine wherein the fuel injectors do not require the conventional, expensive, high pressure fuel pump normally used with fuel injector systems.
Still a further object is to provide a fuel injection system for an internal combustion engine which eliminates the need for a conventional carburetor accelerator pump for supplying an extra charge of fuel to the engine in response to an acceleration command from the throttle control.
Additional objects and advantages of the invention will be set forth in part in the description which follows, and in part will be apparent from the description, or may be learned by practice of the invention. The objects and advantages of the invention may be realized and obtained by means of the instrumentalities and combinations particularly pointed out in the appended claims.
To achieve the foregoing objects and in accordance with the purpose of the invention, as embodied and broadly described herein, the apparatus of the invention comprises a fuel injector valve having an inlet and further including an outlet nozzle in communication with the intake manifold of the internal combustion engine, air-fuel mixing means connected to supply an air-fuel mixture to the injector valve inlet and having means for directing a flow of pressurized air to said inlet through a mixing chamber, means for supplying fuel into said flow of pressurized air whereupon the fuel is mixed with the air in the mixing chamber, and control means for operating the fuel injector valve during engine startup whereby a mixture of air and highly combustible, atomized fuel is fed into the engine intake manifold through the injector valve.
In accordance with a further aspect of the invention, a fuel injection system for an internal combustion engine is provided comprising a fuel injector valve arranged to supply fuel to a combustion chamber of the engine, the valve having an inlet and further including an outlet nozzle in communication with a fuel supply passage to the combustion chamber, air-fuel mixing means connected to supply a air-fuel mixture to the injector inlet and having means for directing a flow of pressurized air to the inlet through a Venturi throat, a fuel source including a low pressure pump for supplying fuel into the flow of pressurized air, the fuel being drawn into and mixed with the flow by the pressure differential produced at said Venturi throat, air supply means for supplying air to the combustion chamber, and control means for operating the fuel injector valve in synchronism with the operating cycle of the engine whereby a highly combustible mixture of air and highly atomized fuel is fed by the injector valve into the combustion chamber in a mix with air from the air supply means during each fuel intake cycle.
In accordance with still another aspect of the invention, a method is provided for starting an internal combustion engine having carburetion means including a throttle control arranged to supply an air-fuel mixture to the engine through an intake manifold, the method comprising the steps of closing the throttle control to minimize the supply of air-fuel mixture from the carburetion means to the engine, operating the starter motor and ignition of the engine, and injecting, while the throttle control is closed and the starter and ignition are in operation, a limited charge of pressurized air mixed with fuel into the intake manifold through a fuel injector valve located downstream of the throttle control whereby a quantity of air mixed with highly atomized fuel is introduced into the engine to induce engine startup.
BRIEF DESCRIPTION OF THE DRAWINGS
The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate preferred embodiments of the invention and, together with the description, serve to explain the principles of the invention.
In the drawings:
FIG. 1 is a schematic diagram illustrating the fuel injection system of the invention as incorporated in a conventional carburetion type internal combustion engine for operation during engine startup.
FIG. 2 is a schematic diagram showing the fuel injector valve and air-fuel mixing apparatus of FIG. 1.
FIG. 3 is a schematic diagram illustrating an alternate embodiment of the invention wherein my novel air-fuel mixing apparatus is incorporated for use in a fuel injection type internal combustion engine.
FIG. 4 is a schematic diagram illustrating a simplified form of the invention not utilizing a separate fuel injector valve.
FIG. 5 is a diagram depicting various control systems for the apparatus of the invention.
DETAILED DESCRIPTION OF EMBODIMENTS
FIG. 1 schematically shows a first embodiment of the invention wherein a conventional ignition-operated internal combustion engine 20 is fed, under normal operating conditions, with an air-fuel mixture through an intake manifold 7. A conventional carburetor 24 having a throttle valve 8 provides a regulated flow of atomized fuel and air in the usual fashion.
An electrically controlled fuel injector valve 6 is mounted on the intake manifold 7 downstream of the throttle control 8. The injector valve 6 is fed a supply of premixed fuel and pressurized air from a mixing device 2. The latter receives a supply of fuel from a conduit or line 22 coupled to the main fuel supply line 26 to carburetor 24. Pressurized air is supplied to the mixing device by a conduit or line 28 coupled to an air compressor 11. The compressor is driven by an electric motor 15 powered, for example, by the battery 42 utilized in the engine ignition system. If desired, the compressor can be mechanically driven from the engine itself, thus eliminating the need for the separate motor 15. A cutoff valve 10 is provided in the air line 28 and is electrically controlled by a solenoid 34.
A dashboard-mounted control switch 9 connected to the battery 42 by electrical lead 36 is arranged via leads 38 and 40 to enable simultaneous energization of motor 15, solenoid 34, and injector valve 6 so that a limited charge of a highly atomized air-fuel mixture is injected into intake manifold 18 during the engine startup cycle.
The details of the fuel injector valve 6 and the air-fuel mixing device 2 are illustrated in FIG. 2. Fuel injector valve 6 is of conventional design and may be of the coil and armature type such as supplied, for example, by the Bosch Company of West Germany. Injector valve 6 has an inlet 51 for receiving a charge of mixed air and fuel and further has a swirl nozzle 54 for discharging a highly atomized spray of air-fuel mixture into the engine intake manifold. A solenoid winding 50 and axially movable armature 52 operate to open and close the valve unit in response to control signals on line 38.
The air-fuel mixing device 2 includes a block 2a of brass, aluminum, or other suitable material having a mixing chamber 1 which is coupled by an adaptor 5 to the inlet 51 of the injector valve. A second adapter 3, including a check valve, couples the fuel supply line 22 to the mixing chamber 1 via a Venturi passage 16. A third adaptor unit 4, also incorporating a check valve, couples the pressurized air supply line 28 to the mixing chamber 1 via a Venturi throat 1a.
Air under pressure flowing from supply line 28 through Venturi throat 1a and into mixing chamber 1 draws fuel into the mixing chamber through the Venturi passage 16. The fuel is drawn into the mixing chamber by the pressure differential produced at the Venturi throat in accordance with the wellknown principle govered by Bernoulli's equation. When the armature 52 in the fuel injector valve 6 is operated to open the valve, a charge of pressurized air and highly atomized fuel flows from mixing chamber 1 through the injector valve and is discharged through swirl nozzle 54 into the engine intake manifold. Flow of the air-fuel mixture through the injection valve and swirl nozzle causes still further mixing action and as a result the air and fuel discharge through the nozzle is very thoroughly mixed.
In operation, the system illustrated in FIGS. 1 and 2 functions as a replacement of the conventional engine choke system. To start the engine the operator actuates the engine starter and ignition and at the same time momentarily actuates control switch 9 for a brief interval such as one or two seconds. Actuation of the control switch opens the normally closed solenoid valve 10 allowing air under pressure to flow from compressor 11 via conduit 28 to the air-fuel mixing unit 2. Simultaneously, coil 50 of the fuel injector 6 is energized via control lead 38 to open the injector valve. Air under pressure of, for example, 35 to 100 p.s.i. passes through Venturi throat 1a and into mixing chamber 1. The reduced pressure induced at Venturi passage 16 by this flow causes fuel from supply line 22 to be drawn into the mixing chamber, where it is atomized and mixed with the flow of air. Further atomization and mixing takes place as the mixture passes through the injector valve and is discharged through swirl nozzle 54.
This finally atomized mixture of air and fuel is highly combustible and causes the cold engine to start instantly as all four, six, or eight cylinders receive an equal charge of the finally atomized mixture. During the startup cycle, throttle control 8 is preferrably kept fully closed to cut off the flow of air-fuel mixture from carburetor 24.
Should the engine hesitate or begin stalling during or just after startup, a second momentary actuation of control switch 9 brings all cylinders instantly to life and as a general rule no additional fuel is required for startup. Since control switch 9 is spring biased to cause cut off valve 10 in air line 28 to close when the switch is released, only a limited quantity of fuel is used during the startup cycle.
Because the startup air-fuel mixture introduced by injector valve 6 is so finely atomized and completely mixed, resulting in a highly combustible volatile air-fuel mixture, more complete combustion is produced and deleterious exhaust emissions are kept to a minimum during the startup cycle. Air compressor 11 may be an extremely low cost unit and would represent a drain of less than one ampere or one hundredth of a horsepower on the system. Automatic chokes used in conventional systems represent a drain several hundred times this amount because of the high current withdrawal from the battery required due to the longer use of the starting motor necessary to get the cold engine running.
Further, whereas conventional cold start fuel injector systems require a fuel pump that must develop 35 to 50 p.s.i. fuel pressure, the injector system of the invention requires only a conventional low pressure fuel pump such as is presently used on carburetion-type fuel control systems.
FIG. 4 shows a modified form of the invention employing a simplified arrangement eliminating the fuel injection valve and check valves associated with the air-fuel mixing unit. In the system shown, the mixing chamber 1" of the air-fuel mixing unit 2" communicates directly with the engine intake manifold 7'. Gasoline is supplied via a feed line 62 from a float chamber 60. A supply of gasoline is maintained in the chamber 60 by a metering valve 66 actuated by a float 64 in convention fashion.
In this system the air-fuel mixing action provided solely by the flow of pressurized air through chamber 1" creates sufficient atomization and mixing to achieve rapid and efficient engine startup. As will be appreciated, a solenoid actuated valve, not shown and similar to valve 10, may be placed in the air supply line to mixing chamber 1" and fuel supply line 22" to prevent siphoning fuel from tank 60 during times start-up assist is not needed. It will also be appreciated that this simplified form of the invention may be suitable for use on less complicated engines, such as those used in motorcycles or boats, or with engines normally operating in more moderate environments.
With any of the arrangements shown, the preferred air-fuel mixture is in the range from 14 parts air to 1 part fuel, which is stoichometric, to 1 part air to 1 part fuel.
Referring to FIG. 3, another preferred embodiment of the invention is described. The schematic diagram of FIG. 3 depicts a fuel injection combustion system wherein an air intake manifold 14 is employed in a conventional manner to supply air at atmospheric pressure to a combustion chamber 56 through an intake valve 58. A conventional fuel injector valve 6', identical to valve 6 described in connection with FIG. 2, is located in proximity to intake valve 58 and is controlled by a conventional distributor mechanism 13 to spray a pressurized fuel charge into the combustion chamber during the intake cycle when valve 58 is open.
An air-fuel mixing unit 2', which may be identical to the unit 2 shown in FIG. 2, or the unit 2" shown in FIG. 4, is employed to feed a pre-mixed pressurized air-fuel mixture into the injection valve. An air compressor 11', which may be identical to the compressor system described above, supplies pressurized air to the mixing unit 2' via a conduit or pressure line 28'.
A fuel supply line 22' feeds fuel from a fuel supply tank 59 into the air-fuel mixing unit 2'. A low pressure fuel pump 12, similar to that used in conventional carburetion-type internal combustion engines, assures positive delivery of fuel from the tank to line 22'. An individual fuel injector valve 6' is employed with each combustion chamber and the several injectors may be fed by individual air-fuel mixing units 2' or by a single mixing unit having a plurality of output lines feeding all of the injector valves in parallel. As with the system of FIGS. 1 and 2, the air compressor 11' serves as the pressure source for operating the injection valves and consequently the complex high pressure fuel pump used with conventional fuel injection systems is not required. The main supply of air for combustion is the manifold 14 such that air compressor 11' need only be a low cost, low capacity battery-powered unit which is less of an energy drain on the engine system than is the high pressure electric fuel-pump required with present fuel injector systems.
The fuel injection system shown in FIG. 3 operates with improved fuel economy and substantially lower emissions than convention fuel injection systems. The system is even more efficient than the well-known stratified charge engine since the initial rich fuel mixture used in the latter system to improve combustion is not necessary. Furthermore, as in the case of the system shown in FIGS. 1 and 2, the FIG. 3 system operates with improved startup efficiency since the highly atomized, completely mixed air-fuel charge supplied by the fuel injectors 6' enables highly efficient engine startup wherein fuel waste and deleterious emissions are kept to a minimum, as described above.
It will be appreciated that a metering valve can be used in lieu of the preferred Venturi throat to mix the air and fuel. That is, air and fuel can be premixed by transmitting gasoline under pressure into a mixing section and using baffles in the mixing section to ensure the supply of a highly combustible volatile air-fuel mixture to the injector valve. In both cases, air under pressure is used to mix the air and fuel and distribute the mixture to the engine.
FIG. 5 shows a system similar to that depicted in FIG. 1 with modified forms of control circuits for actuating the solenoid valve 10, 34. Also, the FIG. 5 system is shown without the injector valve 6 and check valves 3 and 4, but may incorporate these units if desired.
Solenoid valve 10, 34 is connected by a line 75 into the engine ignition circuit so that when the ignition switch 82 is actuated to start the engine, valve 10, 34 is opened to cause mixed gasoline and air under pressure to be injected into manifold 7 through the air-fuel mixing unit 2 to provide a highly combustible air-fuel mixture in the manner previously described. Circuit 75 is also arranged to connect the compressor drive motor 15 (FIG. 1) to the battery power supply 42 so that air line 28 is pressurized.
The control circuit shown in FIG. 5 includes a gating circuit 76 which activates line 75 only if inputs are also simultaneously supplied from a timing circuit 78 and an engine temperature sensor 80. The latter conditions gating circuit 76 only if the engine is cold, such as may be determined, for example, by a thermocouple unit fixed to the engine block.
Timer circuit 78 conditions gate 76 only for a limited interval, such as two or three seconds, following initial actuation of ignition switch 82. Timer 78 may comprise, for example, a single-shot multivibrator circuit. Thus, circuits 75, 76, 78, and 80 enable automatic control of air-fuel mixing unit 2, eliminating the need for the previously described manual switch. The control circuits furthermore operate to disable the system when the engine is already warm and the injection of the highly atomized start-up mixture is not needed. In addition, timer 78 shuts the system down after a sufficient charge of fuel has been applied, thus preventing fuel waste or engine flooding in the event the operator holds the ignition switch on too long.
FIG. 5 also illustrates a control arrangement that permits the mixing unit of the invention to perform the function presently performed by the mechanical acceleration pump in use on conventional carburetor devices. The accelerator pedal or throttle control 68 is connected by a linkage 70 to the throttle actuator on the carburetor in the usual fashion. A motion sensitive switching device 72 is coupled to linkage 70 by a pivotable arm 73 and the switch 72 is connected via line 74 to the solenoid valve 10, 34 of the apparatus of the invention.
When the operator accelerates by depressing pedal 68, the motion sensing mechanism in switch 72 detects the accelerating action and applies a limited duration signal over line 74 to the valve 10, 34. This activates the system of the invention and causes a charge of highly combustible air-fuel mixture to be pressure-injected into the manifold 7, providing the necessary fuel-feed assist. The complicated, often unreliable mechanical acceleration pump presently in use thus may be eliminated.
Thus, in accordance with the preferred embodiments hereinabove described, it is seen that in accordance with the present invention, a fuel injector valve is utilized having an inlet and further including an outlet nozzle in communication with the intake manifold of the engine. As exemplified in the above described embodiments, the fuel injector valve is illustrated as either of the valves 6 or 6'. Further, air-fuel mixing means are utilized to supply an air-fuel mixture to the injector valve inlet and incorporate means for directing a flow of pressurized air to the inlet through a mixing chamber. As exemplified in the above-described embodiment, the air-fuel mixing means includes the mixing units 2, 2', and 2" with their associated air compressor systems 11 and 11' and supply conduits 28 and 28'. Still further, in accordance with the invention, there is provided means for supplying fuel into the flow of pressurized air whereupon the fuel is mixed with the pressurized air in the mixing chamber. As has been described in connection with the preferred embodiments, the pressure differential generated by the flow of air through Venturi throat 1a draws fuel through Venturi passage 1 a into mixing chamber 1. Still further, the invention contemplates the use of control means for operating the fuel injector valve during engine startup whereby a mixture of air and highly atomized fuel is fed into the engine intake manifold through the injector valve. As exemplified in the embodiments described in connection with FIGS. 1 and 2, the control means includes the electrical control switch 9, leads 38 and 40 and power source 42 which operate to control the coil 50 in the injector valve whereby the pressurized charge of air in line 28 is released through the injector valve to introduce a highly atomized air-fuel mixture into the intake manifold. As exemplified in the embodiment of FIG. 3, the control means includes the distributor mechanism 13.
It can further be seen that, in accordance with the embodiment described in connection with FIG. 3, the invention contemplates the employment of a fuel injector valve and air-fuel mixing means and that as exemplified in the FIG. 3 embodiment, these elements are illustrated as valve 6' and mixing device 2', respectively. Further in accordance with this aspect of the invention there is provided a fuel source including a low pressure pump. As exemplified in the described embodiment, the fuel source includes tank 59, pump 12, and fuel line 22'. Still further, there are provided air supply means and control means for operating the fuel injector valve in synchronism with the operating cycle of the engine. As exemplified in the FIG. 3 embodiment, the air supply means is illustrated as air intake manifold 14 and the control means includes the distributor unit 13.
It will be appreciated that various changes in the form and detail of the above described preferred embodiments may be effected by persons of ordinary skill without departing from the true spirit and scope of the invention. | An air and fuel mixing device incorporates a Venturi throat or other mixing means for feeding a highly combustible mixture of fuel and pressurized air to an electrical fuel injector valve or directly to the intake manifold in a system for starting an internal combustion engine. The system replaces the choke in a conventional electrical ignition type internal combustion engine. The fuel injector valve is controlled to inject a limited quantity of a highly combustible atomized air-fuel mixture into the engine intake manifold during engine startup. Startup is achieved with minimum fuel waste and produces a minimum of exhaust pollutants. A modified form of the invention is shown as employed in a fuel injection type internal combustion engine system wherein high pressure air-fuel mixture is fed to the fuel injectors solely through use of a conventional low pressure fuel pump and air supply. The injectors operate to discharge a highly volatile, combustible, air-fuel mixture under pressure, instead of raw fuel thus significantly increasing combustion efficiency during engine startup to minimize fuel waste and reduce deleterious exhaust emissions. Another modified form of the invention is shown wherein the system is employed to feed a mixture of fuel and pressurized air to the engine intake manifold in response to an acceleration command from the engine throttle control during normal engine operation. This eliminates the need for the notoriously troublesome carburetor accelerator pump now in conventional use. | 5 |
CROSS REFERENCE TO RELATED APPLICATIONS
[0001] This application claims the benefit of priority under 35 U.S.C. §119 of European Application 15 195 415.3 filed Nov. 19, 2015, the entire contents of which are incorporated herein by reference.
FIELD OF THE INVENTION
[0002] The invention relates to a multistage centrifugal pump with a pump casing and with a shaft which carries the impellers of the pump stages and which is rotatably arranged within the pump casing.
BACKGROUND OF THE INVENTION
[0003] Centrifugal pumps of this type and in numerous variants are counted as belonging to the state of the art. In this context, Grundfos pumps (of the Applicant) of the CR series, or Lowara X pumps (of the Xylem concern) of the SV-series are referred to. Such multi-stage centrifugal pumps comprise a common shaft, which carries impellers of pump stages and which is rotatably arranged within a pump casing. Thereby, the drive, in particular with pumps of a larger construction type, is mostly effected via an external motor which is drive-connected to the pump shaft via a coupling. Such pumps are often envisaged for operation with a vertical shaft, and the pump casing therefore comprises a foot part forming the placement surface of the centrifugal pump, as well as a head part designed as a motor stool or comprising such, on which the drive motor is fastened. The pump stages are integrated between the head part and the foot part which are often at least partly manufactured from cast metal, and these pump stages are closed off by a peripheral jacket and are connected to one another via tie rods amid the inclusion of the pump stages. If the centrifugal pump is designed as an inline pump, then on the foot part side it comprises a suction connection and a delivery connection which are offset by 180° to one another. The fluid entering into the pump via the suction connection and running through the individual pump stages is led upwards in each case amid the increase of pressure, where in the head part it is led again to the foot part via an annular channel formed between diffusers and the outer casing, and there to the delivery connection. The shaft carrying the impellers is led out at the motor-side end in a sealed manner. It is counted as belonging to the state of the art, to apply a sealing cartridge in this region, in order to be able to exchange the seal in a quick and simple manner in the case of wear. A bearing can be provided at the other end of the shaft, thus the end which is located within the pump casing. It is also counted as belonging to the state of the art to subject this shaft end to the pressure of the delivery side, in order to hydraulically compensate the axial forces acting upon the shaft. It is then regularly necessary to provide a seal in this region.
[0004] It always requires a certain amount of effort to exchange a seal, a bearing or both in the case of a defect or wear, irrespective of whether these are present individually or both are present. The pump is to be dismantled in large parts for this. The tie rods and further components are to be removed, in order to be able to exchange the bearing and/or the seal at the casing-side end, thus in the region of the foot part. This work is time-consuming and is thus expensive.
SUMMARY OF THE INVENTION
[0005] Against this background, it is an object of the invention, to design a generic multistage centrifugal pump such that the previously mentioned repair and maintenance work is simplified, without the manufacturing costs of the pump being significantly increased by way of this.
[0006] The multi-stage centrifugal pump according to the invention comprises a pump casing, in which a shaft is rotatably mounted, said shaft carrying impellers of the pump stages. The pump casing comprises a reversibly closable maintenance opening, via which a shaft end cooperating part, a bearing which is arranged within the pump casing at the shaft end and/or a seal which is arranged within the pump casing at the shaft end, is accessible and exchangeable.
[0007] A basic concept of the solution according to the invention, it to provide a maintenance opening within the pump casing, typically at the base side, said opening only being opened for maintenance purposes and being sealingly closed on remaining operation, but permitting the control, the maintenance or, as the case may be, the exchange of wear-sensitive components on the shaft end (wear-sensitive shaft end cooperating parts) located within the pump casing, be they a bearing and/or seal, in a targeted manner, without having to dismantle the complete pump, in particular without having to release the tie rods, for this. Such an additional maintenance opening as a rule can be provided with little expense with regard to manufacturing technology, and one merely needs only to provide a component closing this opening, as the case may be amid the integration of a seal, which with regard to the design is mostly possible without any problem. The maintenance opening, as the case may be, can be opened and closed again several times, due to the fact that the maintenance opening is reversibly closable.
[0008] The maintenance opening, in particular if it is arranged on the foot part which is mostly designed as a cast component, can be formed by a simple recess in the base. Such an opening in the simplest form can be closed by a screw-fastened cover. Thereby, it can either be the case of a cover which encompasses (overlaps) the opening and which is fastened by way of fastening screws engaging into the respective casing component laterally of the opening, or however it can be the case of a cover which comprises a thread on its outer periphery, said thread engaging into an inner thread of the opening. The first variant is advantageous with regard to the cost and is simple to seal, by way of a flat seal being integrated between the components or by providing an O-ring with the provision of a cover seal-side or casing-side groove.
[0009] Means for blocking the rotation movement of the shaft are advantageously to be provided, in order to be able to exchange the bearing parts or seal parts which are fastened on the shaft end, for example by way of a screw connection. These means do not necessarily have to be provided on this shaft end, but for example can also be provided on the head of the pump outside the casing, if for example the shaft there has a square or hexagonal profile, onto which a spanner can be placed. A suitable profile for the engagement of a tool can alternatively also be provided at the free shaft end within the casing or, or a transverse bore in the shaft end, through which a blocking pin can be placed.
[0010] It is advantageous to arrange the maintenance opening in the base of the pump casing, if the centrifugal pump is designed for operation with a vertically arranged shaft. However, multi-stage centrifugal pumps which are designed for operation with a horizontally arranged shaft are also known. With these pumps too, it is advantageous to incorporate the maintenance opening in a casing wall in a manner aligned to the shaft, and specifically at the side of the casing which is away from the motor, thus on a wall of the casing which is remote from the motor.
[0011] Basically, it is useful to place the maintenance opening such that the bearing and/or the seal at the shaft end is/are easily accessible. This can be effected by a lateral opening in the casing. However, it is particularly useful for the opening to be aligned to the shaft. Aligned to the shaft is not to be understood in the strict geometric sense, but the opening can also be aligned to the shaft, thus to the shaft axis, in a slightly offset manner, depending on which is more favorable with regard to the design.
[0012] It is particularly advantageous if the cover not only has a purely closing function, but simultaneously fulfils further functions. Thus according to a further development of the invention, the cover can comprise a part which passes through the opening and which receives or forms a rotationally fixed part of the seal or of the bearing. Such an arrangement has the advantage that on removal of the cover, not only is an access to the seal or the bearing at the free shaft end created, but at the same time a part of the seal or of the bearing is formed or is held. Then specifically, a part of the bearing or of the seal is also disassembled already after the disassembly of the cover, which on the one hand simplifies the examining of the condition and on the other hand also simplifies the exchange in the case of a repair. It is then advantageous if the other part of the seal or of the bearing is releasably fastened on the shaft end which is arranged within the pump casing. Thereby, the co-rotating part for example can be fastened by way of a screw engaging into a threaded bore of the shaft end or be placed onto the shaft end and be fixed there by way of a nut.
[0013] It is usually necessary to block the shaft, in order to prevent a co-rotation, for the release of such a screw connection. This in the simple case can be envisaged by a profile which is incorporated on the led-out shaft end, or a transverse bore through the shaft. Basically, it is also conceivable for blocking means to be provided on the motor shaft.
[0014] If the cover according to a further development of the invention is designed such that it overlaps the maintenance opening and is screw-fastened on the pump casing in the overlapping part, then this can be sealed in a simple manner, e.g. by way of a flat seal. The assembly and disassembly is configured in a simple manner, since the screws as a rule are easily accessible given a suitable alignment of the pump. Such an arrangement is then advantageous, in particular if the cover assumes further functions such as for example carrying the stationary part of the bearing or of the seal, since one can ensure adequately large contact surfaces, in order to ensure the required exact alignment of the components to one another. Moreover, the machining of the casing around the cover opening as well as the formation of threaded bores or stud bolts which are provided there can be manufactured in the same chucking on the machine tool. The cover itself can be formed of sheet metal or of cast metal.
[0015] It is particularly advantageous to arrange the maintenance opening within the foot part, preferably on the base side, if the centrifugal pump is designed as an inline pump, whose suction and delivery connections are arranged on the foot part side. Thereby, the centrifugal pump advantageously comprises an axial seal at the shaft end, the stationary part of said axial seal comprising a ring which is arranged in an axially movable manner within the pump casing or within a component integrated therein. Such a design, with which on the one hand a hydraulic pressure impingement of the free shaft end is formed for the compensation of the axial forces acting on the pump shaft and on the other hand a low-friction, but effective axial seal which is less prone to wear is formed, is particularly advantageous. This axial seal can be controlled, overhauled and exchanged in a rapid and simple manner by way of the maintenance opening. Thereby, the stationary part of the axial seal which is axially movably mounted within the pump casing is mounted in the cover, with which the maintenance opening is closed.
[0016] The invention is hereinafter explained in more detail by way of embodiment examples represented in the drawing. The various features of novelty which characterize the invention are pointed out with particularity in the claims annexed to and forming a part of this disclosure. For a better understanding of the invention, its operating advantages and specific objects attained by its uses, reference is made to the accompanying drawings and descriptive matter in which preferred embodiments of the invention are illustrated.
BRIEF DESCRIPTION OF THE DRAWINGS
[0017] In the drawings:
[0018] FIG. 1 is a greatly simplified schematic, longitudinal, sectional view through a multi-stage centrifugal pump of the inline construction type with a drive motor;
[0019] FIG. 2 is an enlarged, longitudinal, sectional view of the pump which is rotated by 90° with respect to FIG. 1 ;
[0020] FIG. 3 is an enlarged representation showing the detail III in FIG. 1 ;
[0021] FIG. 4 is an enlarged representation showing the detail IV in FIG. 2 ;
[0022] FIG. 5 is a longitudinal, sectional view showing the rotating part of the axial seal;
[0023] FIG. 6 is an exploded representation showing the components of the rotating part of the axial seal;
[0024] FIG. 7 is a longitudinal, sectional view showing the non-rotating part of the axial seal with a holding ring for integration into the pump casing;
[0025] FIG. 8 is an exploded representation showing the components of the non-rotating part of the axial seal;
[0026] FIG. 9 is an exploded representation showing the axial seal and the foot part of the centrifugal pump; and
[0027] FIG. 10 is an enlarged view of the centrifugal pump from below.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0028] With the centrifugal pump which is represented by way of FIGS. 1-10 it is the case of a multi-stage centrifugal pump 1 of the inline construction type which is operated in a standing manner. The pump casing comprises a foot part 2 , a head part 3 and a cylindrical jacket 4 which is arranged therebetween and which surrounds the pump stages and is clamped between the head part 3 and the foot part 2 . The foot part 2 comprises a suction connection 5 as well as, aligned to this, a delivery connection 6 . The head part 3 is designed as a motor stool and surrounds a coupling 7 which connects a shaft 51 of an electric motor 50 schematically represented in FIG. 1 and attached on the head part 3 , to a shaft 8 of the pump 1 in a rotationally fixed manner. The shaft 8 of the pump 1 carries the impellers 9 of the pump stages and is rotatably arranged within the pump casing. A radial seal 10 is provided in the head part 3 , and an axial seal 11 is provided in the foot part 2 . The construction of this axial seal 11 is evident in detail from the FIGS. 3 to 8 and is described in a detailed manner further below. Fluid is brought into the pump casing on operation via the suction connection 5 , when the shaft 8 rotates, and this fluid enters into the suction port 12 of the first pump stage and is delivered through the pump stages which are formed in each case by an impeller 9 and a surrounding diffuser 13 , until it exits from the last pump stage in the head part 3 and is led back via an annular channel 14 to the delivery connection 6 , through which the fluid leaves the pump again.
[0029] The casing-side shaft end 15 of the pump in the region of the suction port 12 lies below the first pump stage. It comprises a pocket-hole bore 16 which is provided with a thread and in which a cap screw 17 is seated, with which cap screw a holding ring 18 is sealingly and fixedly fastened on the shaft end 15 . The holding ring 18 comprises a wall 19 which is directed to the suction port 12 and is closed with the exception of a central recess for leading through the screw 17 , thus is designed in a pot-like manner and is fixedly connected to the shaft end 15 in a sealed manner.
[0030] The holding ring 18 is designed as a turned part, is stepped to the side which is away from the shaft end 15 and is formed with a peripheral groove which is open to the bottom and which is provided for receiving a rotating ring 20 . The rotating ring 20 consist of silicon carbide and is rotationally secured in the holding ring 18 by way of pins 21 and is otherwise fastened together with the holding ring 18 on the shaft end 15 , by way of a sleeve 22 which radially encompasses the rotating ring 20 on the inner side and by way of the screw 7 . The rotating ring 20 comprises a downwardly directed axial surface 23 thus which is directed away from the shaft end 15 and this surface forms the rotating axial surface of the axial seal 11 . This axial surface 23 is not completely planar, but comprises three macroscopic prominences which are uniformly distributed over the periphery and which on the one hand form a defined contact on the counter-surface 24 , which is to say on the axial surface 24 of the non-rotating axial seal part 25 , and on the other hand serve for the rapid build-up of the lubricative film. The axial surface 24 is designed in a planar manner and is part of the non-rotating part, here of the ring 25 which is arranged in an axially movable manner within a holding ring 26 integrated in a corresponding receiver in the lower side of the foot part 2 of the pump casing.
[0031] The holding ring 26 comprises a peripheral groove 27 on its inner side, in which groove an O-ring 28 is integrated, said O-ring radially sealing the ring 25 with respect to the holding ring 26 and thus with respect to the pump casing. The holding ring 26 is moreover yet sealed with respect to the receiver in the pump casing by way of an outer-peripheral seal 58 , as is evident from the sectioned representations 4 and 7 .
[0032] The non-rotating ring 25 at the rear side which is away from the axial sealing surface 24 is covered by a sheet metal section 29 which almost completely covers this rear side of the sealing ring 25 . The sheet-metal section 29 comprises bent-over tongues 30 , with which the sheet metal section is integrated within corresponding recesses 52 on the rear side of the ring 25 with a positive fit. These tongues 30 project radially beyond the ring 25 and engage into these recesses 52 in the ring 25 and form part of a rotation lock of the non-rotating ring 25 . Moreover, the sheet-metal section 29 comprises two diametrically opposite tongues 31 which are offset by 90° to the tongues 30 and which are bent away upwards out of the plane of the main material by 90° and connect the sheet-metal section 29 in an axially distanced manner to the ring 25 , in which the ends 53 engage into a shoulder 54 on the inner side of the ring 25 in a locking manner.
[0033] The sheet-metal section 29 forms a closed surface of the lower side of the ring 25 and comprises a central rectangular recess 32 , into which a pin 55 which is rectangular in cross section engages, said pin forming part of the holding ring 26 , on which the ring 25 comprising the axial sealing surface 24 is guided in a rotationally fixed, but axially movable manner. The pin 55 and the recess 32 with regard to cross section are dimensioned such that this recess 32 with the pin 55 located therein, together with any gap tolerances of the sheet-metal section 29 form a through-gap with a cross-sectional area which is significantly smaller than the cross-sectional area of channels 33 which are provided in the foot part 2 of the pump casing or in the holding ring 26 and which ensure that the interior 34 of the ring 25 with the sheet-metal section 29 and the holding ring 26 is subjected to the pressure of the delivery side of the pump, thus to the pressure at the delivery connection 6 . These channels 33 , on starting up the pump after an effected pressure build-up ensure that the sheet-metal section 29 with the ring 25 bearing thereon is firstly subjected to force and is pushed, in the direction of the free shaft end, thus towards the motor, since firstly fluid must flow via the smaller cross section of the gap between the recess 32 and the pin 55 , into the space enclosed by the ring, before a corresponding counter-pressure is built up. The ring 25 is moved axial upwards in FIG. 1 , which is to say is moved axially within the holding ring 26 by way of this, until the axial surface 24 bears on the counter-surface 23 , by which means a separation between the suction-side space in the region of the shaft end 15 and the installation space 34 of the stationary part of the axial seal 11 is then also formed. The pressure of the delivery side also prevails within the ring 25 and this at the face side of the shaft 8 , as soon as the space which is enclosed by the ring 25 and the sheet-metal section 29 has filled via the gap of the recess 32 , by which means the certain force compensation with regard to the hydraulically caused axial force of the shaft 8 and which is desired on operation is effected.
[0034] As can particularly be deduced from FIG. 9 , the holding ring 26 is part of a circular disc 56 which is provided for integration in a base-side maintenance opening 60 of the pump casing, here of the foot part 2 . The disc 56 , in a manner closing this base-side opening 60 , lies in a shoulder 64 on the lower side of the foot part 2 and is releasably connected to the foot part 2 via four screws 57 which are led through recesses 61 in the edge 62 of the disc 56 . An O-ring 58 which is integrated in a peripheral radial groove of the ring 26 and serves for sealing this component with respect to a recess 63 in the foot part 2 , is arranged in the upper region of the ring 26 , thus at a small distance to the disc 25 , for sealing with respect to the foot part 2 . A second O-ring 59 is integrated at an axial distance to this, in a peripheral, radial groove in the lower part of the ring 26 and serves for sealing with respect to the maintenance opening 60 in the foot part 2 . A connection to the delivery side of the centrifugal pump 1 which is connected in a fluid-leading manner to the interior of the ring 26 via channels 33 in the ring 26 , connects within the foot part 2 , between the O-rings 58 and 59 , so that the pressure of the delivery side via this connection is present at the surface of the non-rotating part 25 of the axial seal, said surface being formed by the sheet-metal section 29 and at the beginning being pressure-effective. The ring 26 via the O-ring 28 lying in a groove on the inner side of the holding ring 26 is sealed with respect to the ring 25 which forms the non-rotating part of the axial seal with the axial surface 24 of the seal. This O-ring 28 thus forms a radial seal which however only has to accommodate the comparatively small movements in the axial direction and therefore is only subjected to a low wear.
[0035] The axial seal can be overhauled and exchanged as the case may be, by way of removing the disc 56 with the holding ring 26 which is located thereon, after the screws 57 have been released, due to the fact that the pump casing at the lower side, thus in the base of the foot part 2 , comprises a maintenance opening 60 which is closed by the disc 56 . The shaft 38 of the pump does not have to be removed for this. All components of the axial seal which are represented in the exploded representation according to FIG. 9 can be exchanged through the opening 61 in the base of the foot part 2 . An exchange of the components comprising the axial surfaces 23 and 24 as well as of the O-ring 28 is effected in the simplest case. The shaft 8 in the region of the motor stool has a cross-sectional profile which permits a locking of the shaft by way of laterally engaging a tool, in order to be able to release the threaded connections which are connected to the shaft 8 . Thus the cap screw 17 can be released after the shaft 8 is held in a rotationally fixed manner by way of a spanner introduced in the region of the motor stool, and this screw can then be tightly screwed again after exchange of the rotating ring 20 and, as the case may be, further seals of the holding ring 18 .
[0036] The axially stationary part of the seal, thus the non-rotating ring 25 with its seals and the holding ring 26 which with the disc 56 forms the cover for closure of the casing opening of the maintenance opening 60 , together with the cover 56 are pulled out downwards and thereby the upper part of the holding ring 26 with the peripheral O-ring 58 is pulled out of the recess 63 , and the lower part of the holding ring 26 with the O-ring 59 is pulled out of the maintenance opening 60 . These seals as well as the O-ring 28 and the non-rotating part of the axial seal 25 can then be exchanged and together are inserted from below into the maintenance opening 60 or the recess 63 of the foot part 2 , until the upper part of the holding ring 26 with the O-ring 58 sealingly bears in the recess 63 and the lower part with the O-ring 59 sealingly bears in the maintenance opening 60 .
[0037] The exchange of the axial seal at the lower shaft end is described above, however it is to be understood that according to the invention, a bearing which is provided between the shaft and the casing can also be exchanged in an analogous manner, without the shaft having to change its position within the pump casing and thus extensive disassembly and assembly activities becoming necessary.
[0038] While specific embodiments of the invention have been shown and described in detail to illustrate the application of the principles of the invention, it will be understood that the invention may be embodied otherwise without departing from such principles.
APPENDIX
List of Reference Numerals
[0000]
1 —centrifugal pump
2 —foot part
3 —head part
4 —jacket
5 —suction connection
6 —delivery connection
7 —coupling
8 —shaft
9 —impellers
10 —radial seal
11 —axial seal
12 —suction port
13 —diffuser
14 —annular channel
15 —shaft end
16 —pocket-hole bore
17 —cap screw
18 —holding ring
19 —wall
20 —rotating ring
21 —pins
22 —sleeve
23 —axial surface
24 —axial surface
25 —non-rotating part of the axial seal, ring
26 —holding ring
27 —groove
28 —O-ring
29 —sheet-metal section
30 —tongues
31 —tongues
32 —recesses in 29
33 —channels in ring 26
34 —interior of 25
35 —outer thread
36 —nut
37 —sleeve
38 —shaft
50 —motor
51 —motor shaft
52 —recesses in ring 25
53 —ends of the tongues 31
54 —shoulder in ring 25
55 —pin
56 —disc/cover
57 —screws
58 —O-ring
59 —O-ring
60 —maintenance opening
61 —bores for the screws 57
62 —edge of cover
63 —recess
64 —shoulder in foot | A multi-stage centrifugal pump includes a pump casing, in which a shaft ( 8 ) carrying an impeller is rotatably arranged. The pump casing has a pump casing foot part ( 2 ) that includes a reversibly closable maintenance opening ( 60 ), via which a bearing and/or seal ( 20, 25 ), which is arranged at a shaft end within the pump casing, is accessible and exchangeable. | 5 |
BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention relates to automatic washing machines of the vertical axis type and more particularly to a filter system for such automatic washing machines.
2. Description of the Prior Art
U.S. Pat. No. 4,075,876 describes the problem occurring during the agitation and scrubbing of clothing articles in an automatic washing machine when particles of lint are developed from the fabrics being cleaned and become suspended in the laundry liquid. Such lint particles must be removed from the laundry liquid during the washing cycle, otherwise they will be redeposited on the articles being laundered in later steps of the washing program.
It is also known that sediment and debris particles are also removed from clothing articles during the agitation and scrubbing of the clothing articles. Such sediment and debris particles tend to gravitate to the bottom of the washing basket or washing tub.
In one form of automatic washer manufactured and sold by applicants' assignee, the motor in the washing machine is reversed after the agitation cycle and the drain pump is actuated to drain the basket and tub of laundry liquid. At the same time the basket is driven in rotation for the spin cycle or centrifuging mode. Such a cycle sequence is sometimes referred to as a direct-into-spin system because the basket begins its spin cycle before the washing liquid has been drained therefrom.
Such a direct-into-spin system can cause a pressure gradient forcing the laundry liquid from the tub through openings in the bottom of the basket and outwardly through the clothes, thus distributing sediment and debris particles that have settled within the tub on the clean clothes.
U.S. Pat. No. 3,352,130 discloses a filtering arrangement in an automatic washer wherein liquid is pumped from a tub to a closed receptacle or basket by the pumping action of an agitator oscillating within the basket during the washing cycle. Liquid enters the basket from the tub through openings in the bottom of the basket, and liquid circulates from the basket to the tub through perforations in the basket side wall.
Filter elements mounted in the openings in the bottom of the basket collect the lint carried by liquid passing through the openings, and the lint thus collected is thrown off and carried to drain when the basket spins during the centrifuging mode of machine operation. A row of holes is provided in the bottom wall of the basket for permitting sand and other sediment to pass from the basket to the tub. This row of holes formed in the bottom wall of the basket permits unfiltered communication between the basket and the tub. Operating such a structure with a direct-into-spin cycle would allow the deposited sand and sediment particles to reenter the basket area through these holes to be redeposited on the laundered articles.
SUMMARY OF THE INVENTION
A truncated filter cone constructed of a rigid material such as polypropylene is fastened beneath the bottom of a clothes basket, by means of a plurality of fingers at the top of the cone having buttons on the ends thereof being received in holes formed in the hollow center post portion of the basket. The filter cone comprises a generally truncated conical shape which is positioned adjacent the bottom wall of the basket near the upper end of the cone and is spaced from the bottom wall of the basket at the lower end of the cone. The lower end or periphery of the cone has upwardly and outwardly extending rigid teeth spaced closely subjacent the bottom wall of the basket along a generally circular line.
As a pumping agitator mounted in the basket draws liquid along a path radially inward from the periphery of the tub sump beneath the basket, lint carried by the liquid is trapped on and between the teeth of the filter cone. The liquid is drawn through apertures in the bottom wall of the basket and into the basket through the agitator. The liquid then flows outwardly through a side wall in the basket and downwardly toward the sump to repeat the cycle.
During the direct-into-spin portion of the cycle, a pressure differential is established by the spinning of the basket, tending to cause laundry liquid to flow back into the basket through the openings in the bottom wall. During this portion of the cycle, the rotating rigid filter teeth provide a pumping action to oppose this flow and along with the conical shape of the filter prevent sand or sediment from returning to the basket to be deposited on the clothing.
As the water level within the tub is decreased by the drain pump the pumping action of the filter teeth causes water flow outwardly from the basket through the openings in the bottom of the basket, thereby automatically cleaning the filter teeth. The lint then moves to drain from the tub along with the laundry liquid, thus automatically effecting a cleaning of the filter without manual intervention.
DESCRIPTION OF THE DRAWINGS
FIG. 1 is a perspective view of an automatic washing machine with parts broken away to show the mechanical parts of a washing machine including a tub with a vertical agitator and embodying the principles of the present invention.
FIG. 2 is a fragmentary cross sectional view with parts shown in elevation taken generally along line II--II of FIG. 1.
FIG. 3 is a cross sectional view taken generally along the line III--III of FIG. 2 showing the plan view of a filter cone.
FIG. 4 is a partial side elevational view of the filter cone taken generally along the lines IV--IV of FIG. 3.
FIG. 5 is a cross sectional view of the filter cone taken in the plane of line V--V of FIG. 3.
FIG. 6 is a plan view of a filter cone embodying optional features of construction.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
In FIG. 1 a washing machine is generally shown at 10 as having a tub 12 and a vertical agitator 14 therein, a water supply (not shown), a power supply (not shown), an electrically driven motor 16 operably connected via a transmission 18 to the agitator 14, and controls 20 including a pre-settable sequential control means 22 for use in selectively operating the washing machine 10 through a selected programmed sequence of washing, rinsing and spinning or extracting steps.
FIG. 2 shows a cross sectional view of the interior of the tub 12 which shows a concentrically mounted perforate basket 24 having a side wall 26 and a bottom wall 28. The bottom wall slopes upwardly from the outer circumference at the side wall 26 to a center post portion 29. A plurality of openings 30 are formed in the side wall 26 and a series of openings 32 are formed in the bottom wall 28 adjacent the center post portion 29 thereof.
The tub 12 is comprised of an imperforate side wall 36 and a generally imperforate bottom wall 38 having a single drain opening 40 formed in a sump portion 42 of the bottom wall 38. The agitator 14 has a plurality of vanes 44 extending radially from a central vertical portion 46 thereof. The vanes 44 may have flexibility if so desired. The agitator vertical portion 46 is concentrically mounted about the basket center post 29 and is driven by an agitator drive shaft 47 by means of a conventional spline connection (not shown).
A skirt portion 48 of the agitator 14 is provided below the flexible vanes 44 and includes a pumping means 50 comprising radial vanes located beneath the skirt portion 48 by which the agitator pumping means 50 pumps laundry liquid outwardly upon each oscillation of the agitator 14. The openings 32 in the bottom wall 28 of the basket are located below and near a radially inward end 52 of the pumping means 50 of the agitator such that laundry liquid is drawn up through openings 32 and is caused to flow radially outwardly through pumping means 50 by the centrifugal force imparted by the oscillating agitator 14.
Liquid flows out from under the skirt 48 as at arrow 54 to enter the basket 24 and then flows outwardly through the holes 30 in the basket side wall 26 as at arrows 56 and downwardly past the sump portion 42 of the tub radially inwardly along the underside of the basket bottom wall 28 as at arrows 58 to return to the interior of the basket 24 through openings 32. As the laundry liquid passes in this liquid circuit, sand and other heavy dirt particles or debris are generally deposited along the sump portion 42 of the tub 12.
A conical filter means or element 60 is provided between the sloping bottom wall 28 of the basket 24 and the bottom wall 38 of the tub 12. The cross sectional shape of the filter element is best seen in FIG. 5. The filter element 60 is attached to the basket 24 by means of a plurality of fingers 62 which extend radially upwardly at a top end 63 of a conical wall 64 which forms the main body of the filter element 60. The fingers 62 have radially protruding buttons 65 formed at a top end thereof which are received through complementary shaped openings 66 in the basket center post 29 as best seen in FIG. 2.
A groove 68 is formed on the interior side wall 70 of the buttons 65 to receive a retaining ring 72 which urges the fingers 62 and buttons 64 in a radially outward direction to retain buttons 65 in the openings 66 of the center post 29. The finger portions 62 of the cone filter element 60 merge with the conical wall 64 in a generally curved manner as at 74 where the conical wall 64 is in close proximity to the bottom wall 28 of the basket 24.
As the conical wall 64 progresses radially outwardly from merger point 74, it is sloped downwardly at a greater angle than the slope of the bottom wall 28 of the basket 24 such that a lower end 76 of the conical wall 64 is spaced from the bottom wall 28 of the basket 24. To maintain this spaced relationship, a plurality of steps 78 are provided in the conical wall 64 to abut against the bottom wall 28 of the basket 24.
A plurality of teeth 80 are provided at the lower end 76 of the conical wall 64 which extend radially outwardly to a position closely subjacent the bottom wall 28 of the basket 24 leaving an opening 81 there between. In accordance with this invention, the teeth 80 are made rigid. Thus, the teeth 80 form a stable barrier between a first tub region or chamber 82 located radially inward of the teeth 80 and above the conical wall 64 and a second tub region or chamber 84 radially outward of the teeth 80. The first tub region or chamber 82 comprises an annular passageway between the second tub region or chamber 84 and the openings 32 leading into the basket 24 which is bounded on an upper side by the basket bottom wall 28 and on the lower side by the conical wall 64.
When the agitator 14 oscillates, the pumping means 50 pumps liquid radially outwardly on the interior of the basket 24 along the bottom wall 28 of the basket. The liquid then flows upwardly through the basket and out through the openings 30 in the side wall 26 of the basket 24 into the second tub chamber or portion 84. The liquid passes the sump portion 42 and then flows between and over the filter teeth 80 into the first tub portion or chamber 82 and back through the openings 32 in the bottom wall 28 of the basket 24 to repeat the cycle. Any lint suspended in the liquid is retained against an outside surface 86 of the teeth preventing the lint from being redeposited on the laundered articles.
When the washing cycle progresses into a direct-into-spin portion of the cycle spinning the basket 24 and thus the filter element 60, a pressure gradient, as shown by line 87 in FIG. 2, results in the liquid wherein the pressure along the tub bottom wall 38 is greatest at the side wall 36 and lowest adjacent the agitator center post 14. This pressure difference or gradient would normally cause a flow of water radially inwardly along the tub bottom wall 38 tending to result in a return flow into the basket 24 through openings 32. The rotating rigid filter teeth 80, however, provide a pumping action opposing flow from the tub through the teeth and inwardly through openings 32 into the basket. There is thus no flow into the basket through openings 32. As the water level in the basket decreases, the pumping action of the teeth 80 causes an increased flow outwardly from the basket, through openings 32 and teeth 80 into the tub 12. Thus, the rotating rigid filter teeth 80 and the conical wall 64 provide a barrier which prevents the sediment and debris which has accumulated in the sump portion 42 from returning to the basket 24.
When the water level in the tub 12 is sufficiently decreased by passage of liquid through the drain 40, the pumping action of the filter increases due to the reduced pressure at side wall 36. The flow of water increases through the holes 32 in the bottom wall 28 of the basket 24, flowing radially outwardly between the teeth 80, to thereby aid the centrifugal force created by the rotation of the filter element 60 in cleaning the lint and debris from the outer surface 86 of the teeth 80. The annular opening 81 allows any lint or debris in region 82 to pass outwardly into region 84. Such lint and debris in region 84 is carried by the draining liquid through the drain 40 with the waste water.
As seen in FIG. 3, the teeth 80 may be formed in a direction extending radially outwardly from the agitator drive shaft 47. The steps 78 are provided at sufficiently spaced apart locations to allow for unimpeded flow along the conical wall 64 as the wash liquid travels between the teeth 80 and the openings 32 in the basket bottom wall 28.
A side elevational view of a portion of the filter cone 60 is shown in FIG. 4 showing the relationship between the filter teeth 80 and front surfaces 86 thereof, the lower end 76 of the cone wall 64 and the steps 78.
An alternative embodiment of the invention is shown in FIG. 6 wherein an alternative cone filter element 600 is shown having teeth 800 formed at an angle A with respect to radial lines projecting from a conical center 810.
Although a filter cone having fingers of a configuration like those shown in FIGS. 3 and 6 is preferred, it will be understood that many different forms of filtering barriers and many different configurations of lint collecting teeth could be effectively utilized within the scope of our invention. While these and other various modifications might be suggested by those versed in the art, it should be understood that we wish to embody within the scope of the patent warranted hereon all such modifications as reasonably and properly come within the scope of our contribution to the art. | A filter cone fixed to the bottom of a washing machine basket includes a plurality of closely spaced rigid teeth in a circumferential row extending outwardly and upwardly to divide the tub into first and second chambers for filtering laundry liquid during a washing cycle and for preventing sediment and debris from returning into the basket during a direct-into-spin portion of the wash cycle. The reverse flow of water through the filter teeth during the drain portion of the washing cycle effects self-cleaning of the teeth. | 3 |
CLAIM OF PRIORITY
The present invention claims priority to provisional U.S. Application No. 61/831,370 filed on Jun. 5, 2013, entitled “Enhanced Environment Simulator for Proxy Robot Handlers.”
FIELD OF THE INVENTION
The present claimed invention generally relates to robotics. More specifically the present invention relates to human proxy robot systems and environment simulators for the human handlers of proxy robots.
BACKGROUND OF THE INVENTION
This specification is about human telepresence in space. During his or her turn in control of a given proxy robot, the human handler sees and feels and acts through the “person” of that robot: guiding the proxy in exploring; mining; doing science experiments; constructing; observing the earth, planets or stars; launching spaceships to further destinations; rescuing other robots or humans; or simply enjoying an earthrise over the moon's horizon. To maximize this interface, the human handler should have access to an environment simulator that replicates the conditions of the proxy robot's remote location to the greatest possible extent.
In the prior art are several patents dealing with omni-directional and spherical treadmills, all involving simulated virtual reality (VR) generated by a computer program as opposed to the simulation of the actual environment being experienced by a proxy robot in its remote environment as taught in the present invention. Carmein U.S. Pat. No. 5,562,572 discloses ways to make an omni directional treadmill for VR and other purposes, but the methods and apparatus employed do not anticipate the specification to follow. Nor are his treadmill designs very stable, with the human constrained by balance cuffs, support struts, hand grips and the like just to stay upright.
Carmein '572 also makes brief mention of how the omni-directional treadmill of his invention may be utilized in telepresence in a one-paragraph description of FIG. 18 (FIG. 39 in C.I.P. '256 below), but fails to claim or adequately teach how a human can be productively linked in practice to a robot in some remote location. In the present specification and a companion application pertaining to handler environment simulation, prior art weaknesses, defects and “science fiction” will be overcome as methods and apparatus for a complete human handler-proxy robot system are disclosed.
Latypov U.S. Pat. No. 5,846,134 features a spherical shell inside of which a human walks in treadmill fashion, but this concept is quite distinct from the spherical treadmill disclosed in the current application, where the human handler of a proxy robot stands and moves on the top exterior of a sphere with diameter sufficiently large (typically 30 feet in diameter) that the handler, to all intents and purposes, is moving on a flat surface if that is the remote terrain being simulated.
U.S. Pat. No. 5,980,256, also by Carmein, is a continuation-in-part of '572 above and U.S. Pat. No. 5,490,784. The latter pertains to spherical capsules within which humans can walk (albeit uphill) in any direction, but does not apply to the present invention. The circular form in Carmein's ('256) FIG. 23 does not denote a turntable, but rather defines a circular track unlike the current invention. While Carmein's FIG. 37 and description are somewhat akin to the motion simulator in the current specification's FIG. 7, the point is moot in any case since such motion simulators are well-established in the prior art.
Butterfield U.S. Pat. No. 6,135,928. This patent, which expired in 2008, discloses a spherical treadmill for VR gaming, but it is so small at 6-7 ft. diameter as to never seem flat to its human “rider,” who requires a restraining harness and support system just to stay upright. In the Butterfield patent, the sphere basically represents a human-powered trackball, operating in exactly that manner to input x- and y-axis orientation and movement to a VR game on a computer.
Put another way, Butterfield's focus is virtual reality, for fantasy games, while the application below is all about the best-possible simulation of actual reality in a remote location. As a consequence, the Stephens specification does not utilize a small, inflatable sphere as a computer trackball or mouse as taught by Butterfield, but rather uses a much larger and firmer motor-driven spherical treadmill to replicate the terrain upon which a proxy robot is walking, climbing or carrying out various tasks. (Butterfield does depict how a “hill” can be created by moving the user off-center, but the problem with such a small sphere is that there is a constant “hill” created by the small-diameter sphere itself.)
These and other distinctions over the current art will become evident from study of the specification and drawings to follow, which discloses novel systems, methods and apparatus to simulate the environment present at the proxy robotic mission site and thus assure the best possible outcome for that mission.
OBJECTS OF THE INVENTION
One object of the present invention is to describe a viable methodology for human space exploration utilizing proxy robot surrogates in space controlled by humans in environment simulators on earth or elsewhere.
A second object of the present invention is to provide human telepresence on the moon and other locations near earth utilizing proxy robots capable of being controlled by one or more human handlers in real or approximated real time.
A third object of the present invention is to achieve human telepresence on the moon and other locations in space utilizing proxy robot surrogates for humans in simulated environments back on earth or at some other location.
A fourth object of this invention is to provide a viable methodology for space exploration utilizing proxy robots, proxy robot-driven vehicles and robotic vehicles in space controlled by humans on Earth, including a terrain analysis computer which generates an approximated real time video display that allows the human handler to control the movements of each robot or robotic vehicle, as well as data streams representing “terrain just ahead”, handler heading, handler step distance, and handler step moment which are fed to circuitry to turns said data into signals to drive motors controlling the roll, pitch and yaw of an environment simulator to maximize the reality of the human handler's environment as the handler controls every move of a remote proxy robot.
A fifth object of this invention is a method and apparatus for the establishment of a surveillance grid through the provision of a plurality of pole cameras which can be dropped onto a body in space from an orbiting spacecraft, satellite, or a balloon or other aircraft.
A sixth object of the present invention is to provide a treadmill for the human handler with provision for changing the pitch and roll of the treadmill to match conditions in the remote location of the proxy robot, where pitch, roll and other positional data are continually adjusted in the handler environment by mechanisms driven by a computer that continually analyzes video and other data from the proxy robot and its remote environment.
A seventh object of the present invention is to provide a method and apparatus for a circular treadmill utilizing a plurality of conveyors to maintain a human handler centered in a simulator staging area.
An eighth object of this invention is further to object seven, wherein an array of cylinders, each housing one or more ball bearing feet and capped with a tile in the shape of an equilateral triangle, can be impelled to move in treadmill fashion along various axes on a staging area.
A ninth object of this invention is further to the circular treadmill of object seven, wherein data representing human handler heading, step distance and step moment is analyzed by a computer that send appropriate signals to the various conveyor mechanisms that constitute the circular treadmill to compensate for handler movement by re-centering the handler on the stage.
A tenth object of this invention is a method and apparatus for varying the pitch and roll of a treadmill by housing that treadmill and a human proxy robot handler in a modified or custom made motion simulator, complete with gravity harness and large video screen, and wherein pitch and/or roll can be modified by signals from a computer that act to vary the length of four or more large hydraulically extending arms supporting the motion simulator, said computer continually monitoring and analyzing video and other data from the remote environment of a proxy robot.
An eleventh object of the present invention is a method and apparatus for varying the momentary elevation as well as the pitch and roll of a vehicle simulator in time with the actual movements and aspect of a vehicle in a remote or off-earth location operated by at least one proxy robot, wherein the vehicle's elevation, pitch and roll are controlled by hydraulic means in communication with data from the remote location signifying the pitch, roll and such path conditions as roughness, bumps and obstacles experienced by the off-earth vehicle; and “follow me” commands from human handler motion sensing means and control monitoring means located within the vehicle simulator to guide the every move of the proxy robot operating the said remotely-located vehicle.
A twelfth object of the present invention is the provision of an environment simulator including a treadmill with variable pitch and roll and infinitely variable heading; wherein the treadmill takes the form of a large sphere which rests upon several large bearings and is rotated by a plurality of rollers in contact with the surface of the sphere so as to turn the sphere in any direction when commanded by circuitry monitoring both the steps of a human handler and the pitch and roll of terrain immediately ahead in the remote location.
A thirteenth object of the present invention is further to object twelve, wherein the spherical treadmill itself moves the handler to a location on the surface of the sphere which exhibits pitch and roll matching terrain conditions in the remote location of the handler's proxy robot.
A fourteenth object of the present invention is further to object twelve, with the added feature of the simulator receiving data from sources on the “person” of the proxy robot as well as surveillance video and stored information from other sources at the remote site that can be analyzed to maximize the simulated environment experience of the handler.
A fifteenth object of the present invention is the provision of a spherical treadmill environment simulator as in object twelve above, wherein the handler is performing tasks in approximated real time such that the handler's “follow me” commands anticipate the position of a proxy robot at some time in the future due to path delay.
A sixteenth object of the present invention is to create an accurate simulation of the terrain in a remote environment by analyzing that terrain on a computer; computer-generating a three-dimensional bar chart of the terrain; and producing a physical rendering of that bar chart by mechanical means.
A seventeenth object of the present invention is further to object fifteen, wherein the mechanical means constitute piston rods that extend and retract hydraulically from signals received by the computer that generates the three-dimensional bar chart.
SUMMARY OF THE INVENTION
Disclosed herein are apparatuses that provide simulation of remote environments in order to enable control of a robotic device in the remote environment.
Pursuant thereto an omnidirectional treadmill environment simulator is disclosed. The omnidirectional treadmill environment simulator includes a circular simulator stage area, a plurality of transport mechanisms that maintain an object at or near the center of a circular simulator stage area and at least one processor. The processor is configured to collect position data of the object and process the position data to control the transport mechanisms. Also included is a receiver for receiving data from a remote location and a terrain analysis computer for processing the data received from the remote location. The terrain analysis computer collects the data received from the remote location to form an accurate simulation of an upcoming condition at the remote location. The omnidirectional treadmill environment simulator includes a transmitter for transmitting the position data to a remote location.
Further disclosed is a remote vehicle simulator. The remote vehicle simulator includes a plurality of extendable legs configured to extend and contract to simulate the contours of a surface terrain of a remote location. The remote vehicle simulator also includes a terrain analysis computer, wherein the terrain analysis computer is configured to receive terrain data of the surface terrain of the remote location and wherein the computer is enabled thereby to construct upcoming terrain conditions for use in the remote vehicle simulator and a processor that is configured to receive terrain data of the surface terrain of the remote location. The processor processes the terrain data to control the plurality of extendible legs to simulate the surface terrain of the remote location. The processor is also configured to collect operational data of a vehicle mounted on the plurality of extendible legs. The terrain analysis computer receives terrain data of the surface terrain of the remote location and the computer is enabled thereby to construct upcoming terrain conditions for use in the remote vehicle simulator and the simulator includes a transmitter for transmitting the operational data to a robotic device at the remote location.
Further disclosed is an omnidirectional treadmill environment simulator in which the circular simulator stage is a spherical platform. The spherical platform includes an upper support from which the spherical platform protrudes through a circular opening in the upper support, a boundary between the spherical platform and the upper floor which facilitates movement of the spherical platform and a lower support upon which the spherical platform rests and allows the spherical platform to rotate with a minimal of resistance.
Further disclosed is an immersive environment simulator apparatus that includes a plurality of cylindrical telescoping piston mechanisms configured to extend and retract to simulate a three-dimensional physical terrain and a computer that receives data of an actual physical terrain and generates a data matrix of the simulated three-dimensional physical terrain. A control unit is included that is in communication with the computer that provides commands to the plurality of the cylindrical telescoping piston mechanisms to extend and/or contract the plurality of the cylindrical telescoping piston mechanisms to correspond to the simulated three-dimensional physical terrain and a plurality of tiles resting on each of the plurality of the cylindrical telescoping piston mechanisms upon which an object is placed. Furthermore, the received data is continuously streamed such that as the object moves along the simulated three-dimensional physical terrain provided by the plurality of the cylindrical telescoping piston mechanisms, the object movement along the simulated three-dimensional physical terrain mimics the actual physical terrain.
DESCRIPTION OF THE DRAWINGS
FIG. 1A is an illustration of a perspective view of an exemplary apparatus for achieving a novel “circular” or omnidirectional treadmill incorporating three two-way conveyor mechanisms;
FIG. 1B is an illustration of an exemplary plane view of an apparatus for achieving a novel “circular” or omnidirectional treadmill incorporating three two-way conveyor mechanisms;
FIG. 1C is an illustration of an exemplary plane view of a conveyor mechanism;
FIG. 1D is an illustration of an exemplary perspective view of a circular treadmill incorporating three two-way conveyor mechanisms;
FIG. 1E is an illustration of an exemplary elongated gear of a roller transport mechanism;
FIG. 1F is an illustration of a tile with ball bearing cylinder;
FIG. 1G is an illustration of a tile with a bearing housing including a lower profile cylinder;
FIG. 1H is an illustration of an exemplary partial plane view of a conveyor mechanism;
FIG. 2A is an illustration of an exemplary perspective view of a circular treadmill showing a mesh of individual equilateral triangular tiles;
FIG. 2B is an illustration of an exemplary perspective view of a circular treadmill highlighting an active conveyor;
FIG. 2C is an illustration of an exemplary perspective view of a circular treadmill highlighting another active conveyor;
FIG. 2D is an illustration of an exemplary perspective view of a circular treadmill highlighting still another active conveyor;
FIG. 2E is a block diagram of exemplary motor control and processor electronics for a three-conveyor circular treadmill;
FIG. 2F is a perspective view of a circular treadmill with one conveyor in motion and out of alignment;
FIG. 2G is a magnified illustration of tile misalignment;
FIG. 2H is a perspective view of a circular treadmill with one conveyor in motion and slightly out of alignment;
FIG. 2J is a magnified illustration of slight tile misalignment;
FIG. 2K is a perspective view of a circular treadmill with all conveyors stopped and in alignment;
FIG. 2L is a magnified illustration of complete tile alignment;
FIG. 2M is a plane view of a conveyor illustrating several alignment means;
FIG. 2N is a magnified illustration of a conveyor stop mechanism;
FIG. 2P is an illustration of a perspective view of an exemplary apparatus for achieving a novel “circular” or omnidirectional treadmill incorporating two two-way conveyor mechanisms;
FIG. 2Q is a block diagram of exemplary motor control and processor electronics for a two-conveyor circular treadmill;
FIG. 3 is a plane view of a treadmill with hydraulic aspect control including exemplary control electronics;
FIG. 3A is a plane view of an omnidirectional “circular” treadmill with variable pitch and roll including exemplary control electronics;
FIG. 3B is a block diagram including plane view illustrations of an exemplary simulator for the control and operation of an extra-terrestrial land vehicle;
FIG. 4 is a block diagram and plane view illustration of an exemplary spherical treadmill including control electronics;
FIG. 5A is an illustration of an exemplary scene on the Moon;
FIG. 5B is an illustration of the same exemplary scene on the Moon in bar chart form;
FIG. 6A is an illustration of an exemplary array of extendable piston rods;
FIG. 6B is a detailed illustration of four exemplary extendable piston rods including control electronics; and
FIG. 6C is a magnified view of a section of an exemplary extendable piston mechanism.
DETAILED DESCRIPTION OF THE INVENTION
The description set forth below in connection with the appended drawings is intended as a description of various configurations and is not intended to represent the only configurations in which the concepts and features described herein may be practiced. The following description includes specific details for the purpose of providing a thorough understanding of various concepts. However, it will be apparent to those skilled in the art that these concepts may be practiced without these specific details. In some instances, well known circuits, structures, techniques and components are shown in block diagram form to avoid obscuring the described concepts and features.
FIGS. 1A-1H and 2A-2M depict methods and apparatus for achieving a novel “circular” or omnidirectional treadmill incorporating three two-way conveyor mechanisms. Specifically, FIG. 1A illustrates the active area of the entire apparatus, with a handler 40 standing in the middle of a circle 41 that defines the simulator stage.
Vertical lines 42 - 43 are over the width of that active area along horizontal line 44 - 45 generating FIG. 1B , a cross-section diagram of one of three transport mechanisms used to maintain handler 46 at or near the center of the simulator stage. A representative line of ball bearings 48 capped with tile sections 47 contact the top of stage table surface 55 . At each end of the tile transport mechanism is a roller 49 , which may also take the form of a paddle-wheel or gear with offset sections to conform to individual tile-bearing elements (see FIG. 1E below).
A guide structure 50 wraps around the transport mechanism and bottom portion of the conveyor. As individual bearing-tile elements leave the stage they are flipped over and slide tile-down through the guide structure, with their bearings rolling on the top. To facilitate this upside-down transit, the inner bottom surface of the guide structure should have a hard, slippery surface like a coating of Teflon® or similar material.
FIG. 1C is a magnified view of portion 51 in FIG. 1B , with tile elements 52 are visible atop cylinder 52 a and on the bottom of cylinders 52 b . Tiles 52 a and 52 b slide against ball bearings 2 , 3 between them and the entire guide structure 1 not active as the treadmill surface. In FIG. 1B this guide structure is labelled 50 . Each cylinder in turn houses one or more ball bearings facing away from the tile surface, per FIGS. 1F and 1G below. Also shown in FIG. 1C is stage support table 55 a , roller or gear mechanism 53 , and the bottom portion of the stage table 56 , and an exemplary position 4 where the conveyor might be halted in perfect alignment with the other conveyors. This will be discussed more fully in FIG. 2M and FIG. 2N below.
FIG. 1E shows an elongated gear 54 alternative to roller transport mechanism 53 . The width of the “paddle wheel” gear is proportional to the width of the conveyor (see 59 , 59 c in FIG. 1D ), and each paddle can be angled or broken into individual sections to better accommodate individual cylinder elements.
FIG. 1F is a further magnified view of one ball bearing cylinder 63 , including triangular tile surface 57 , cylindrical bearing cup 65 , and large ball bearing element 64 .
A presently preferred bearing housing is depicted in FIG. 1G , including a lower profile cylinder 68 that supports three ball bearings 67 rather than the single, larger bearing depicted elsewhere for simplicity. The advantage of the three-bearing housing is that each such element is stand-alone, so that any weight exerted on triangular tile 66 will be equally distributed on the three bearings and maintain the entire element stable and level at all times.
FIG. 1D illustrates the environment simulator concept, including a circular stage area 62 covered by a plurality of tiles 60 , individually shaped as equilateral triangles 57 which mesh together to form the floor of the simulator stage. The simulator includes three conveyor mechanisms, all powered by pressure rollers 58 or paddle wheel gears like the one 54 shown in FIG. 1E .
One conveyor is powered by transport mechanisms 59 , 59 c in the 3 o'clock-9 o'clock position on the circle. This conveyor compensates for any handler movement along a 90 degree-270 degree line, moving in either direction to continually keep the handler centered on this axis.
Another conveyor has transport mechanisms 59 a and 59 d at the 150 and 330 degree positions on the circle, and similarly acts to continually compensate for any handler movement along this axis. The third conveyor's transport mechanisms 59 e and 59 b are at the 30 and 210 degree positions on the circle, similarly moving the handler's floor in one direction or the other to compensate for movements off center.
Beneath the entire tile surface 60 depicted is a second tile surface 61 , directly corresponding to the surface above but inverted (upside down) from the top surface. This lower surface constitutes the bottom side of each of the three conveyors depicted, with each forming a continuous loop of tile/cup/bearing elements as shown in FIGS. 1B and 1C .
FIG. 1H shows a modified form of the conveyor mechanism depicted in FIG. 1C , wherein the housing ball bearings 2 a extend only around the portion of the housing 1 a that extends beyond the active treadmill stage area ( 62 in FIG. 1D ). In the configuration of FIG. 1H , the bearing area is replaced by a smooth sliding surface 5 extending under the entire stage area to result in smoother conveyor motion.
FIG. 2A is a more detailed look at the omnidirectional treadmill simulator of FIG. 1 , showing a mesh of individual equilateral triangular tiles 70 completely filling the active stage area. Point 83 marks the center of the stage, and defines the general area where the proxy robot human handler is to be maintained by compensating movement of one or more of the three treadmill conveyors.
Assuming the top of the page to be north for this discussion, one conveyor mechanism 71 , 74 spans between rollers or paddle wheel gears 77 - 78 and compensates for handler movements in either a northeast or southwest direction (30 degree-210 degree axis). A second conveyor mechanism 72 , 75 is located between rollers or gears 79 and 80 , and compensates for handler movements to either the east or west (90 degree-270 degree axis). The third conveyor mechanism 73 , 76 is located between transport rollers or gears 81 , 82 , and compensates for handler movements to the northwest or southeast (150 degree-330 degree axis). A line 35 , 35 a perfectly bisects conveyor 72 , 75 , passing through the center point 83 on the stage. A second line 36 , 36 a similarly bisects conveyor 73 , 76 , while a third line 37 , 37 a bisects remaining conveyor 71 , 74 .
FIGS. 2A and 2B illustrate the operation of the circular treadmill. If the handler steps from stage center 83 directly to the east (right on the figures), the conveyor that will become active is the one highlighted in FIG. 2B , running between 90 degrees and 270 degrees, i.e., between motorized rollers 79 and 80 in FIG. 2A . Since the handler moved a step to the east, this conveyor will move toward the west in approximately the same amount, but come to rest in a position where all the tiles align once again. This is absolutely necessary to the operation of the circular treadmill, since all tiles must be in alignment so that conveyors in the other directions can similarly activate (see FIG. 2E below).
If the handler moves to the northwest 76 or southeast 73 on FIG. 2A , this will activate the conveyor highlighted in FIG. 2C . Conveyor motors on that axis will compensate for the handler's steps, maintaining handler position near center 83 at all times.
What happens when the handler travels in a north (or south) direction, a position between conveyors 71 , 74 and 76 , 73 ? In this case, the processor 95 will assign priority to one conveyor; for example first moving the handler along axis 71 , 74 to center the handler on line 37 , 37 a ; and next along axis 76 , 73 to center that conveyor on line 36 , 36 a . The reasons for this two-step process are 1) that only one conveyor can move at a time; and 2) any handler movement off center can be corrected by the compensating movement of two conveyors. When each of the two effected conveyors have moved that handler to their particular center line, the handler will once again be located in the center of the stage.
If the handler moved to the west rather than the east, the same conveyor 79 , 80 would activate, but the motors would turn their rollers in the opposite direction, causing that conveyor to travel to the east. Likewise, the handler might move to the northeast or southwest, causing conveyor 71 , 74 to activate and reposition the handler to center point 83 . This conveyor is depicted in FIG. 2D .
FIG. 2E shows how the circular treadmill of FIGS. 2A-2L functions electronically. Motion capture cameras or other monitor means 90 turn essential movement on the treadmill into “follow me” commands for the proxy robot, and may also be utilized in keeping the handler centered on the circular simulator stage. Specifically, handler step motion data 91 can be broken into handler heading (yaw or bearing) information 92 , handler step distance 93 , and step moment or velocity 94 .
This data is fed into processor 95 , which produces signals that ultimately control the current driving conveyor 1 motor pairs 77 , 78 ; conveyor 2 motor pairs 79 , 80 ; and conveyor 3 motor pairs 81 and 82 ; from conveyor 1 motor control circuit 96 ; conveyor 2 motor control circuit 97 ; and conveyor 3 motor control circuit 98 , respectively.
Processor 95 also receives data from park sensor means 99 , which monitors each conveyor's movement and continuously feeds alignment data to the processor 95 , enabling that processor to signal each conveyor to park (stop) at a point where all tiles line up.
FIGS. 2F, 2H and 2K further illustrate conveyor park operation, utilizing the northwest-southeast conveyor of FIG. 2C as an example in each case. In FIG. 2F , the referenced conveyor 320 a is moving in a southeast direction (arrow) to compensate for a handler step.
The insert of FIG. 2G depicts a magnified view 321 b of the junction between tiles at location 321 a , a point where all three conveyors converge. Pattern 322 is the required park position of the various tile edges: note that the actual conveyor tile position at point 321 b is considerably off-alignment from the necessary pattern 322 .
In FIG. 2H , conveyor 320 b continues to move to the southeast (arrow), and relative tile positioning at the same point 323 a is considerably closer to alignment now, per magnified view 323 b in insert FIG. 2J . But the tiles are not yet aligned as they must be in pattern 322 , so conveyor movement continues.
In FIG. 2K , conveyor 320 c has reached the point of alignment, as depicted at point 324 a and the magnified view 324 b of FIG. 2L . At this point, park sensor 99 notifies processor 95 of correct alignment, and processor 95 commands conveyor 320 c to stop via treadmill 3 motor control circuit 98 .
FIG. 2M illustrates how the park sensor 99 in FIG. 2E can achieve the objective of parking one of the conveyors in perfect alignment with the other two via a number of means. In FIG. 2M , tiles 326 top the simulator stage, comprising conveyors that keep a handler relatively centered at all times. One way to stop a conveyor in correct alignment is to cause “paddle-wheel” gear 327 in FIG. 2M to stop with a tile in some precise position, as, for example, when a paddle of wheel 327 is between two tiles at exact right angles to the horizontal stage 328 supporting the handler.
Such alignment may also be achieved through pattern recognition, as by watching tiles on the moving conveyor for a dot, circle or “x” etched or painted at the center of each tile and stopping the belt when the mark is observed. A stop of this sort may be accomplished by halting paddle wheels 327 or drive roller 49 ( FIG. 1B ) in proper position, and/or through the employment of a braking mechanism like pads against the correct tile as it passes by roller 49 .
In another configuration, a mask or reference pattern such as 322 in FIG. 2G is compared with an area 321 b between tiles. When the monitored pattern coincides with the reference, as in FIG. 2L ( 324 b , 322 ), the park sensor 99 sends a “stop” signal to processor 95 which in turn commands the appropriate treadmill motor control circuit to stop its motors.
A presently preferred mechanical stop apparatus embodiment employs a a semi-flexible blade 325 which can be commanded to protrude from a cylinder 331 . The cylinder 331 may represent electro-mechanical solenoid or other means, with the protruding blade scraping against a passing line of tiles 326 which are upside-down on the lower portion of conveyor 328 (c.f. position 4 in FIGS. 1C and 4 a in FIG. 1H ).
In this case, a small port in the underside 330 of the conveyor housing can be positioned to coincide with a specific position where tiles from all conveyors intersect. This would be like the position shown in FIGS. 2G, 2J and 2L , but 180-degrees removed to the bottom of the unit such as to cause no interference with the active (topside) portion of the simulator stage. Into this small port, the blade 325 of FIG. 2M could be made to protrude through some combination of electromagnetic, spring or hydraulic means in cylinder 331 , with flexible blade element 325 flapping against moving tiles as they pass upside-down along the bottom 329 of the conveyor loop, until the blade fits snugly between two tile sets, causing the moving conveyor to stop in precisely the proper position.
FIG. 2N shows the circled area 332 in FIG. 2M in amplified detail, including an electro-mechanical portion represented by cylinder 331 a ; a line of tiles 334 passing in directions 335 ; and a blade element 325 a moving up and down line 333 upon command from park sensor 99 in FIG. 2E .
To achieve such a stop, semi-flexible blade 325 a might be made of spring steel or a strong plastic compound, or the blade might protrude only sufficiently to stop a powered-down conveyor's final momentum. In this latter case, a conveyor would cease being powered as the handler's position approaches stage center. Thereafter, when the handler moves in some direction creating a need for a conveyor to compensate, blade 325 a would retract until the handler has been re-centered on the treadmill stage.
FIG. 2P illustrates another omnidirectional treadmill arrangement utilizing square tiles 340 and two conveyor mechanisms. One conveyor moves between the 6 o'clock and 12 o'clock positions by means of motor-driven rollers or paddle-wheel gears 342 a and 342 b , while the other conveyor moves between 3 o'clock and 9 o'clock positions via rollers or paddle-wheel gears 341 a and 341 b . Although simpler to manufacture and operate, the square-tile, two conveyor configuration of FIG. 2P is not currently preferred due to the jerky movements necessary to keep a handler centered on the treadmill stage. Otherwise, this treadmill would generally incorporate elements discussed heretofore in FIGS. 1 and 2 with one exception:
FIG. 2Q depicts that exception: treadmill motor control means for two rather than three conveyors. In this diagram, motion capture cameras or other monitor means 343 turn essential movement on the treadmill into “follow me” commands for the proxy robot, and may also be utilized in keeping the handler centered on the circular simulator stage. Specifically, handler step motion data 344 can be broken into handler heading (yaw or bearing) information 345 , handler step distance 346 , and step moment or velocity 347 .
This data is fed into processor 348 , which produces signals that ultimately control the current driving conveyor 1 motor pairs 341 a and 341 b , and conveyor 2 motor pairs 342 a and 342 b : from conveyor 1 motor control circuit 349 and conveyor 2 motor control circuit 350 , respectively.
Processor 348 also receives data from park sensor means 351 , which monitors each conveyor's movement and continuously feeds alignment data to the processor 348 , enabling that processor to signal each conveyor to park (stop) at a point where all tiles line up.
FIG. 3 illustrates one exemplary method and apparatus for the addition of pitch and roll to a circular treadmill simulator for human proxy robot handlers, wherein legs 120 under an ommnidirectional treadmill 108 like the one shown in 1 B above are firmly mounted to the floor of a modified or custom made motion simulator 101 . Motion simulators are typically costly devices, with pitch, roll and various vibratory sensations (like earthquakes, rocket engines or runaway trains) are created by varying the length of four or more large hydraulically extending arms 102 - 105 resting on large floor pads 106 , 107 , and a large wrap-around video screen 112 creates the appropriate visual environment.
As a consequence, the goggles 113 worn by the handler in this drawing are likely for 3-D viewing, while a two-way headset 114 may still be employed for mission and team communication as well as voice commands like “Freeze, Freeze.” Although the same ends could be accomplished via a microphone and speakers not directly connected to the person of the handler, the headset 114 serves the additional purpose of isolating the handler from ambient noise including operational sounds of the motion simulator.
As she walks or otherwise moves on the circular treadmill 108 , the handler is held in place by a gravity harness 109 with bungee cords or springs 110 which hang from hooks 111 in the top of the motion simulator capsule 101 and provide lift to her suited body sufficient to equal the weight of the proxy robot on Mars or some other location in space.
Let us turn now to meeting the challenges of long path delay, as in the case of Earth-Mars. As we have explored in the description of previous figures, the approximated real time (ART) video generating terrain analysis computer 153 receives streaming video and other data from multiple sources 151 at the remote location (e.g., Mars), and combines this information with data 152 already stored and fully accessible to the terrain analysis computer.
While the most major function of the terrain analysis computer is the generation of accurate ART video 157 for the proxy robot handler as well as an ongoing stream of “terrain just ahead” data 156 to warn and otherwise guide that handler's every move, the terrain analysis computer can also supply data to a processor 155 that controls the environment simulators in which handlers perform their functions.
In the case of motion simulator capsule 101 , processor 155 can feed signals to hydraulic leg pumps 121 - 124 , where each hydraulic pump controls the height of an extendable-contractible leg. So, for example, pump 121 controls the amount of extension in leg 104 , while pump 122 controls the same function in leg 105 . In practice, any normally-encountered amount of pitch (tilt forward or backward) roll (tilt from one side to the other) or combination thereof can be replicated via signals originating in incoming data from a remote location such as Mars together with stored mapping data that becomes an augmented virtual reality view of the time in the future when “follow me” data from the handler will reach the proxy robot. Put another way, the terrain analysis computer is not only providing a handler with video that is 10 minutes or more in the future, but also replicating the terrain conditions that handler will be encountering at that moment in time.
FIG. 3A depicts an exemplary embodiment of an omnidirectional treadmill 125 , under which are four legs 128 - 131 extendable via hydraulic, pneumatic or other means from a relatively flat profile 132 to many times that height 128 . When all legs are in their compacted state, the plane of treadmill 125 is flat, without tilt in any direction, but this state can be altered by signals originating at the terrain analysis computer 153 and passing through processor 155 and the four hydraulic leg pumps 121 - 124 .
Let us first consider pitch. If we want to tilt the treadmill up from front to back 145 , front legs 129 and 130 should be in their compressed state, while back legs 128 and 131 will be totally or partially extended to achieve the desired rise to the rear of the treadmill. Front-up, rear-down pitch 146 is achieved by doing the opposite: extend front legs 129 and 130 and compress back legs 128 and 131 .
In the case of roll, we can tilt (roll) the treadmill downward toward the right side 149 by compressing legs 130 and 131 while extending legs 128 and 129 , or conversely tilt downward toward the left side 150 by compressing legs 128 and 129 while extending legs 130 and 131 .
The accurate simulation of some remote terrain might involve a degree of both pitch and roll: for example, as the proxy robot climbs an irregular incline. Simulating this condition might involve fully compressing left rear leg 128 , fully extending right front leg 130 , and partially extending legs 129 and 131 —all in accordance with terrain data received from video and sensors on the proxy robot.
FIG. 3B illustrates an exemplary method and apparatus for a remote vehicle simulator in a capsule 300 , wherein pitch, roll and various vibratory sensations may be created by varying the length of four or more large hydraulically extending legs 268 - 271 resting on large floor pads 273 , with the extension of each leg controlled by a hydraulic valve 272 connected to a pump and motor 287 - 290 .
The employment and utilization of proxy robots for missions on remote locations like space environments permits the use of vehicles of the sort that can be operated and driven by humans as opposed to robotic vehicles in a space location that are programmed and/or remotely operated from earth or some other control point. In the proxy robotic case, it is the proxy robot 295 that actually drives and operates the remote vehicle 296 , in concert with a human handler 260 who “drives and operates” a simulation 261 of the proxy's vehicle from the safety of the simulator in capsule 300 .
Controls like steering, brake and throttle 302 in the remote vehicle 296 are precisely replicated 262 in simulated vehicle module 261 . The human handler 260 can either control the remote vehicle 296 by viewing a large wrap-around video screen 263 or via goggles 264 in a head-mounted display. Either or both create the exact visual environment perspective of the remote proxy robot 295 at an upcoming future point in time when the operational data reaches the remote vehicle 296 .
Terrain analysis computer 282 receives video, positional data and other information from aggregator 281 which aggregates streaming video 299 from the camera “eyes” 298 of proxy robot 295 , look-ahead video from mast camera 297 and other video and data from multiple sources 301 at the remote location (e.g., the moon or Mars). This information from the remote location is combined with data 283 already stored in and fully accessible to the analysis computer 282 .
A primary function of terrain analysis computer 282 is the generation of accurate approximated real time (ART) video 294 for the proxy robot handler as well as to a “terrain just ahead” processor 285 that generates an ongoing stream of data 291 to warn and otherwise guide that handler's every move.
The terrain analysis computer 282 also supplies data to a processor 286 that controls the pitch, roll and replicates other conditions like a rough or bumpy environment being experienced by the remote vehicle 296 and its proxy robot driver 295 .
In the case of vehicle motion simulator capsule 300 , processor 286 feeds signals to hydraulic leg valves 272 a - d , where each hydraulic valve controls the height of an extendable-contractible leg. For example, pump 287 and valve 272 d control the amount of extension in leg 269 , while pump 288 and valve 272 c control the same function in leg 270 .
In practice, any normally-encountered amount of pitch (tilt forward or backward) roll (tilt from one side to the other), rough or bumpy ride, or combination thereof can be replicated via signals originating in incoming data from a remote location such as Mars together with stored mapping data that becomes an augmented virtual reality view of the time in the future when “follow me” data from the handler will reach the proxy robot vehicle operator. Thus, terrain analysis computer 282 is not only providing a handler on Earth with video that is 10 minutes or more in the future in the case of Mars, but also is replicating the terrain conditions that the proxy robot's remote vehicle will be encountering at that very moment in time.
“Follow me” commands from human handler “driver” to proxy robot driver are a composite of data from several sources. Positional information from the handler, including head angles, hand and foot positions and so forth, are collected by a plurality of motion capture cameras 266 - 267 and aggregated in handler data circuit 279 . Control and reading data 274 from the vehicle simulator, including steering position and vehicle heading information 275 ; throttle position and vehicle velocity 276 ; gear and braking data 277 are fed into vehicle data module 278 , along with other information such as blade or backhoe position, depending on the vehicle and the mission requirements.
Handler data 279 and vehicle data 278 are weighed and combined in a “follow me” data processor 280 which uses both sources to send the most precise position commands possible over path uplink 304 to the remotely-located proxy robot operator 295 of vehicle 296 on the surface of the moon, Mars, or some other location remote from mission control. It should be pointed out that the definition of a remote location does not exclude locales on the Earth, like disaster sites, under sea projects, natural event locations like volcanoes, tsunami and tornados as well as survey vehicles, mining, and even the movement of goods and services from one place to another.
In like manner, data and readings from vehicle data 292 and terrain just ahead 293 modules are routed to mission control, including panel 265 or a portion of either wrap-around video screen 263 or handler head-mounted display 264 to maintain the handler informed to the greatest possible extent.
FIG. 4 illustrates an example of a spherical treadmill with variable pitch, roll and infinitely variable heading. In this novel approach, the treadmill takes the form of a large sphere 190 , with a diameter many times average human height; e.g., at least three times but preferably five or more times human height. The diameter of sphere 190 in this figure is approximately 30 feet, but the simulator staging area typically occupies only the top 25% to 35%, as depicted by floor line 170 . The sphere protrudes from a circular opening in upper floor 170 , and a small area 194 where floor meets sphere is magnified 195 to depict Teflon® or a flexible, renewable material such as bristles, rubber or plastic between the two surfaces. In addition to keeping debris from falling through the floor, this junction 195 serves to stabilize the sphere and smooth its motion.
The sphere 190 can be made of a lightweight but strong material such as plastic, aluminum or composite coated with rubber or a similar no-slip substance. It rests upon three or more large bearings 164 , with each bearing seated in a socket 164 a which is mounted firmly in place to the support floor under sphere 190 . Bearings 164 and their lubricated sockets 164 a assure movement of the sphere with minimum friction, allowing pressure wheel motors 161 and 163 to be relatively small and economical.
In the upper (simulator stage) portion of the sphere 190 , a human handler 165 is taking a step to direct her proxy robot's course. As this takes place, data indicating handler heading 171 , step distance 172 and step moment (time duration and velocity) 173 is sent to handler step motion circuitry 166 which sends appropriate data representing each parameter to both the proxy robot as part of a “follow me” data string 169 and to a processor 167 that feeds either digital or analog data to motor control circuitry 168 a , 168 b as well as to boom control 189 .
If the proxy robot is walking on flat terrain, the human handler will occupy position 165 a at the very top, center of sphere 190 . Although that handler will be atop a very slight rise equal to the rise atop that section of the sphere, the simulation from a sphere five times the human's height will be of a relatively flat surface.
But if the robot is walking up a rise akin the slope in FIG. 3C , this positive (nose up) pitch of around 10 degrees can be simulated by situating the handler in position 165 b on the sphere. A more severe forward pitch of approximately 20 degrees is shown as position 165 c on the sphere, while at position 165 d near floor level, rise in pitch approaches 45 degrees. Positive (upward) pitch is represented by arrow 174 in the drawing, while downward or negative pitch is represented by arrow 175 .
Downward pitches on the same heading at −10, −20 and −45 degrees can be simulated from positions to the left of the sphere, at 165 e , 165 f and 165 g , respectively. If the handler's position moves left in the direction of arrow 176 , there will be leftward roll (left tilt) in that position. For example, position 165 h would exhibit severe roll, tilting some 25 degrees to the left. Moving the operating stage in the opposite direction (hidden from view) will result in roll to the right (right tilt). From the foregoing, it can be seen that any conceivable combination of pitch and roll can be found at various locations on the surface of the spherical treadmill 190 .
Since the pitch and roll conditions in the simulator beneath the human controller are determined by feedback 181 from the proxy robot's remote location, suitable means must be present to change the location of the handler staging area to one matching the average pitch and roll of the remote terrain. Positional and other data is received from sources on the “person” of the proxy robot, including both near- and far-field 3-D video from its various camera “eyes” and possibly even a long-range 360-degree view from a camera system on top of the robot's head (c.f. FIG. 2 ) Video and other data come as well from sources external to the proxy robot: orbiting satellites, balloons, pole cameras, buoy cameras and other robots.
The video feed from the remote location is routed to display devices for the analysis of mission personnel, but it does little good for the handler, since it is delayed on the order of 3-22 minutes from Mars. All video and data 161 from the remote locale moves over this communication path before being routed to a Terrain Analysis Computer 185 which generates a highly-precise augmented virtual reality view of the terrain and setting of the proxy robot at 10 minutes into the future when signals from the handler actually arrive at the mission site on Mars. Computer 185 also uses the stored and incoming information to generate data 186 about terrain just ahead 184 for the information and use of the handler.
The “terrain just ahead” data 186 , heading 171 , step distance 172 , and step moment 173 data are bundled and fed to a processor 167 which turns all the input data streams into meaningful signals to drive motor control circuitry 168 a , 168 b and boom control 189 .
Motor control circuits 168 a and 168 b convert the data from processor 167 into positive or negative direct current to drive motors 161 and 163 and their respective pressure rollers 161 a and 163 a in either direction when so instructed by processor 167 , causing the sphere to turn under the handler's feet to compensate for steps the handler takes forward, backward or in any direction whatever. But since it is also acting from signals representing such upcoming terrain conditions as pitch 174 - 175 and roll 176 , it is the function of the roller motors to effectively move the sphere under the handler as each step is taken to place that person in average pitch and roll conditions matching the remote terrain to the greatest extent possible.
Motor mounts 162 are illustrated to show a possible position for a pressure solenoid that can activate whenever a roller motor is called into service, pushing, for example motor 161 and its attendant roller 161 a harder into the sphere to gain traction. The advantage of using solenoids in this manner is that the non-active roller(s)—from motor 163 and its roller 163 a in the example—provides less drag for the active motor and roller to overcome. Of course there may be instances when both roller motors (or two or more motors from a multiplicity of roller motors spaced at even intervals around the sphere) may be called into action simultaneously. But in this case there will be less drag to overcome as motion overcomes inertia, even with all solenoids pushing the motors' rollers into the sphere. Although roller motors 161 and 163 are depicted as mounted against the upper floor 170 , they can also be mounted at the sphere's equator or in any other convenient position.
In the simulator, the human handler would be strapped into a gravity harness suspended from a platform 178 , 179 by a number of bungee cords or cables with springs 177 . A rotation collar 179 a allows the platform to rotate freely in any direction. As the handler is effectively moved about on the staging surface of the upper sphere, it is important that the gravity harness follow those movements to maintain the handler's correct effective weight, by lifting from a position directly above the handler and harness. In the drawing, three handler positions are depicted: 165 a which is relatively flat, 165 b with a positive pitch 10 degrees, and 165 c with a forward incline of some 20 degrees.
Roller motors 161 and 163 can place the handler in any of the above positions or virtually anywhere else on the simulator stage, but an additional mechanism is needed to move the gravity harness as the handler is moved. This mechanism is an extendable boom or robotic arm 192 shown at the top of the drawing, which provides overhead lift as well as positional correctness directly over whatever handler's position. The boom or robotic arm depicted is for illustrative purposes only, as it can be appreciated that other combinations of tracks, motors and cables can place the handler at the required positions.
At the tip of the boom is a winch 191 . The motorized winch maintains constant torque (upward pull) on the handler at some predetermined level. For example, if the handler is to match the 76 lb. weight on Mars of a 200 lb. robot, that handler's weight should be effectively 76 lbs. So a 160 lb. human handler would require a constant upward pull of 84 lbs., and a downward pull by gravity of 76 lbs. It is the job of winch 191 to maintain this effective weight. The winch pays out as much cable 180 as necessary to constantly maintain the desired upward pull on the handler, and it receives data from processor 167 via boom motor control circuit 189 . The cable positions 180 , 180 a and 180 b are maintained directly over handler positions 165 a , 165 b and 165 c , respectively, by lateral movement of the boom, which can extend/retract; swing right or left, and tilt up or down in accordance with data instructions from processor 167 and boom motor control 189 .
Maintaining constant torque solves one problem; namely, that the length of cable 180 must change the further the handler is moved from the “flat” position 165 a at top center. So when processor 167 and roller motors 161 , 163 act to place the handler in position 165 c , for example, the length of cable 180 would leave the handler dangling in mid-air. But not really, since such dangling weight would equal 160 lbs downward. Immediately, the constant torque mechanism would tell the winch to let out more cable until the handler once again exerts 76 lbs downward and 84 lbs upward.
Boom 192 does more than extend and retract to replicate various up and down levels of pitch, however. In response to instructions from processor 167 , which in turn receives “terrain just ahead” data 184 and other position and mapping information from the terrain analysis computer 185 , boom 192 can also move from side to side to replicate roll—the sideways tilt of the place where the proxy robot will be walking some ten minutes in the future. Together, these boom movements account for both pitch and roll: two of the three movements possible in three-dimensional space.
The third element is yaw—in this case the direction the handler is facing or moving on a 360-degree plane. This element is determined by the handler, and is translated into heading signals 171 , which, together with step distance 172 and step moment 173 data, are packaged and translated by Handler Step Motion Data electronics 166 into “follow me” proxy robot language 169 to guide the proxy's every move. The “follow me” data that travels over an uplink path to Mars or whatever remote mission location, arriving at the exact moment anticipated by Terrain Analysis Computer 185 .
FIG. 5A illustrates a scene on the moon, rendered pictorially, while FIG. 5B depicts the same scene in 3D bar chart form. In the photographic version of the scene 200 (top), we see two hills with summits 201 and 205 , with a saddle 203 between them. In front of these two hills is a smaller hill with summit 204 , and two low or valley areas 202 and 206 .
This same terrain can be computer-rendered into a three-dimensional bar chart like 210 in FIG. 5B , where individual bars 209 in a matrix represent the elevation at each charted point. For example, the summit of the first hill 201 in FIG. 5A is represented by point 211 in FIG. 5B ; higher hill summit 205 is represented by bar 215 ; saddle 203 by bar 213 ; front hill summit 204 by bar 214 ; valley 202 by bar 212 ; and valley 206 by bar 216 .
Programs already exist to make such 3D bar chart renderings, but the purpose of the figure and description to follow is to bring the bar chart into material reality through the creation of physical hills and valleys as part of a highly immersive environment simulator.
FIG. 6A depicts a matrix similar to that of the 3D bar chart in FIG. 5B above, but with physical piston rods replacing each bar in the drawing. In FIG. 6A , a matrix array 220 of piston rods 221 are enclosed in individual cylinder housings 223 of some uniform height 222 . Each individual piston rod can be controlled hydraulically to extend above its cylinder by an amount either equal to the height of the cylinder 224 or even greater if the rod portion uses telescoping means such as 224 a and 224 b.
The plane area 225 defines the floor of an environment simulator, with tiles atop the embedded rod elements 221 forming a three-dimensional surface. Immediately beneath cylinder matrix 220 in area 227 is an array of hydraulic valves that connect to each individual cylinder. Beneath this is another area 228 reserved for one or more hydraulic motors, pumps and the electronic equipment that connects to a valve under each cylinder.
FIG. 6B shows four adjacent cylinder-rod assemblies in greater detail, where the simulator floor 230 corresponds to plane 225 in FIG. 6A , and rods 231 , 233 , 235 and 237 are depicted in various stages of extension above that floor. While widely-varying positions are shown for rod ends 239 , in actual practice adjacent rods would be only slightly removed one from the other, creating a smooth incline or decline in the overall 3D environment. Rods 231 , 233 , 235 and 237 in FIG. 6 are basically pistons that move up and down from their positions in cylinders 232 , 234 , 236 and 238 , respectively.
The non-shaded portion in each of these cylinders represents space filled with the hydraulic fluid that displaces each piston. For example, piston 237 is shown fully extended, so its cylinder is completely full of hydraulic fluid, while cylinder 323 is extended about 65%. It should be noted that FIG. 7B utilizes non-telescoping cylinder elements, a presently preferred configuration.
A complete three-dimension environment can be created when the terrain analysis computer 240 described in previous figures is harnessed to provide a terrain-generating data stream 241 in addition to approximated real time (ART) video and other outputs. The terrain-generating data is fed to hydraulic array driver electronics 241 which produce elevation signals 243 for each individual hydraulic cylinder-piston element in the electronically-operated hydraulic valve array 246 . The number of these cylinder-piston elements may be large indeed. For example, a 40 ft×40 ft simulator room with 2 inch×2 inch tiles would require 40×6=240 tiles per side, or 57,600 tiles total, translating to 57,600 individual cylinders and pistons, 57,600 hydraulic valves, and 57,600 circuit connections from hydraulic array driver electronics 242 .
FIG. 6B shows four such valves 247 - 250 . Each of these receives signals from hydraulic driver array electronics 242 that cause each valve to open and permit a designated pressure and volume of fluid from hydraulic pump and fluid tank 244 to enter the cylinder and push the piston rod to the elevation called out by terrain analysis computer 240 .
In FIG. 6C , a single section of cylinder 252 , piston rod 253 , hydraulic fluid intake 254 , electrically-controlled hydraulic valve 255 , electronic signal 256 , and hydraulic fluid pipe 257 connect together to fill chamber 258 to the level that generates the required elevation for that particular cylinder-piston rod element.
In sum, the circuitry and apparatus described in FIG. 6 can rapidly generate a physical replica of a mission area on the moon, Mars, or other locations in space or on earth with the physical integrity to support the weight of human handlers, robotic “follow me” vehicles and the like, to ensure the accuracy and maximize the productivity of a proxy robotic mission to that area. When it is time for the proxy robots or robotic vehicles to move on, a new physical landscape can rapidly be generated and put to good use by human handlers on the earth and their robotic counterparts at some remote location.
The various features associate with the examples described herein and shown in the accompanying drawings can be implemented in different examples and implementations without departing from the scope of the present disclosure. Therefore, although certain specific constructions and arrangements have been described and shown in the accompanying drawings, such embodiments are merely illustrative and not restrictive of the scope of the disclosure, since various other additions and modifications to, and deletions from, the described embodiments will be apparent to one of ordinary skill in the art. Thus, the scope of the disclosure is only determined by the literal language, and legal equivalents, of the claims which follow. | An omnidirectional treadmill environment simulator is disclosed. The omnidirectional treadmill environment simulator includes a circular simulator stage area, a plurality of transport mechanisms that maintain an object at or near the center of a circular simulator stage area and at least one processor. The processor is configured to collect position data of the object and process the position data to control the transport mechanisms. Also included is a receiver for receiving data from a remote location and a terrain analysis computer for processing the data received from the remote location. The terrain analysis computer collects the data received from the remote location to form an accurate simulation of an upcoming condition at the remote location. The omnidirectional treadmill environment simulator includes a transmitter for transmitting the position data to a remote location. | 1 |
BACKGROUND OF THE INVENTION
[0001] The present invention relates to a watertight seal made between the interface of a sink and the laminate counter which it is mounted underneath. It provides both an aesthetically pleasing alternative to conventional undermounted sinks and also provides a much user friendly and dimensionally precise method of on-site installation.
[0002] The countertop industry has seen a shift from the standard laminate countertops with top mount stainless steel (or other material) sinks to solid surface countertops with undermount stainless steel, porcelain or polymer sinks. Under counter mount sinks are more desirable than top mount sinks because there is no lip on top of the counter to catch debris and stain. Further they prevent the continuous wiping of the counter into the sink. Man made and natural solid surface countertops lend themselves better to under counter mount sinks than do laminate countertops because of their solid construction. When water contacts the sides of a laminate countertop the glued wood particle makeup absorbs water, swells and eventually deteriorates and crumbles away. The point of failure (where this water substrate contact occurs) in the prior art generally occurs at interface at the bottom edge of the laminate and the sink seal. In top mounted sinks the water can seep under the sink top flange and the laminate and run down between the sink and the particle board substrate. Thus solid surface countertops have dominated the market where under counter mounted sinks are desired.
[0003] The solution for the laminate countertop is to have a seal that prevents the deterioration of the laminate substrate by preventing water from ever contacting it. Of course it must also be aesthetically pleasing.
[0004] Henceforth, a visually appealing sealing interface between an undermount sink and a laminate countertop would fulfill a long felt need in the building industry. This new invention utilizes and combines known and new technologies in a unique and novel configuration to overcome the aforementioned problems and accomplish this.
SUMMARY OF THE INVENTION
[0005] The general purpose of the present invention, which will be described subsequently in greater detail, is to provide a sealing interface between an under counter mount sink and a laminate counter as well as a simplified and more dimensionally accurate method of field installing the sink below the counter. The key concept of accomplishing a water impervious seal between an under counter mount sink and a laminate countertop is to provide a seal that is tightly, directly, chemically bonded to the cutout lip of the laminate and the sink cutout edge in the particle board substrate as well as to the entire area on the bottom face of the laminate countertop's particle board substrate that contacts the top face of the under counter mount sink. In this way there is never the possibility of water contacting an unprotected area of the countertop substrate. Critical to accomplishing this are two other key concepts: aligning the sink onto the seal correctly and ensuring that the seal face that contacts the top flange of the sink is deck aligned or completely parallel to the sink top flange.
[0006] The undermount sink seal of the present invention has many of the advantages mentioned heretofore and many novel features that result in a new system for mounting an under counter mount sink to a laminate countertop which is not anticipated, rendered obvious, suggested, or even implied by any of the prior art, either alone or in any combination thereof.
[0007] The subject matter of the present invention is particularly pointed out and distinctly claimed in the concluding portion of this specification. However, both the organization and method of operation, together with further advantages and objects thereof, may best be understood by reference to the following description taken in connection with accompanying drawings wherein like reference characters refer to like elements. Other objects, features and aspects of the present invention are discussed in greater detail below.
BRIEF DESCRIPTION OF THE DRAWINGS
[0008] FIG. 1 is a front perspective view of the under counter mount sink sealing system showing an under counter mounted sink mated to a countertop with the sealing interface;
[0009] FIG. 2 is a bottom perspective view of the under counter mount sink sealing system showing the clamping assembly;
[0010] FIG. 3 is a top perspective view of the inner routing ring;
[0011] FIG. 4 is a top perspective view of the surface routing jig;
[0012] FIG. 5 is a top perspective view of the hole routing jig;
[0013] FIG. 6 is a top perspective view of the locator/dam ring;
[0014] FIG. 7 is a top perspective view of the countertop cutout support jig;
[0015] FIG. 8 is a top perspective view of an under counter mount sink;
[0016] FIG. 9 is a top perspective view of an inverted laminate countertop;
[0017] FIG. 10 is a top perspective view of the sink seal mold;
[0018] FIG. 11 is a top perspective view of the surface routing assembly;
[0019] FIG. 12 is a top perspective view of the locator/dam ring with the hole routing jig and the countertop cutout support jig installed;
[0020] FIG. 13 is a top perspective of the countertop sink cutout being routed out from the top side of the countertop;
[0021] FIG. 14 is a top perspective view of an inverted countertop with the locator/dam ring, the hole routing jig and the countertop cutout support jig installed;
[0022] FIG. 15 is a top perspective of an inverted countertop with the locator/dam ring installed thereon;
[0023] FIG. 16 is a top perspective view of an inverted countertop with a locator/dam ring and the mold installed;
[0024] FIG. 17 is a top perspective of the surface routing jig, planing the exposed face of the seal with the inner ring installed;
[0025] FIG. 18 is a top perspective of the surface routing jig planing the exposed face of the flange with the inner ring removed;
[0026] FIG. 19 is a side cross section of a laminate countertop with a seal and under counter mounted sink; and
[0027] FIG. 20 is a bottom perspective view of the locator/dam ring showing the two positioning pins that extend therefrom.
DETAILED DESCRIPTION
[0028] There has thus been outlined, rather broadly, the more important features of the invention in order that the detailed description thereof that follows may be better understood and in order that the present contribution to the art may be better appreciated. There are, of course, additional features of the invention that will be described hereinafter and which will form the subject matter of the claims appended hereto.
[0029] In this respect, before explaining at least one embodiment of the invention in detail, it is to be understood that the invention is not limited in its application to the details of construction and to the arrangements of the components set forth in the following description or illustrated in the drawings. The invention is capable of other embodiments and of being practiced and carried out in various ways. Also, it is to be understood that the phraseology and terminology employed herein are for the purpose of descriptions and should not be regarded as limiting.
[0030] Looking at FIGS. 1 , 2 and 19 the undermount sink seal can best be seen. A sink 4 is located beneath a laminate countertop 2 ( FIG. 9 ) and physically held into place about numerous points of the bottom face of the sink flange 8 ( FIG. 8 ) by a series of clamping assemblies 16 which are affixed to the bottom face of the countertop 2 . A generally oval seal 10 having a planar flange 12 extending normally from its bottom edge is chemically bonded to the countertop 2 on the exposed edge of the sink cutout 14 and the bottom face of the countertop in an area matingly profiling that of the sink flange 8 . It is to be noted that this seal 10 is chemically bonded directly to the cut edge of the laminate and the cut edge of the particle board substrate that the laminate is affixed to. By directly affixing the seal 10 to both of the parts that make up the countertop 2 there can be no leakage. Direct chemical affixation of the seal 10 means that the polymer of the seal 10 is bonded to the laminate and the particle board substrate without the use of any other material. It is the use of a polymer such as an epoxy, a polyester, a urethane, an acrylic or combination thereof that in the seal forming process bonds directly to the laminate and substrate. (The inclusion of such material would leave just another point of water leakage as in the prior art.) The flange 12 of the seal is surface planed to be parallel to the top of the sink flange 8 and to be of a uniform thickness with respect to the planar countertop. In this fashion when fully installed, no water can get between the sink 4 and the countertop 2 , or contact the sink cutout.
[0031] The clamping assemblies 6 consist of clamp blocks 18 affixed to the bottom face of the countertop 2 , which constrain arced metal clamping plates 16 that cantilever beyond the edge of the clamp blocks 18 and onto the bottom face of the sink flange 8 . Short screws inserted through oblong slots in the center of the clamping plates 16 serve to tension upwardly the sink 4 onto the seal flange 12 . (Alternatively inverted bolts may be secured under the clamp blocks 18 so as to leave threaded studs protruding normally from the exposed bottom face of the clamp block, onto which nuts could be threaded.) One edge of each of the clamp blocks 18 abuts an edge of the flange 12 on the seal 10 . Since the clamp blocks 18 are thicker than the flange 12 this arrangement serves to define a positioning device for the placement of the sink 4 under the counter 2 such that the sink flange 8 resides directly atop the flange 12 on the seal.
[0032] With the seal flange 12 , matingly configured to the sink flange 8 and planed to enable full surface contact between the sink and the flange, a watertight seal can be formed between the two with the inclusion of a sealant, especially since the sink 4 may be precisely located onto the seal flange 12 when installed by virtue of the placement of the clamp blocks 18 about the seal flange's periphery.
[0033] The seal 10 is made of a polymer epoxy resin so as to be economical, of minimal toxicity to work with, extremely resilient and quick to set up and cure. There is a plethora of materials that would work suitably as seal material but in the preferred embodiment an epoxy resin is used. Other suitable casting resin materials include but are not limited to polyester, polyurethane, epoxy and acrylic casting resins or any modified combination there of. The seal is poured in place as a liquid polymer into a mold around the sink cutout region so as to directly bond to the laminate and the particle board substrate of the countertop.
[0034] Prior art seals used with top mounted sinks notoriously let water contact the laminate substrate as most of them were glued or frictionally fit into place. They did not have an extended seal flange 12 and seal 10 that were chemically affixed (epoxied) to the entire countertop cutout, a seal flange 12 that extended over the entire top face of the sink flange 8 , and a seal flange 12 that was matingly profiled to and planed parallel to the sink flange 8 so as to make a watertight seal. Additionally, the existing sink sealing systems did not have a physical positioning guide for the mounting of the sink precisely under their various seal arrangements.
[0035] The method of manufacturing the undermount sink seal utilizes a set of accurately dimensioned and interrelated jigs/templates including a locator/dam ring 20 , a hole routing jig 22 , a countertop cutout support jig 24 , a seal mold 26 , an inner routing ring 28 , and a surface routing jig 30 . A router 50 and a surface planing jig 52 are used for the cutting, trimming and surface planning operations. There are also the attendant mechanical fasteners, (preferably screws) as well as the polymer material used to make the sink seal, the silicon to bond the sink 2 to the seal flange 12 , and the release products for the mold and the locator/dam ring. In the preferred embodiment these are carnauba wax and a spray release agent (commonly of a silicon variety.)
[0036] The key component to making the seal 10 is the locator/dam ring 20 best seen in FIG. 6 . It is this jig that is anchored to the countertop, thus establishing all the positioning for the various operations, and upon which all the other jigs attach to. The locator/dam ring 20 is a generally enclosed rectangular template with two positioning pins 32 extending therefrom that are used to align the other templates associated with the seal creation and affixation and planning (Reference FIG. 20 for an underside view.) It is dimensioned so that when its leading edge contacts the front lip of the countertop this will determine and set the depth onto the countertop 2 that the sink 4 will reside and ensure that the front and back sides of the hole routed through the countertop 2 for the sink 4 will lie perpendicular to the front and back edges of the countertop 2 . The center cutout region of the locator/dam ring 34 has the same dimensions as the outside of the sink top flange 8 . On the two short sides of the locator/dam ring 20 are template locating members 36 also used to position and affix the other jigs/templates. In these members 36 there are screw attachment orifices 38 that allow the passage of screws therethrough to secure the jig to the bottom face of the countertop.
[0037] The hole routing jig 22 is best seen in FIG. 5 . It is a rectangular template designed to tightly fit within the center cutout region of the locator/dam ring 34 . The central cutout region of the hole routing jig 41 is matingly conformed to the sunken or concave region of the sink. There are also screw attachment orifices 38 that allow the passage of screws therethrough to secure it to the bottom face of the countertop 2 .
[0038] The countertop cutout support jig 24 as best seen in FIG. 7 merely has a set of linear arms 44 that span the template locating members 36 and are affixed to them through screws 40 passing through the linear arm 44 and into t-nut attachment orifices 39 located on the underside of the locator/dam ring 20 . Across the linear arms 44 are a pair of cutout arms 46 also having screw attachment orifices 38 that allow the linear arms 44 to be screwed to the countertop in the region to be cutout for the sink 2 installation.
[0039] FIG. 12 shows the locator/dam ring 20 with the hole routing jig 22 installed and the countertop cutout support jig 24 attached.
[0040] Looking at FIG. 10 the seal mold 26 can best be seen. It has a rectangular frame 54 that supports the mold form 56 and toggle pressure clamps 58 . On two sides of the seal mold 26 are alignment strips 60 with locating orifices 62 formed therethrough. These locating orifices 62 are dimensionally sized to receive positioning pins 32 of the locator/dam ring 20 . (The pins are visible in FIG. 13 .) When the seal mold 26 is located beneath the countertop 2 and the pins 32 are inserted in the locating orifices 62 , the seal mold 26 will be correctly aligned with the sink cutout such that the mold form 56 will extend through the sink cutout and the exterior profile of the mold form 56 will reside in a uniformly spaced placement about the periphery of the sink cutout. This is the gap or region into which the seal mold polymer resin will be poured and the sink seal 10 will be formed.
[0041] There is a series of toggle pressure clamps 58 positioned about the mold form 56 and mounted on the support backer plate 64 . The clamp arms of these toggle pressure clamps 58 span across the gap onto the locator/dam ring 20 and when actuated serve to raise the mold form 56 into tight contact with the laminate countertop, thus allowing no seepage by of the seal material and resulting in a sharply defined interface between the countertop laminate and the seal 10 . This is critical to both the visual aesthetics and the integrity of the waterproof seal at the laminate seal interface. In this manner there will be no seepage of seal material onto the top face of the countertop laminate.
[0042] The mold form 56 is made of polyurethane resin in the preferred embodiment as it works well with the preferred embodiment casting of the seal 10 with epoxy casting resin although room temperature vulcanizing (RTV) silicon has also been successfully used. The polyurethane resin of the mold generally will be of a low enough durometer so as to be flexible and slightly compressive. These features of the mold are critical as they allow the mold form 56 to be tightly fitted and compressed against the laminate countertop 2 so as to make a leak proof seal preventing the seal casting resin material from leaking out during fabrication of the seal 10 , and securely maintaining the mold form 56 in its proper position.
[0043] The surface routing jig 30 ( FIG. 4 ) is a rectangular template with a recess on the bottom side which dimensionally matches the exterior dimensions or profile of the flange 8 . It has screw attachment orifices 38 about it to allow it to be mechanically secured to the countertop 2 . About its inner periphery is a rabbeted edge 60 that accepts the inner routing ring 28 .
[0044] The inner routing ring 28 , ( FIG. 3 ) is a template sized for insertion into the surface routing jig 30 . The outer profile of the inner routing ring 28 is matingly dimensioned and profiled to fit into the inner periphery of the surface routing jig 30 . The inner profile of the inner routing ring 62 matches the profile of the outer edge of the seal 10 .
[0045] FIG. 11 shows the router 50 attached to the surface routing spanner board 52 . The spanner board is of a length sufficient to span over the sides of the surface routing jig 30 , so as to maintain the cutting bit of the router at a constant height with respect to the bottom face of the laminate countertop. As is well known in the field of surface routing, a bushing is affixed at a uniform radius from the center of the cutting bit (affixed to either the spanner board or the router base.) This will allow precision locating when routing the surface as the busing will contact the peripheral sides of the templates used in the surface routing process as described herein.
[0046] The mounting of the sink to the countertop uses the clamping assembly 6 detailed above and best illustrated in FIG. 2 .
[0047] The steps to fabricating the sink seal as described above are as follows:
[0000] 1. Paint a coat of release wax (preferably carnauba paste wax) on the underside and inside edge of the locator/dam ring 20 and allow sufficient time to dry. (Note it is only put onto the underside as a precaution if epoxy resin leaks under the rim.)
2. Spray RTV release bond onto the mold form 56 portion of the mold 26 .
3. Lay the countertop 2 upside down so that the laminate surface is face down and the bottom face of the countertop 2 is facing upward. Place locator/dam ring 20 onto the bottom face of the countertop, ensuring the outside leading edge of the locator/dam ring 20 firmly contacts and abuts the inside edge of the front lip of the countertop 2 . Slide the locator/dam ring 20 to the position where the sink 4 is to be located. Insert screws through the screw attachment orifices 38 located along the four sides of the locator/dam ring 20 and threadingly engage them into the bottom face of the laminate countertop 2 to secure the locator/dam ring 20 in its desired position. A screw should be used at numerous locations about all four sides to eliminate any movement of the locator/dam ring 20 during routing/placement operations. Before inserting screws the bottom face of the countertop should be center punched through the screw attachment orifices 38 . This step allows the screws to go in perpendicular to the bottom face and completely parallel to the attachment orifices 38 . Any angular insertion of a screw will distort the locator/dam ring's profile.
4. Insert the hole routing jig 22 into the locator/dam ring 20 . These are close tolerance fits with the outside dimensions of the hole routing jig 22 approximating the inside dimensions of the locator/dam ring 20 . Affix the hole routing jig 22 to the bottom face of the countertop 2 in the same fashion as was done with the locator/dam ring 20 above using screws through the screw attachment orifices 38 .
5. Attach the countertop cutout support jig 24 to the locator/dam ring 20 by placing screws through screw attachment orifices 38 in the corners of the countertop cutout support jig 24 that pass through aligned screw attachment orifices 38 in the locator/dam ring 20 . Attach the countertop cutout support jig 24 to the bottom face of the countertop 2 through the use of screws through the screw attachment orifices 38 as described above. The assembly of the locator/dam ring 20 , the hole routing jig 22 and the countertop cutout support jig 24 is seen in FIG. 12 . FIG. 14 shows this assembly mounted onto the countertop.
6. Drill a starting hole for the router bit through the countertop 2 within the area bounded by the inside of the locator/dam ring 20 .
7. Install a flush cut straight router bit with a ⅛ inch diameter oversized guide bearing on the bottom. The guide bearing has a diameter that is ⅛ of an inch larger than the diameter of the flush cut bit. Flip the entire assembly over and insert the router bit through the starting hole so the router resides on the top surface of the counter. Route the sink opening out so that the center cutout of the countertop is no longer a contiguous section of the countertop as best seen in FIG. 13 .
8. Remove the oversized guide bearing and install a size for size guide bearing on the bottom of the flush cut straight router bid. Reroute the sink opening. This step now removes the final 1/16 inch of countertop material and ensures the finish cut in the laminate countertop is extremely smooth. This step of double routing is key to getting a proper tight interface edge between the seal and the countertop. Aesthetically this will allow for a clean demarcation between the seal 10 and the countertop 2 .
9. Flip the routed assembly over and remove the countertop cutout support 24 by removing screws 40 and lift the countertop cutout support 24 from the locator/dam ring 20 with the sink cutout still affixed to the countertop cutout support 24 . The locator/dam ring 20 remains affixed to the countertop.
10. Remove the hole routing jig 22 by removing the screws and lifting it out of the locator/dam ring 20 .
11. Spray silicon release wax onto the mold form 56 . (All toggle clamps fully released.) Place the locator/dam ring 20 onto the mold 26 aligning the two into their critical nested spacing with the countertop 2 still attached and oriented face down. To accomplish this, there is a set of alignment pins 32 on the bottom face of the locator/dam ring 20 that engage in a set of mating locator orifices 62 in the mold 26 . All of the numerous toggle (compression) clamps 58 about the periphery of the mold form 56 are engaged to frictionally contact the locator/dam ring 20 . This step is critical to get a perfectly tight seal that does not allow any of the seal resin to leak by the cutout edge of the laminate countertop 2 .
12. Mix the seal material as per manufacturer's directions adding pigment as necessary. Although the preferred embodiment uses an epoxy casting resin there is a plethora of other materials that may also be used to form the sink seal 10 . Epoxy resin was chosen because of its long working times, hand mixing ability, low odor and volatile organic vapors.
13. Pour the epoxy into the annulus created between the mold form 56 , the sink cutout in the countertop and the locator/dam ring 20 . Let cure as per the manufacturer's directions.
14. Release all toggle pressure clamps 58 and lift the countertop 2 away from the mold 26 (with the locator/dam ring 20 still attached.) Remove the locator/dam ring 20 from the countertop 2 by removing the screws. (The counter sink hole now has an interior periphery epoxy seal ring 10 with an extended epoxy flange 12 formed on the bottom face of the counter.)
15. Place a surface routing jig 30 over the extended epoxy flange 12 . The inside profile of the surface routing jig 30 dimensionally matches the exterior dimensions or profile of the extended epoxy flange 12 . Attach a surface routing jig 30 onto the bottom face of the counter 2 with screws through screw attachment orifices 38 . Place the inner routing ring 28 into the surface routing jig 30 . The outer profile of the inner routing ring is matingly dimensioned and profiled to fit into the inner periphery of the surface routing jig 30 . A router on a spanner board ( FIG. 11 ) is used (as is well known in the industry) to allow the router bit to be held a constant depth off of the bottom face of the countertop. Counterclockwise rout the inside edge of the flange's 12 bottom face planar, tracing the inner routing ring.
16. Remove the inner routing ring 28 and then clockwise rout the outside edge of the of the flange 12 . The entire seal 10 should now be a uniform thickness with respect to the bottom face of the counter and parallel to the sink flange 8 . There should be no nicks in either of the edges of the flange 12 .
17. Remove the surface routing jig 30 .
18. Place the sink attachment blocks 6 directly abutting the extended epoxy flange 12 . These are glued and screwed directly to the bottom face of the counter 2 with their embedded studs extending normally therefrom. These give a solid surface for the cantilever clips 16 to be secured into and serve as a locator for the sink placement for the in field installation of the sink.
[0048] In the field, the installer need just apply a suitable silicone or other sealant to the top face of the sink flange 8 , raise the undermount sink 4 below the sink cutout aligning the edges of the sink 4 with the sides of the clamp blocks 6 . The sink 4 is then propped up in place while a mechanical fastener is utilized in the slot of a clamping plate 16 and the clamping plate in tensioned until one end of the contacts the sink flange 8 and one end contacts the clamp block 6 .
[0049] In an alternate embodiment, the seal 10 would be removably cast and hardened on a surface that had a profile that matched the sink cutout and the finished seal 10 would then be affixed to the sink cutout by an adhesive. The seal 10 in this case may be made to an extended height and once adhesively affixed to the sink cutout, routed down level with the top face of the laminate.
[0050] The above description will enable any person skilled in the art to make and use this invention. It also sets forth the best modes for carrying out this invention. There are numerous variations and modifications thereof that will also remain readily apparent to others skilled in the art, now that the general principles of the present invention have been disclosed. As such, those skilled in the art will appreciate that the conception, upon which this disclosure is based, may readily be utilized as a basis for the designing of other structures, methods and systems for carrying out the several purposes of the present invention. It is important, therefore, that the claims be regarded as including such equivalent constructions insofar as they do not depart from the spirit and scope of the present invention. | An under counter mount sink sealing surface and method of making that provides a watertight interface between an under counter mount sink and a laminate counter as well as a simplified and more dimensionally accurate method of field installing the sink below the counter. The water impervious seal is tightly chemically bonded to the cutout lip of the laminate as well as to the entire area on the bottom face of the laminate countertop that contacts the entire profile of the top face of the under counter mount sink. The seal also aligns the sink into the correct location and contacts the entire surface of the as it is deck aligned or completely parallel to the sink top flange. | 4 |
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates generally to novel peptides of formula I R 1 -His-Asp-Glu-Ala-R, wherein R 1 is Ala-Gln and R is
Gln-Gln-Asn-Ala-Phe-Tyr-Gln-Val-Leu-Asn-Met-Pro-Asn-Leu-Asn-Ala-Asp-Gln-Arg-Asn-Gly-Phe-Ile-Gln-Ser-Leu-Lys-Asp-Asp-Pro-Ser-Gln-Ser-Ala-Asn-Val-Leu-Gly-Glu-Ala-Gln-Lys-Leu-Asn-Asp-Ser-Gln-Ala-Pro-Lys
and wherein at least one, more or all of the amino acid residues in R 1 , R, or both is omitted; and physiologically compatible salts or esters thereof. These peptides exhibit interesting and surprising pharmacological properties in that they possess the ability to augment cell-mediated cytotoxity. The present invention therefore also relates to pharmaceutical compositions containing at least one of these peptides, their use as a medicament, e.g. an anticancer or antiviral agent, and methods for augmenting cell-mediated cytotoxicity in humans and other mammals.
In the following specification and claims the nomenclature used herein complies with that stated in J.Biol.Chem 247 (1972), 977 et seq.
2. Brief Description of the Background Art
Cancers and viral infections are serious conditions and until now no medicament has been found which can be used against all cancers or viral infections without side effects.
Natural killing (hereinafter NK) and antibody-dependent cellular cytotoxicity (hereinafter ADCC) are known examples of immunological defense mechanisms against cancer and viral infections. Several studies have indicated the relation between these types of cellular cytotoxic reactions and defense mechanisms against cancer as well as against viral infections. Therefore, stimulation of NK- and/or ADCC-activity as well as other mechanisms of cellular cytotoxicity (hereinafter collectively designated cellular killing (K-cell activity)) in vivo is believed to be of great relevance for the treatment of cancers and viral infections.
It has been demonstrated that one group of proteins, i.e. the interferons, stimulates these types of reactions. It is also known that certain other peptides and proteins stimulate K-cell activities. The lymphokine interleukin-2 has been indicated as particularly important for the stimulation of K-cell activity, and the augmentation of K-cell activity by lymphokines after stimulation for 3-5 days is often referred to as lymphokine activated killing (hereinafter LAK) and stimulated cells are referred to as lymphokine activated killer cells (hereinafter LAK-cells).
It is known that protein A from Staphylococcus aureus stimulates K-cell activities.
It is further known that S. aureus protein A (hereinafter SpA) has a number of other immunologic properties, including activation of the complement system, polyclonal stimulation of B- and T-lympocytes, polyclonal activation of antibody synthesis and interferon induction.
These properties of SpA have led to a great deal of interest in the use of SpA as an immunologic reagent, and it is most desirable to find a way to exploit the useful properties of SpA without triggering the more adverse properties of this protein.
SpA cannot be employed directly in vivo since it may cause hypersensitive reactions (probably due to its binding to the Fc part of immunoglobulins with subsequent activation of complement etc.). Various preparations of the complete SpA molecule have, however, been utilized either for extracorporeal large-scale plasma adsorption (J. Balint jr. et al.: Cancer Research 44 (1984), 734-743), which was interpreted in terms of interaction with immunoglobulins in immune complexes, or for intravenous infusion in animals (H.D. Harper et al.: Cancer 55 (1985), 1863-1867) with beneficial results.
Protein A from S. aureus is a protein of which the NH 2 -terminal part contains five homologous units comprising from 56 to 61 amino acids each, and the COOH-terminal part contains several repeats of an octapeptide (cf. Uhlen M. et al.: J.Biol.Chem. 259, 3 (1984), 1695-1702).
The five homologous regions in the N-terminal part are usually designated E, D, A, B, and C regions, and the C-terminal part is designated the X region.
The structure of SpA has been extensively studied and is described in a number of publications such as WO No. 8400773, WO No. 8400774, WO No. 840310 all to Pharmacia AB, and EP No. A2 107,509 to Repligen Corp. whereto reference is made.
The results obtained in studies performed by J. Sjodahl and G. Moller (Scand.J.Immunol. 10 (1979), 593-596) and Olinescu et al. (Immunol.Letters 6 (1983), 231-237) have been interpreted as indicating that the active part of the SpA molecule should be in the so-called X region, the C-terminally located portion of the molecule.
SUMMARY OF THE INVENTION
It has now, surprisingly, been found that peptides of formula I below have K-cell stimulating activity. A number of compounds of formula I have been identified from proteolytic cleavage of SpA and isolation of fragments that show no or low binding to immunoglobulins (i.e. they are substantially devoid of immunoglobulin cross-linking activity). These fragments have been shown to have K-cell stimulating activity in vitro against both NK-sensitive and insensitive target cells.
As indicated above the peptides of this invention may be derived from SpA as fragments consisting of a continous part of the amino acid sequence of the so-called region E, (cf. Uhlen M. et al.: J.Biol.Chem. 259, 3 (1984), 1695-1702), which fragments comprise from 4 and up to 55 amino acid residues from the entire sequence of region E.
In one aspect the invention thus relates to peptides of the general formula I
R.sup.1 -His-Asp-Glu-Ala-R (I)
wherein R 1 is Ala-Gln and R is
Gln-Gln-Asn-Ala-Phe-Tyr-Gln-Val-Leu-Asn-Met-Pro-Asn-Leu-Asn-Ala-Asp-Gln-Arg-Asn-Gly-Phe-Ile-Gln-Ser-Leu-Lys-Asp- Asp-Pro-Ser-Gln-Ser-Ala-Asn-Val-Leu-Gly-Glu-Ala-Gln-Lys-Leu-Asn-Asp-Ser-Gln-Ala-Pro-Lys
and wherein at least one, more or all of the amino acid residues in R 1 , R, or both is omitted; and physiologically compatible salts or esters thereof.
A subclass of peptides according to the invention is peptides of formula I wherein R 1 and R are defined as above, and wherein the only part of R 1 that is omitted constitutes a continuous part of the amino acid sequence of R 1 from the N-terminal end, and the only part of R that is omitted constitutes a continuous part of the amino acid sequence of R from the C-terminal end.
As examples of specific and preferred peptides of formula I the following can be mentioned
Ala-Gln-His-Asp-Glu-Ala-Gln-Gln-Asn-Ala-Phe-Tyr-Gln-Val-Leu- Asn-Met-Pro-Asn-Leu-Asn-Ala-Asp-Gln-Arg-Asn-Gly-Phe-Ile-Gln- Ser-Leu-Lys-Asp-Asp-Pro-Ser-Gln-Ser-Ala-Asn-Val-Leu-Gly-Glu- Ala-Gln-Lys-Leu-Asn-Asp-Ser-Gln-Ala-Pro, pX-3' (corresponding to the 55 N-terminal amino acid residues in region of SpA),
Ala-Gln-His-Asp-Glu-Ala-Gln-Gln-Asn-Ala-Phe-Tyr-Gln-Val-Leu- Asn-Met-Pro-Asn-Leu-Asn-Ala-Asp-Gln-Arg, pX-1' (corresponding to the first 25 amino acid residues in region E),
Ala-Gln-His-Asp-Glu-Ala-Gln-Gln-Asn-Ala-Phe-Tyr-Gln-Val-Leu- Asn-Met-Pro-Asn-Leu, pX-2' (corresponding to the first 20 amino acid residues in region E),
Gln-His-Asp-Glu-Ala-Gln-Gln-Asn-Ala-Phe-Tyr-Gln-Val-Leu-Asn- Met-Pro-Asn-Leu, pX-4' (corresponding to amino acid residues 2 to 20 in region E), and
His-Asp-Glu-Ala-Gln-Gln-Asn-Ala-Phe-Tyr-Gln-Val-Leu-Asn-Met- Pro-Asn-Leu, pX-5' (corresponding to amino acids 3 to 20 in region E).
In another aspect the invention relates to pharmaceutical compositions containing at least one peptide of the general formula I in combination with an inert carrier or excipient.
In a further aspect the invention relates to compositions useful for augmenting K-cell activity in animal cells which comprise a peptide with an amino acid sequence corresponding to the E-region of SpA or fragments thereof, said peptide characterized further in that it is substantially devoid of immunoglobulin binding activity, and physiologically acceptable salts or esters thereof, together with a physiologically acceptable carrier.
The compositions of the invention may further contain one or more other active substances, e.g. interferons, lymphokines and/or monokines.
In a further aspect the invention relates to a method of combating conditions of cancers or viral infections in mammals including humans by administering a therapeutically effective amount of at least one of said compositions to a subject suffering from cancer or a viral infection.
In a still further aspect the invention relates to the use of a peptide of the formula I or a peptide with an amino acid sequence corresponding to the E region of SpA or fragments thereof as a medicament for administration to mammals, including humans.
In yet another aspect the invention relates to a method of augmenting cell mediated cytotoxicity in mammals by administering an effective amount of at least one peptide of formula I in a quantity sufficient to augment K-cell activity.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 shows the amino acid sequences of the region E of protein A from Staphylococcus aureus strain 8325-4 (cf. Uhlen et al., above),
FIG. 2 shows the elution pattern obtained in the isolation of a peptide according to the invention,
FIG. 3 shows the results of a comparative test between SpA and non IgG binding fragments, and
FIG. 4 shows the results of a test for complement activation by SpA and a peptide according to the invention.
DETAILED DESCRIPTION OF THE INVENTION
The invention is based on the surprising observation that apparently the ability of SpA to augment cell mediated cytotoxicity resides in the E region or fragments thereof.
Further it has also surprisingly been found that the E region or fragments thereof have no or low affinity to immunoglobulins whereby activation of complement is substantially eliminated.
All these fragments in question comprise the amino acid residues His-Asp-Glu-Ala.
In FIG. 1 the amino acid sequence of region E is shown with markers indicating the preferred peptides of the invention.
The present invention provides a number of peptides which may be derived from the amino acid sequence of the E region of SpA. One of these was derived from plasmin digestion of SpA and the amino acid sequence defined as follows: ##STR1##
Another was synthesized as: ##STR2##
Both these peptides of the invention were tested and observed to augment cell mediated cytotoxicity in in vitro assays for the augmentation of K-cell activity.
The amino acid sequences of pX-1' and pX-2' correspond to those of the first 25 and 20 amino acid residues, respectively, in SpA, corresponding to the N-terminal part of region E, which region comprises the first 56 amino acids of SpA.
The peptides of the invention may be synthesized by any method known to those skilled in the art. A summary of such techniques may be found in J.M. Stewart and J.D. Young, Solid Phase Peptide Synthesis, W.H. Freeman, San Francisco, 1969 and J. Meienhofer, Hormonal Proteins and Peptides, Vol. 2, (1973), p. 46, Academic Press, New York, for solid phase synthesis, and in E. Schroder and K. Lubke, The Peptides, Vol. 1, (1965), Academic Press, New York, for classical solution synthesis.
In general these methods comprise the sequential addition of one or more amino acids, or suitably protected amino acids, to a growing peptide chain. Normally, either the amino or the carboxyl group of the first amino acid is protected by a suitable protecting group. The protected or derivatized amino acid can then be either attached to an inert solid support or utilized in solution by adding the next amino acid in the sequence having the complementary (amino or carboxyl) group suitably protected, under conditions suitable for forming the amide linkage. The protecting group is then removed from this newly added amino acid residue and the next amino acid (suitably protected) is then added, and so forth. After all the desired amino acids have been linked in the proper sequence, any remaining protecting groups (and any solid support) are removed sequentially or concurrently, to afford the final peptide. By simple modification of this general procedure, it is possible to add more than one amino acid at a time to a growing chain, for example, by coupling (under conditions which do not racemize chiral centers) a protected tripeptide with a properly protected dipeptide to form, after deprotection, a pentapeptide.
In addition the subject polypeptides may be prepared by recombinant DNA technology, for example by modification and utilization of a part of the DNA sequences coding for S. aureus protein A.
The peptides of the invention may also be produced by proteolytic or chemical cleavage of SpA and subsequent fractionation and isolation of the SpA fragments.
For the digestion various proteolytic enzymes may be used such as trypsin, plasmin, Armillaria mellea protease or clostripain, chymotrypsin, carboxypeptidases or S. aureus V8 protease. For chemical cleavage CNBr, acids or bases could be used.
The isolation of the peptides may be performed by any suitable method known to those skilled in the art, such as by High Pressure Liquid Chromatography (HPLC).
Peptides of formula I or peptides with an amino acid sequence corresponding to the E-region of SpA or fragments thereof are converted into pharmaceutical compositions and administered, preferably to humans, in analogy with known methods. Said peptides and salts or esters thereof can be administered perorally, topically, rectally, vaginally, intraveneously, intramuscularily, intrathecally or subcutaneously at dosages in the range of from about 1 to 1000 μg/kg body weight, although a lower or higher dosage may be administered. The required dosage will depend on the severity of the condition of the patient, the peptide used, the mode of administration and the duration of treatment.
The compositions may be formulated in the form of slow-release or depot preparations.
For the purpose of parenteral administration, the said peptides are dissolved in sterile, isotonic saline solutions.
As examples of salts of the above mentioned peptides, for example sodium, potassium, magnesium, calcium and zinc salts and acid addition salts with organic or inorganic acids such as formic acid, methanesulphonic acid, hydrochloric acid and sulphoric acid can be mentioned. Preferred salts of the said peptides are physiologically and pharmaceutically acceptable salts.
Over and above one of said peptides or a salt or ester thereof the pharmaceutical compositions may comprise a pharmaceutically acceptable carrier, diluent, preferably isotonic saline solutions, and/or excipient.
The present invention will be described in greater detail in the following examples, which in no way are intended to limit the scope of the invention as set forth in the appended claims.
EXAMPLE 1
Preparation of peptides by proteolytic cleavage of SpA
(a) Digestion with Plasmin
15 mg of purified SpA from Pharmacia, Uppsala, Sweden, were dissolved in 600 μl of 0.1 M ammonium formate (pH 7.5) and 600 μl of plasmin (corresponding to 14 CU (casein units)) dissolved in the same buffer was added. The mixture was incubated at 37° C. for 205 minutes. The reaction was terminated by adding aprotinin coupled to Sepharose® 4B followed by a further 15 minutes of incubation at room temperature. Subsequently, the reaction mixture was centrifuged, and the supernatant was drawn out by suction. 1.0 ml of 0.1 M ammonium formate was added to the pellet (containing immobilized aprotinin as well as remaining reaction mixture), the sample was mixed and centrifuged, and the supernatant was drawn out by suction. The latter procedure was repeated twice.
Finally all the supernatants were combined and lyophilized repeatedly.
(b) Purification.
The peptides from above were purified by high pressure liquid chromatography (HPLC) on a reverse phase column (Nucleosil® 5C 18 ) using the following equipment: 2 LKB 2150 HPLC pumps, LKB 2151 variable wavelength monitor, LKB 2152 HPLC controller, LKB 2220 recording integrator and LKB Superrac.
The purification was performed as follows:
Buffer A: 0,02 M ammonium formate (pH 6.5); buffer B: 40% 0.05 M ammonium formate (pH 6.5) and 60% ethanol; flow rate: 0.5 ml/min; fraction volume: 0.25 ml.
The material in fractions 150-152 was selected for characterization.
The results of the HPLC purification are shown in FIG. 2, wherein the selected fractions are indicated.
The product contained two peptides that were sequenced according to the following protocol:
Edman degradations of the peptides were performed with an Applied Biosystems model 470A gas phase sequencer as described (R.M. Hewick, M.W. Hunkapiller, L.E. Hood and W.J. Dreyer: J.Biol.Chem. 256 (1981) 7990-7997; M.W. Hunkapiller, R.M. Hewick, W.J. Dreyer and L.E. Hood: Methods Enzymol. 91 (1983) 399-413) with several modifications. A fourth solvent (Sl =n-heptane) was included for washing the filter for 30 seconds after coupling with phenylisothiocyanate (PITC). In order to obtain the methylated derivatives of Asp and Glu, the conversion of amino acid anilinothiazolinones to phenylthiohydantoins was carried out with 1 N methanolic HCl instead of 25% trifluoroacetic acid (TFA). The sequencer program was adjusted to this reagent, as shorter drying periods were necessary. The phenylthiohydantoine amino acids (PTH-a.a.) were dissolved in approximately 0.25 ml of methanol and dried in a Savant vacuum centrifuge for 10 min at 45° C. Dried PTH-a.a. were redissolved in 0.025 ml of methanol containing methylthiohydantoin-(MTH)-tyrosine as internal standard. The PTH-a.a. were identified and quantified by reverse phase HPLC on a 25 cm×0.46 cm IBM cyano column equipped with a 5 cm×0.46 cm Permaphase® ETH cyano guard column (DuPont) (M.W. Hunkapiller and L.E. Hood: Methods Enzymol. 91 (1983) 486 Hunkapiller 493) in a Hewlett Packard Liquid Chromatograph Model 1084B equipped with a variable UV detector Model 79875. The A solvent was 16 mM sodium acetate, pH 5.60, and the B solvent was acetonitrile/methanol, 9:1 (v/v). The column was equilibrated with 15% of B and eluted with a linear gradient of 15% - 51.4% B for 0-15.30 min. The PTH-a.a. were detected at 263 nm at 1.5 mAUFS (Absorption Unit Full Scale).
The amino acid sequence data are shown in table 1 below:
TABLE 1______________________________________Sequence analysis of peptide poolSample: Fraction 150-152 (see FIG. 2)Average repetitive yield: 95.7% Amount AmountCyclus No. PTH-a.a. (pmol) PTH-a.a. (pmol)______________________________________ 1 Asp 391 Ala 853 2* Gln (1500) Gln (750) 3 Gln 1405 His 266 4 Ser 59 Asp 168 5 Ala 870 Glu 424 6 Phe 715 Ala 505 7 Tyr 1062 Gln 749 8* Glu (850) Gln (425) 9 Ile 746 Asn 66510 Leu 624 Ala 36011 Asn 531 Phe 29812 Met 575 Tyr 45413 Pro 519 Gln 56014 Asn 820 Val 383 15* Leu (483) Leu (241) 16* Asn (737) Asn (368)17 Glu 198 Met 32318 Ala 288 Pro 17619 Gln 540 Asn 41920 Arg 140 Leu 39221 Y.sub.1 --22 Ala 28023 Y.sub.2 --24 Gln 7925 Arg 177______________________________________ *Here the same amino acid residue appears in both peptides, the amount found is therefore shared proportionally between the peptides.
It appears from table 1 that the purified pooled material contains a mixture of two peptides. The unidentified amino acid residues Y 1 and Y 2 can be assigned as Asn and Asp, respectively, by comparing the sequence with the sequence of protein A from S. aureus (Uhlen et al., above).
The product thus consist of 33% of a peptide, pX-1', of formula I with R 1 being Ala-Gln, and R being Gln-Gln-Asn- Ala-Phe-Tyr-Gln-Val-Leu-Asn-Met-Pro-Asn-Leu-Asn-Ala-Asp-Gln-Arg (III) corresponding to the first 25 amino acid residues in the N-terminal part of SpA, which are also the first 25 amino acid residues in the N-terminal part of region E; and 67% of a peptide corresponding to amino acid residues 11 to 30 in region D.
The product was shown to have K-cell activity augmenting activity in the assay procedures detailed below.
EXAMPLE 2
Preparation of peptide mixtures by proteolytic cleavage of SpA
(a) Digestion with plasmin
150 μg purified SpA were digested with 0.3 CU (casein units) plasmin (KABI) at 37° C. for 60 min.
The reaction was terminated by adding aprotinin coupled to Sepharose® 4B and incubation for 15 minutes at room temperature. The supernatants were removed after centrifugation and used in the experiments below.
(b) Analysis of K cell stimulation activity
To evaluate the importance of non-Fc binding peptides in in vitro stimulation of K cell activity, the proteolytic digests from above (corresponding to 8 μg SpA) were incubated with human IgG coupled to Sepharose 4B or with control Sepharose 4B for 30 minutes at room temperature. Purified SpA was incubated under identical conditions as control. The reaction mixtures were centrifuged and the supernatants were used directly in the K cell assay as detailed below. Thus normal peripheral blood leukocytes (PBL) were incubated with (1) SpA absorbed with IgG-Sepharose 4B, (2) SpA absorbed with control-Sepharose 4B, (3) plasmin-digested SpA absorbed with IgG Sepharose 4B, (4) plasmin-digested SpA absorbed with control-Sepharose 4B. PBL incubated with medium alone served as controls. The results expressed as Kill % are given in FIG. 3. It appears that it is possible by proteolytic cleavage of purified SpA to obtain peptides with no or low IgG binding, but with K cell stimulation activity.
EXAMPLE 3
Synthetic preparation of peptides
pX-2'
(a) Ala-Gln-His-Asp-Glu-Ala-Gln-Gln-Asn-Ala-Phe-Tyr- Gln-Val-Leu-Asn-Met-Pro-Asn-Leu, pX-2', corresponding to the first 20 amino acid residues of the N-terminal part of region E was prepared synthetically as indicated above.
pX-2' showed K-cell activity augmenting activity in the assay procedures below.
Assay procedures
K-cell activity is here defined as the increase in cell mediated cytotoxicity of normal peripheral blood leukocytes (PBL) against tumor derived target cells. PBL were isolated by the Boyum method (Scand.J.Clin.Lab.Invest. 22 (1968) 77) by centrifugation of heparinized blood from healthy donors on Ficoll-Hypaque® (Pharmacia, Uppsala, Sweden). In many experiments adherent cells were removed by incubating PBL in sterile glass bottles at 37° C. for 1 to 2 hours. As target cells the NK-sensitive K562 (C.B. and B.B. Lozzio, J.Nat.Cancer Inst. 50 (1973) 535-538) as well as the relatively NK-resistant Daudi (E. Klein et al., Cancer Res. 28 (1968) 1300-1310) and Raji (R.J.V. Pulvertaft, J.Clin.Pathol. 18 (1965) 261-273) cell lines were used for the peptides obtained by proteolytic digestion of SpA, while only Raji and Daudi cell lines were used for the synthetic peptides.
The cell lines were kept in culture in RPMI 1640 (Gibco, Paisley, Scotland, Cat. No. 041-1875) to which was added fetal calf serum (10% v/v) (FCS) as well as penicillin (100 IU/ml) and streptomycin (100 μg/ml) at 37° C. and carbon dioxide in air.
The target cells were labelled with 51 Cr (New England Nuclear, Dreieich, West Germany).
K-cell assay
PBL were incubated with purified peptides or with SpA for 24 h at 37° C. with 6% CO 2 in air. The medium used was RPMI 1640 to which was added 10% of FCS, penicillin (100 IU/ml) and streptomycin (100 μg/ml). After incubation, the cell density was adjusted and the cells were distributed in round-bottom microtiter plates (NUNC, Roskilde, Denmark). 51 Cr-labeled K562 target cells were added to a desired ratio between effector (E) and target (T) cells (E/T 10:1). After a further 4 hours of incubation at 37° C. with 6% CO 2 in air, the plates were placed on a Titertek® microtiter plate shaker (Flow Laboratories Ltd., Ayrshire, Scotland). The microtiter plates were centrifuged and known volumes of the supernatant removed by suction and counted 51 Cr-sample). As maximum value ( 51 Cr-max), use was made of the supernatant from K562 incubated with saponin. The spontaneous release of 51 Cr ( 51 Cr-spont) was measured by incubating 51 Cr-K562 without effector cells. The specific percentage of killing (Kill %) was calculated using the following equation (all values referring to 51 Cr in directly comparable supernatants):
Kill %: 100( 51 Cr-sample - Cr-max 51 Cr-sample - 51 Cr-spont)/( 51 Cr-may / 51 Cr-spont)
The method employed was practically the same as above for Daudi and Raji targets. The only substantial difference was that no preincubation was performed prior to addition of the 51 Cr-labelled target cells, and the complete incubation of effector and target cells was done in 24 hours. The Kill % was calculated as described above.
The above assays for the activity of the peptides were used for the final characterization as well as in several screening tests. The screening tests were performed directly on fractions from the different steps of the HPLC-purification, and in most instances the fractions were lyophilized first. Two different target cells (K562 and Daudi) were used in the screening tests. Only those fractions that were positive in both test systems were used in the further purification and characterization.
Short-term test. NK-like activity
4×10 5 monocyte-depleted mononuclear cells were incubated with 4×10 4 51 Cr-labelled Raji cells. Total volume: 800 μl. To this was added 1.5, 6, 25 or 100 μg of peptide per ml, respectively. Controls were unstimulated effector cells + 51 Cr-labelled Raji and effector cells stimulated with SpA (20 μg/ml) (in duplicate). After 2 hours of incubation 3×200 μl were taken out for incubation in round-bottom microtiter trays. Incubation was carried out at 37° C., 7% CO 2 , 18h.
Long-term test. LAK-like activity
6×10 6 monocyte-depleted mononuclear cells were incubated in 6 ml RPMI 1640 +5% FCS, penicillin (100 IU/ml) and streptomycin (100 μg/ml) in vertically suspended Falcon flasks (Falcon Plastics, Oxnard, CA., USA, Cat. No. 3013). As in the short-term test, 1.5, 6, 25 or 100 μg peptide per ml, respectively, were added. Controls: unstimulated effector cells and effector cells +SpA (20 μg/ml). Incubation for 72 h at 37° C., 7% CO 2 . The cells were counted, density adjusted and the cells incubated together with 51 Cr-labelled Raji and Daudi target cells. E/T ratios were: 10:1 and 20:1. In the Daudi test the incubation lasted 16 hours, in the Raji test it was 18 hours (round-bottom microtiter plates, as above).
The results of the above assays are shown in the following table 2 for the SpA peptides and in table 3 for the synthetic peptides.
TABLE 2______________________________________Natural killer (NK)-like activity induced by incubation ofperipheral blood lymphocytes (PBL) with peptides isolated fromproteolytic digests of SpA or intact SpA. % kill* Raji Daudi______________________________________Control 15 46Pool (pX-1'**) approx. 100 pmol/ml 27 75 20 pmol/ml 27 72 4 pmol/ml 24 68Protein A 10 μg/ml (250 pmol/ml) 46 77 5 μg/ml (125 pmol/ml) 46 71 5 μg/ml (12.5 pmol/ml) 31 66______________________________________ *E/T ratio = effector to target cell ratio = 10:1 **Concentrations of pX1' are estimates.
TABLE 3______________________________________Effect of synthetic peptide, pX-2', on the NK- and LAK-likeactivities of PBL. Stimulation index* Short-term assay Long-term assay (NK-like activity) (LAK-like activity)Targets Raji Raji Daudi______________________________________E/T** ratio 10:1 10:1 20:1 10:1 20:1100 μg/ml 0.79 n.d.*** n.d. n.d. n.d. 25 μg/ml 1.15 1.41 1.48 1.15 1.07 6 μg/ml 1.23 1.02 1.12 1.05 1.031.5 μg/ml 0.97 0.94 0.97 1.00 0.99SpA 20 μg/ml 1.08 1.51 1.17 1.19 1.07______________________________________ *(activity of sample)/(activity of control) **E/T ratio = effector to target cell ratio ***not done
From table 2 it is seen that an estimated amount of 100 pmol/ml of material (calculated on the basis of pX-1') showed the same NK-cell stimulating activity as 125 to 250 pmol/ml of intact SpA using Daudi cells as targets, while its activity against Raji cells was somewhat lower.
From table 3 it is seen that pX-2' has an activity in all the tests that is equal to the activity of intact SpA.
Activation of Complement
In order to investigate the influence of the compounds of the invention on the complement system a test was performed in which the generation of the complement split product C5a was used as a measure of the activation of complement.
The test was performed by incubating normal human serum with SpA (Pharmacia Fine Chemicals Upsala, Sweden) or pX-2' for 60 minutes. Aliquots were taken after 0, 30, and 60 minutes and the generated C5a des-Arg was quantitated by a commercial RIA-kit (Upjohn Company, Kalamazoo, MI).
The results are shown in FIG. 4 and it is clearly seen that pX-2' is completely devoid of any activating effect, while SpA has a considerable C5a generating capacity, which dose-dependently increased the formation of C5a-des-Arg (the stable metabolite of C5a).
Guinea Pig Model
A further test was performed wherein the ability of peptides of the invention and SpA to induce an anaphylactoid-like reaction when administered intravenously into anaesthesized and artificially ventilated guinea pigs was investigated.
Guinea pigs of Dunkin-Hartley strain (ca. 500 g) were anaesthesized with sodium pentobarbital and were surgically prepared with a catheter in the jugular vein for drug infusion. The blood pressure was registered from a carotid artery. The animals were artificially ventilated by a Harvard small animal respirator at a cycle of 38 insufflations per min. and a volume of 1 ml per 100 g animal.
Protein A and pX-2' was administered intravenously, and it was found that protein A dose-dependently (10-100 μg/ml i.v.) produced an anaphylactoid-like reaction indicated by an initial bronchoconstriction and hypertension (later hypotension) subsequent to intravenous administration, while pX-2' did not induce any such reaction.
EXAMPLE 4
A preparation for parenteral administration, containing 1 mg of a peptide of formula I per ml, may be prepared as follows:
1 g of a peptide of formula I and 99 g of lactose are dissolved in 1 liter of distilled water and the pH is adjusted to about 7.0. The solution is sterile filtered. The sterile solution is filled in 10 ml vials in such a way that each vial contains 1.0 ml of the solution. The solutions are lyophilized and the vials are sealed under aseptic conditions.
The preparation in any single vial is to be dissolved in 1.0 ml of sterile, isotonic saline solution before administration.
EXAMPLE 5
Rectal suppositories are prepared by mixing 1 mg of a formula peptide with 4 g of cocoa butter. | Peptides of the formula R 1 -His-Asp-Glu-Ala-R wherein R 1 is Ala-Gln, and R is a polypeptide residue with up to 50 amino acid residues, and wherein one, more or all of the amino acid residues in R 1 and/or R independently may be omitted, can be used to augment cell mediated cytotoxicity and thereby to treat cancers and viral infections. These peptides may be prepared by proteolytic digestion of Staphylococcus aureus protein A, as well as by protein synthesis, recombinant DNA methods or any other methods known in the art. | 2 |
BACKGROUND OF THE INVENTION
Primary and secondary cells have a loss of capacity on storing because of a self-discharge and dissolution of the metal electrodes. Thus, more specifically, the shelf life of a cell employing a zinc anode, such as a Leclanche system, is limited by, among other factors, the open circuit corrosion of the zinc anode which causes dissolution of the metallic zinc and discharge of hydrogen gas.
To avoid the corrosion of the zinc, a variety of corrosion inhibitors have been added to the electrolyte. One of the oldest and most effective corrosion inhibition techniques involves the amalgamation of the zinc by mercury. While a pre-amalgamation treatment of the zinc may be carried out, it is more conventional to apply mercuric chloride to the zinc as a component of the electrolyte.
Flat or planar batteries of the general type disclosed, for example, in U.S. Pat. Nos. 3,563,805; 3,617,387; 3,734,780; and the like, comprise superposed planar anode/cathode combinations possessing a separator disposed intermediate each anode and cathode and electrolyte disposed on or impregnated in the separator and in contact with respective facing surfaces of the anode and cathode.
Planar batteries of the type disclosed in the aforementioned U.S. patents are generally intended to be employed as an individual power source for portable electrically operated devices wherein the selected device design parameters are optimized by the availability and employment of a planar battery exhibiting reliability with respect to its power delivery characteristics. Batteries of the type in question presently are employed commercially to operate the various electrically powered systems of the photographic camera sold by Polaroid Corporation, Cambridge, Mass., U.S.A., under the trademark "SX-70". In such cameras, the battery, disposed as a component of a film pack for employment in and in combination with the camera, provides the electrical energy necessary to operate the camera's exposure control, film transport and photoflash systems and, accordingly, such battery is required to operate in a sequential series of power generating modes which may or may not be interrupted by more or less extended recovery and/or storage times and under which conditions to deliver the required series of high current pulses dictated by the photographic system design.
Particular problems of amalgamation are presented with the above-described flat, planar batteries. Generally, powdered zinc is employed as the anode, which contains a relatively large amount, e.g., 5% or more, of zinc oxide and which presents a large surface area to the electrolyte. Amalgamation proceeds rapidly with the available zinc surfaces being protected by the interaction of the zinc with mercuric ions to form a zinc amalgam.
Subsequent to amalgamation and in contact with the electrolyte, the zinc oxide portion of the anode slowly dissolves providing fresh, unamalgamated zinc surfaces which result in increased hydrogen gas generation and attendant increase in impedence and general deterioration of the battery. Also, if less than full surface coverage by electrolyte occurs initially upon assembly subsequent redistribution of mercury-ion depleted electrolyte will also result in inadequately amalgamated zinc surfaces. The art has recognized that the effectiveness of amalgamation to inhibit corrosion is superior at room temperature but inadequate at elevated temperatures.
Copending application Ser. No. 50,354 filed June 26, 1970 now U.S. Pat. No. 3,945,849 is directed to the employment of quaternary ammonium halide as a corrosion inhibitor for zinc anodes. This inhibitor has been found to be more effective at elevated temperatures than at room temperature.
A novel corrosion inhibition system has now been found which is not susceptible to the deficiencies of the prior art.
SUMMARY OF THE INVENTION
The present invention is directed to a galvanic cell having a zinc anode having disposed in the electrolyte a chloride double salt containing both mercuric ion and a quaternary ion. The double salts suitable for employment in the present invention are represented by the formula:
M Hg.sub.x Cl.sub.y
wherein M is a quaternary cation, x is 1, 2 or 3, and y is 3 to 8.
The novel corrosion inhibitor of the present invention provides for a relatively continuous source of mercuric ion to the zinc as required to minimize corrosion of unamalgamated zinc as zinc oxide goes into solution and new zinc surfaces are exposed. The corrosion inhibitor also provides high temperature corrosion inhibition associated with the use of a quaternary halide as well as the room temperature effectiveness of mercury amalgamation.
BRIEF DESCRIPTION OF THE DRAWING
The FIGURE is a graphic representation showing the evolution of gas as a function of time from cells containing prior art inhibitors as compared with the novel double salt corrosion inhibitors of the present invention.
DETAILED DESCRIPTION OF THE INVENTION
The present invention is directed to the attenuation of corrosion of zinc anodes by providing to the electrolyte a double salt of a quaternary chloride and mercuric chloride which will provide a double corrosion inhibition system. As demanded by the zinc anode, the novel corrosion inhibitor of the present invention will provide mercury for amalgamation of zinc surfaces, especially newly exposed zinc surfaces resulting from the dissolution of zinc oxide in the electrolyte as well as a quaternary chloride which can provide room temperature corrosion inhibition and is particularly effective at elevated temperatures, e.g., 120° F.
The objects of the present invention are achieved by disposing in the electrolyte a double salt as described above. While not intending to be bound by the theory, it is believed that the mechanism may be represented as follows:
M Hg.sub.x Cl.sub.y ⃡ M.sup.+ + Hg.sub.x Cl.sub.y.sup.-(A)
hg.sub.x Cl.sub.y ⃡ X Hg.sup.++ + 3Cl.sup.- (B)
hg.sup.++ Zn ⃡ Hg + Zn.sup.+2
Hg + Zn → Hg Zn amalgam (C)
wherein M is a quaternary compound. Thus, the equilibrium reaction of the double salt provides a finite amount of Hg ++ ions. However, as the Hg ++ ions are reduced by the zinc, the reaction would shift toward the right providing a continuous supply of Hg ++ ions on demand as new zinc surfaces became available for amalgamation. Substantially contemporaneously, quaternary cations, as indicated in (A) above, become available to the zinc as a corrosion inhibitor.
The particular quaternary chloride employed to form the double salt of the present invention is not critical. It should be understood that the term "quaternary chloride" as used herein is intended to include both quaternary ammonium chloride and quaternized heterocyclic compounds. Suitable quaternary ammonium chlorides are those disclosed in copending application Ser. No. 50,354 filed June 26, 1970, particularly the tetraalkyl ammonium chlorides, such as tetraalkyl ammonium chloride and tetraethylammonium chloride. Suitable quaternary ammonium chlorides include the following:
[(CH.sub.3).sub.4 N]Cl (1)
[(C.sub.2 H.sub.5)N]Cl (2)
[(n-C.sub.4 H.sub.g).sub.4 N]Cl (3)
Suitable quaternized heterocyclic compounds include the following: ##STR1##
The double salts employed in the present invention are prepared by mixing aqueous solutions of the mercuric chloride and quaternary chloride and collecting the resulting precipitate. Generally, relatively dilute solutions are employed, e.g., about 5% solution. The two reactants are employed in the proportions desired in the double salt. The procedure for preparing such double salts is set forth in J. Chem. Soc., 1961, pages 3929-3935.
The following example illustrates the preparation of double salts within the scope of the present invention.
EXAMPLE I
A 5% solution of tetraethyl ammonium chloride and a 5% solution of mercuric chloride were mixed in a 1:1 ratio by weight. The thus-formed precipitate was separated and dried. The double salt (C 2 H 5 ) 4 NHg 2 Cl 5 was then analyzed.
______________________________________ % of Element C H N Cl______________________________________Calculated: 13.54 2.86 1.97 25.04Found: 13.46 2.88 1.94 22.64______________________________________
EXAMPLE II
Stoichiometric amounts of 5% aqueous solutions of N-benzyl-α-picolinium chloride and mercuric chloride were mixed and the resulting precipitate was separated. The double salt ##STR2## was then analyzed.
______________________________________ C H N Cl______________________________________Calculated: 31.72 2.91 2.97 20.00Found: 31.72 2.85 2.85 21.60______________________________________
The double salts may be disposed in the electrolyte in various concentrations. Such concentrations may range between 0.02% and 2.0% based on the weight of electrolyte.
The corrosion inhibition properties of various materials were ascertained by preparing an electrolyte comprising 68-69 cc. of water, 22 g. of ammonium chloride and 10 g. of zinc chloride. Various inhibitors, both the double salts of the present invention and prior art inhibitors, were added to the indicated electrolyte composition and then 50 mgs. of particulate zinc anode were immersed in 3 g. of the electrolyte mix, and the gas evolved over a period of time was measured as an indication of corrosion of the zinc. The FIGURE graphically represents the degree of corrosion resistance provided by the various inhibitors. The inhibitors and their concentration in the electrolyte are set forth in the following table:
A -- no inhibitor
B -- 200 mgs. [(CH 3 ) 4 N] Hg 2 Cl 5
C -- 200 mgs. [(C 2 H 5 ) 4 N] Hg 2 Cl 5
D -- 200 mgs. [CH 3 (C 4 H 9 ) 3 N] Cl
E -- 60 mgs. mercuric chloride
F -- 200 mgs. [(C 4 H 9 ) 4 N] Cl
From the FIGURE it can be seen that the corrosion inhibitors of the present invention are far superior to the mercuric chloride and some of the quaternary ammonium chloride compounds and even shows less gassing with one of the preferred quaternary ammonium chloride compounds, t-butyl ammonium chloride.
With regard to the above table, it should be noted that an excess amount of mercuric chloride necessary to amalgamate zinc was employed. Thus, the advantages achieved by employing the double salt cannot be attributed to the greater relative quantity of mercury employed. The art has found that excess mercury does not enhance corrosion inhibition.
The novel method of the present invention is particularly suitable for use with anodes prepared from zinc dust. Such anodes, which are widely used in flat, planar batteries as described above, are particularly susceptible to corrosion because of the large surface area and because of the relatively high amount of zinc oxide present. It will also be readily recognized that the present invention is particularly useful in batteries which may be stored for relatively long periods of time before use. Deterioration of the battery due to corrosion is reduced, thus enhancing the reliability of the stored batteries.
Batteries of the type disclosed in U.S. Pat. Nos. 3,563,805; 3,617,387; and 3,734,780 were prepared employing the double salts of the present invention as corrosion inhibitors. The electrical properties of the batteries were substantially the same or slightly better than control batteries (amalgamated zinc).
It should also be noted that the double salt corrosion inhibitors of the present invention can also be employed in conjunction with conventional stabilizers such as mercuric chloride, quaternary ammonium compounds and chromates. The employment of the double salts in conjunction with these inhibitors would serve to provide long-term and continuing protection to late exposed zinc surfaces and also serve to control the direction of the equilibrium of the above-indicated reactions as desired. | A galvanic cell having a zinc anode which contains in the electrolyte as a corrosion inhibitor a chloride double salt containing mercuric ions and quaternary ions. The corrosion inhibitor may be represented by the formula:
M Hg.sub.x Cl.sub.y
wherein M is a quaternary ammonium cation, x is 1, 2 or 3, and y is 3 to 8. | 7 |
CROSS REFERENCE TO RELATED APPLICATIONS
The application is a continuation-in-part of application Ser. No. 495,563, filed May 18, 1983, now U.S. Pat. No. 4,630,192. This application is distinguishable from application Ser. No. 495,563, in that the former claims an apparatus for rapidly processing a pair of vectors and storing the results of the processing whereas the latter claims an apparatus for executing an instruction and for simultaneously generating and storing related information.
BACKGROUND OF THE INVENTION
The present invention pertains to a computer system, and more particularly, to a parallel vector processor in said computer system for rapidly processing a pair of vectors and storing the results of said processing.
A typical vector processor, such as the vector processor shown in FIG. 1, includes a plurality of vector registers, each vector register storing a vector. The vector comprises a plurality of vector elements. A pipeline processing unit is connected to a selector associated with the vector registers for receiving corresponding elements of a first vector from a first vector register and utilizing the corresponding elements to perform an arithmetic operation on the corresponding elements of a second vector stored in a second vector register. The results of the arithmetic operation are stored in corresponding locations of one of the vector registers, or in corresponding locations of a third vector register.
However, with this configuration, it is necessary to perform operations on each of the corresponding elements of the vectors in sequence. If the vectors include 128 elements, 128 operations must be performed in sequence. The time required to complete operations on all 128 elements of the vector is a function of the cycle time per operation of the pipeline unit as is operates on each of the corresponding elements.
As a result of increasing sophistication of computer systems, there is a need to increase the performance of the vector processor portion of the computer system by decreasing the time required to process or perform arithmetic operations on each of the corresponding elements of a plurality of vectors stored in the vector registers within the computer system.
SUMMARY OF THE INVENTION
Accordingly, it is a primary object of the present invention to increase the performance of the vector processor portion of a computer system by decreasing the time required to process the corresponding elements of the vectors stored in a plurality of vector registers comprising said vector processor portion of the computer system.
It is a further object of the present invention to increase the performance of the vector processor portion of the computer system by subdividing the plurality of vector registers into a plurality of smaller registers, and processing each of the elements of the smaller registers in parallel with one another.
These and other objects are accomplished, in accordance with the present invention, by reducing the time required to complete processing operations on all elements of the vector. The vector registers are subdivided into a plurality of smaller registers, each of which store, for example, four elements of a 128 element vector. An element processor is associated with each smaller register, the element processor performing the same function as the pipeline processing unit. Each element processor, and corresponding smaller register, is connected in parallel fashion with respect to other element processors and their corresponding smaller registers. With this configuration, when an arithmetic operation is performed with respect to a first and second vector, the arithmetic operation, performed on all of the elements of the vector (for example, all 128 elements), is completed in the time required to complete an arithmetic operation on, in this example, four corresponding elements of the vectors. As a result, the performance of a vector processor is improved substantially as a result of a utilization of the concepts of the present invention.
Further scope of applicability of the present invention will become apparent from the text presented hereinafter. It should be understood, however, that the detailed description and the specific examples, while representing a preferred embodiment of the invention, are given by way of illustration only, since various changes and modifications within the spirit and scope of the invention would become obvious to one skilled in the art as a result of a reading of the following detailed description.
BRIEF DESCRIPTION OF THE DRAWINGS
A full understanding of the present invention will be obtained from a reading of the detailed description given hereinbelow and the accompanying drawings, which are given by way of illustration invention, and wherein:
FIG. 1 illustrates a conventional vector processor;
FIG. 2 illustrates the parallel vector processor of the present invention;
FIG. 3 illustrates the connection of the Processor Interface Adaptor to each of the element processors of FIG. 2;
FIG. 4 illustrates the construction of the Processor Interface Adaptor of FIGS. 2 and 3; and
FIG. 5 illustrates a detailed construction of an element processor shown in FIGS. 2 and 3.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
Referring to FIG. 1, a pipeline vector processor 10 is illustrated. In FIG. 1, a plurality of vector registers 12 (VR0 through VR15) are shown, each register storing 128 elements (element 0 through element 127). In the preferred embodiment, an element comprises a four (4) byte binary word. A selector 14 is connected to each of the vector registers 12 for selecting corresponding elements from the vector registers 12 and gating the selected elements through to a pipeline processing unit 16. The pipeline processing unit 16 is connected to the selector for receiving the corresponding elements and for performing selected operations on said elements, such as arithmetic operations. For example, the processing unit 16 may receive element 0 from vector register VR0 and corresponding element 0 from vector register VR15 and perform the following arithmetic operation on said elements: VR0+VR15→VR3. In this arithmetic operation, each of the binary bits of element 0 in VR0 is added to each of the binary bits of element 0 in VR15, and the resultant sum is stored in the element 0 position of vector register VR3. A result register 18 is connected to the pipeline processing unit for storing the resultant sum received from the pipeline processing unit. The result register 18 is connected to each of the vector registers 12 via a select gate 20 for transferring the resultant sum from the result register 18 to vector register VR3.
The configuration illustrated in FIG. 1 possesses certain disadvantages. Utilizing the example, a first element is selected from register VR0 and a corresponding element is selected from register VR15. The elements are added in the above manner. A second element is selected from registers VR0 and VR15 and are added together in the above manner. Each of the 128 elements must be selected from registers VR0 and VR15 and added together, in sequence, in order to complete the processing of the vectors stored in vector registers VR0 and VR15. As a result, the time required to complete the processing of the vectors stored in vector registers VR0 and VR15 is a function of the number of elements per vector and the cycle time required to process a set of corresponding elements per vector. The performance of a vector processor could be improved by decreasing the time required to process a pair of vectors stored in a set of vector registers.
Referring to FIG. 2, a parallel vector processor according to the present invention is illustrated. In FIG. 2, each of the vector registers VR0 through VR15 of FIG. 1 are subdivided into a plurality of smaller registers 12a, each smaller register 12a containing, for example, four elements. A corresponding plurality of element processors 20 are connected to the plurality of smaller registers 12a for performing processing (arithmetic) operations on the corresponding elements of the vectors stored in vector register VR0 through VR15, each of the element processors 20 performing processing operations on four corresponding elements of said vectors. The results of the processing operation are simultaneously produced by each element processor, in parallel, and may be stored in corresponding locations of any one of the vector registers VR0 through VR15. A processor interface adaptor (PIA) 22 is connected to each of the element processors 20 for transmitting address, data, and command information to each of the element processors. The actual connection of the PIA 22 to each of the element processors 0-31 is illustrated in FIG. 3 of the drawings. An instruction processing unit (IPU) 24 is connected to the PIA 22 for transmitting vector instructions to the PIA 22. A main memory or storage 26 is connected to the PIA 22 for transmitting the data information and address control information to the PIA in response to its request for such data.
Referring to FIG. 3, the actual connection of the PIA 22 to each of the element processors 20 (processor 0 through processor 31) is illustrated. The PIA 22 is connected to element processors 0, 8, 16, and 24. Element processor 0 is serially connected to element processors 1 through 7. Element processor 8 is serially connected to element processors 9 through 15. Element processor 16 is serially connected to element processors 17 through 23. Element processor 24 is serially connected to element processors 25 through 31.
Referring to FIG. 4, the construction of the PIA 22 is illustrated. The PIA 22 includes a vector instruction register (VIR) 22a connected to the IPU 24 for receiving a vector instruction from the IPU and temporarily storing the vector instruction. A vector data register (VDR) 22b is connected to storage 26 and to the IPU 24 for receiving data from storage 26 and temporarily storing the data. A vector status register (VSR) 22c is connected to the storage 26 and to IPU 24 for receiving address control information from storage and for temporarily storing the information. A pico control store 22d is connected to the VIR 22a for decoding the vector instruction stored in the VIR 22a and for selecting a pico control routine stored in the store 22d. A command register 22e is connected to the pico control store 22d and to the element processors via a command bus for driving the element processors. A bus control 22f is connected to the VDR 22b for receiving data from the VDR 22b and transmitting the data to the element processors 20 via a data bus. The bus control 22f can also steer data from one element processor to another element processor. The VSR 22c is also connected to a bus control 22g via an address control 22h. The address control 22h generates addresses corresponding to the data received from the VSR 22c. The bus control 22g transmits the generated addresses to the element processors 20 via an address bus.
The functional operation of the parallel vector processor of FIG. 2 will now be described with reference to FIGS. 2 through 4 of the drawings.
The IPU 24 instructs the PIA 22 to load specific data into vector registers VR0 and VR15. The IPU 24 transmits a LOAD instruction to the PIA 22. The LOAD instruction is temporarily stored in the VIR 22a. The DATA to be loaded into the vector registers VR0 and VR15 is stored in storage 26. When the PIA receives the LOAD instruction, it retrieves specific data from storage 26 and loads said data into the VDR 22b. Previous to the issuance of the LOAD instruction, the IPU 24 loaded address control information into the VSR 22c. As a result, specific address information is generated by the address control 22h. The address information comprises the address of selected element processors 20 into which the data is to be loaded and the address of selected elements associated with the selected element processors 20 into which the data is to be stored. The LOAD instruction, stored in the VIR 22a, is decoded by the pico control store 22d. Command information, corresponding to the LOAD instruction, stored in the pico control store 22d, is selected. In accordance with the address information generated by the address control 22h, the data stored in the VDR 22b is transmitted for storage in the selected processors 20 via the bus control 22f and a data bus. Furthermore, in accordance with the address information generated by the address control 22h, the command information stored in the pico control store 22d and selected by the decoded LOAD instruction, is transmitted to the selected processors 20 via command register 22e and a command bus. The selected command information causes the data stored in the selected processors to be loaded into the selected elements of the smaller registers 12a, the selected elements being identified by the address information generated by the address control 22h.
Accordingly, assume, by way of example, that a 128 element vector is stored in each of vector registers VR0 and VR15. An element comprises a four (4) byte binary word. Assume further that the following vector arithmetic operation is to be performed on the vectors stored in vector registers VR0 and VR15: VR0+VR15→VR15. The IPU 24 instructs the PIA 22 to perform an ADD operation wherein the vector stored in vector register VR0 is to be added to the vector stored in vector register VR15, the results to be stored in vector register VR15. The IPU 24 transmits this ADD instruction to the PIA 22. The ADD instruction is temporarily stored in the VIR 22a. In accordance with the ADD instruction, particular command information stored in the store 22d is selected. As the ADD instruction is received by the PIA 22, the IPU 24 retrieves specific data from storage 26 representative of the addresses of the elements in the smaller registers undergoing the ADD operation and the address of the selected processors 20 which will perform the ADD operation. As a result, address information is generated by the address control 22h. The address information is transmitted to the selected processors 20 via the bus control 22g and an address bus. In accordance with this address information, the selected command information, selected from the pico control store 22d, instructs the selected processors 20 to retrieve the selected elements of its associated smaller register 12a corresponding to vector registers VR0 and VR15. When the elements are retrieved, the selected command information causes the selected processors 20 to execute the ADD instruction. For example, elements 0 through 3, associated with the vectors stored in vector registers VR0 and VR15, are received by element processor number 0. Element processor 0 adds the corresponding elements together, and, in accordance with the selected command information, stores the results of the addition operation in the corresponding locations of vector register VR15. That is, element 0 of vector register VR0 is added to element 0 of vector register VR15, and the sum is stored in the element 0 location of vector register VR15. Elements 1, 2, and 3 of vector registers VR0 and VR15 are similarly added together, the sums being stored in the element 1, 2, and 3 locations of vector register VR15. Elements 4, 5, 6, and 7, associated with vector registers VR0 and VR15, are processed by element processor 1, in the same manner as described above, the processing of these elements being performed simultaneously with the processing of elements 0, 1, 2, and 3. The remaining elements of the vectors, stored in vector registers VR0 and VR15, are processed by element processors 2 through 31, in groups of four elements each, simultaneously with the processing of elements 0 through 3 and elements 4 through 7 by element processors 0 and 1 respectively. As a result, the above referenced vector arithmetic operation, performed on the vectors stored in vector registers VR0 and VR15, is completed in the time required to process four elements of the vector, as compared to the time required to process 128 elements of the vector, typical of the conventional vector processor systems. Therefore, the parallel vector processor of the present invention represents an improvement over the conventional vector processor systems.
Referring to FIG. 5, a block diagram construction of an element processor 20 is illustrated. In FIG. 5, a local storage 12 is analogous to the vector registers 12 shown in FIG. 19 2 of the drawings. A system bus 11 and 11a is connected to a driver circuit 9 on one end and to a receiver circuit 7 on the other end. A first input data assembler (ASM) 13 is connected to a driver circuit 9 and to a receiver circuit 7. The ASM 13 is further connected to local storage 12 and to the element processor 20. The element processor 20 shown in FIG. 5 comprises a second input data assembler (ASM) 20a connected to the local storage 12 and to the first input data assembler 13. A Bus Interface Register (BIR) 15 is connected to bus 11 and bus 11a, on one end, and to the second input data assembler (ASM) 20a on the other end. A shift select register 20b and a flush select register 20c are connected to the input data assembler 20a. The flush select register 20c is connected directly to a trues/complement gate 20d whereas the shift select register 20b is connected to another trues/complement gates 36 via a pre-shifter control 20f. The trues/complements gates 20d and 20e are each connected to an operation means, such as an arithmetic logic unit (ALU) 20g. The ALU 20g is connected to a result register 20h via a post shifter control 20i, the result register 20h being connected to the local storage 12 for storing a result therein when the element processor 20 has completed an arithmetic processing operation on the four elements of a pair of vectors stored in a corresponding pair of vector registers 12. A multiplier circuit 20j is interconnected between the input data assembler 20a and the ALU 20g. Two operands are received by the multiplier circuit 20j. A sum output and a carry output is generated by the multiplier circuit 20j, the sum and carry outputs being received by the ALU 20g.
A description of the functional operation of an element processor 20 will be provided in the following paragraphs with reference to FIG. 5 of the drawings.
The functional operation of the element processor 20 shown in FIG. 5 may be subdivided into four cycles of operation: a read local storage and shift select cycle, alternatively known as a first cycle; a pre-normalize shift cycle, known as a second cycle; an ALU operation cycle, known as a third cycle; and a post-normalize shift cycle, known as a fourth cycle.
Utilizing the assumptions made previously, wherein the respective elements of vector registers VR0 and VR15 are added together and the results of the summation operation are stored in vector register VR0, elements 0 through 3 are received by receiver 7 of bus 11a and stored in local storage 12 via ASM 13, the local storage 12 being analogous to the first smaller register 12a shown in FIG. 2 which stores elements 0 through 3. Assume further that the elements 0 through 3 represent floating point element operands.
When a command is issued to add elements 0-3 stored in register VR0 to elements 0-3 stored in register VR15, on the first cycle, the operands of the respective elements are read from the local storage 12 and are temporarily stored in the flush register 20c and the shift register 20b via the input data assembler 20a. However, at the same time, the exponents of the respective elements enter an exponent control path (not shown) where the difference in magnitude of the exponents is calculated. Therefore, the element having the smaller exponent is gated to the shift select register 20b whereas the element having the greater exponent is gated to the flush select register 20c. The flush and shift select registers 20c and 20b are latched by a latch clock at the end of the first cycle.
At the beginning of the second cycle, a shift operation is started. The element having the greater exponent, stored in the flush select register 20c, is gated into one input of the arithmetic logic unit (ALU) 20g. Shift control information is passed from the exponent control path (not shown) to the pre-shifter 20f wherein the shift select register 20b, is right-shifted by the pre-shifter 20f to align said element with the element having the greater exponent, which is currently being gated into the one input of the ALU 20g. Concurrently, the ALU 20g is selecting the appropriate inputs from the trues/complement gates 20d and 20e for receiving the elements from the flush and shift select registers 20c and 20b via the trues/complement gates 20d and 20e, respectively.
The third cycle, in the operation of the element processor 20 of FIG. 5, is dedicated to the functional operation of the arithmetic logic unit (ALU) 20g. The ALU is an 8-byte high speed carry look ahead adder, designed with 1's complement arithmetic and with end around carry and recomplementation. The ALU performs an addition operation, wherein the bits of four respective elements, in the example, elements 0 through 3 stored in one of the smaller registers 12a, associated with vector register VR0, are added to the bits of four respective elements, associated with vector register VR15. The results of the addition operation are ultimately stored in the local storage 12 (in the example, analogous to the vector register VR0 illustrated in FIG. 2). However, prior to this step, a post-normalization step must take place during the fourth cycle.
When the addition operation is completed by the ALU 20g, a post-normalization step takes place during the fourth cycle. The term "post-normalization", in data processing terms, comprises the steps of detecting leading zero hexadecimal digits in the results produced by the ALU, and left shifting the results in accordance with the number of zero digits detected. The results exponent must be adjusted by decrementing the exponent by a value of 1 for each digit shifted. Digits of the output of the ALU 20g are examined by the post shifter 20i for their zero state, and the results of the ALU output are left shifted in accordance with the number of zero digits detected. The left shifted results of the ALU output are passed to the result register 20h for temporary storage therein. The exponent control path (not shown) increments or decrements the exponent value of the result element (output from the ALU) so that a correct final exponent value is gated to the result register 20h. As a result, a result element is stored in the result register 20h, the operand of which is left shifted a proper amount in accordance with the number of zero digits detected in the ALU output, the exponent of which is the correct final exponent value. During the next cycle, following the fourth cycle, the result element is passed to the local storage 12 for storage therein (the local storage being analogous to one of the smaller registers 12a of FIG. 2, in the example, the smaller register 12a which stores elements 0 through 3).
Therefore, the performance of a vector processor is improved by virtue of the utilization of the concepts of the present invention. Although an increased number of circuits is necessary to implement the present invention, this increased number of circuits is economically justifiable as a result of the utilization of very large scale integrated circuit (VLSI) technology.
The invention being thus described, it will be obvious that the same may be varied in many ways. Such variations are not to be regarded as a departure from the spirit and scope of the invention, and all such modifications as would be obvious to one skilled in the art are intended to be included within the scope of the following claims. | A pipelined parallel vector processor is disclosed. In order to increase the performance of the parallel vector processor, the present invention decreases the time required to process a pair of vectors stored in a pair of vector registers. The vector registers are subdivided into a plurality of smaller registers. A vector, stored in a vector register, comprises N elements; however, each of the smaller registers store M elements of the vector, where M is less than N. An element processor, functioning in a pipeline mode, is associated with each smaller register for processing the M elements of the vectors stored in the smaller register and generating results of the processing, the results being stored in one of the vector registers. The smaller registers of the vector registers, and their corresponding element processors, are structurally configured in a parallel fashion. The element processors and their associated smaller registers operate simultaneously. Consequently, processing of the N element vectors, stored in the vector registers, is complete in the time required to complete the processing of the M elements of the N element vector. | 6 |
RELATED APPLICATION
The present application is a non-provisional application claiming priority to U.S. Provisional Application No. 60/548,635, filed 27 Feb. 2004.
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates generally to the field of chemical analysis. More particularly, it concerns tag reagents for sensitive, high throughput detection and analysis of target molecules.
2. Description of the Related Art
Chemical labels, otherwise known as tags or signal groups, are widely used in chemical analysis. Among the types of molecules used are radioactive atoms, fluorescent reagents, luminescent reagents, metal-containing compounds, electron-absorbing substances and light absorbing compounds. A number of different types of molecules have been used as tags that can be differentiated under mass spectrometry. Chemical signal groups can be combined with reactivity groups so that they might be covalently attached to the target, the substance being detected.
However, current detection probes do not adequately allow highly multiplex detection and analysis of molecules. Microarrays can analyze the expression profiles of thousands of genes, but researchers can typically handle only one or two samples on a single microarray chip or slide because their fluorescent or luminescent detection systems have very limited multiplex capability. In addition to the added costs caused by the necessary use of multiple chips or slides, the limited analytical capacity of existing methods makes it difficult to replicate microarray experiments and/or compare data among samples. Moreover, while many other applications and assays have been developed using microplate formats, the use of current multiplex methods and devices limit the number of the samples that can be used in each well. Using current methods and devices of multiplex analysis of molecules requires multiple wells and/or plates for higher throughput and reproducible data.
SUMMARY OF THE INVENTION
Embodiments of the present invention provide compositions and methods relating to the use of release tag compounds for detection and analysis of target molecules, which increase signal intensity of molecular probes and allows for sensitive, high-throughput multiplex analysis. Liposome embodiments preferably contain a plurality of mass tag molecules, ranging in number from 1 to 2×10 8 , which provides stronger signaling and allows for highly sensitive multiplex analysis of molecules. Other embodiments can contain many orders of magnitude more mass tag molecules. For example, a solid particle having a diameter of 0.5 μm can contain up to 2×10 10 mass tag molecules. Still other embodiments can contain even more mass tag molecules, depending the size of the embodiments and the density of the mass tag molecules, but ordinarily there are less than 1×10 20 , and more preferably less than 1×10 15 molecules.
Preferred embodiments comprise detection probes utilizing vesicles to retain multiple mass tag molecules, which are molecules with a specific molecular mass (or mobility) detectable by mass spectrometry, electrophoresis, chromatography or other analytical methods known to those skilled in the art. As used herein, a “vesicle” may include molecules encapsulated within the vesicle. Embodiments include, but are not limited to, encapsulation vesicles, uni-lamellar vesicles, and multi-lamellar vesicles. The various vesicles preferably comprise liposomes, which preferably comprise a plurality of phospholipids. In certain embodiments, the mass tag molecules can be attached to the phospholipids themselves. Other molecules, such as cholesterol or other hydrophobic molecules, also can be entrapped in the lipid bilayer through hydrophobic interaction as mass tag molecules.
Further embodiments of the present invention comprise various carriers of mass tag molecules, including, but not limited to: emulsions, soluble beads, soluble capsules, and soluble porous beads.
Embodiments of the present invention can be used with various analytical methods and systems, including, but not limited to: hybridization assays, multiplex microarray assays, multiplex immunoassays, multiplex hybridization assays, multiplex CpG methylation assays, capillary assays, mass spectrometry, electrophoresis, and other analytical methods and systems known to those skilled in the art.
One embodiment of the present invention is a detection probe comprising an external vesicle comprising a plurality of amphiphilic molecules forming a vesicle membrane; a plurality of mass tag molecules encapsulated within the vesicle, within the vesicle membrane or adsorbed on the vesicle membrane; and a probe attached to the vesicle. In further embodiments, the external vesicle is easily disrupted to release the mass tag molecules, the plurality of mass tag molecules comprise at least a part of the vesicle membrane. Further embodiments additionally comprise at least one vesicle encapsulated within the external vesicle, at least a part of the external and encapsulated vesicles comprising the mass tag molecules, and in a further embodiment thereof, the external and encapsulated vesicles are easily disrupted to release the mass tag molecule. In further embodiments, the external vesicle is a liposome, a polymersome, or an emulsion such as an oil-in-water (O/W) emulsion, water-in-oil-in-water (W/O/W) emulsion or solid-in-oil-in-water (S/O/W) emulsion. In a further embodiment, the probe comprises at least one molecule selected from the group consisting of chemical residues, polynucleotides, polypeptides, and carbohydrates, and the molecule may be immobilized. In further embodiments, the mass tag molecules are a biopolymer such as a polynucleotide, polypeptide or polysaccharide; a synthetic polymer such as a block copolymer; amphiphilic molecules bound to a biopolymer such as a polynucleotide, polypeptide, polysaccharide or a synthetic polymer such as a block copolymer.
Another embodiment of the invention is a detection probe, comprising a body comprising a material that can become soluble upon physical or chemical stimulation and at least one mass tag molecule, and a probe attached to the body. In further embodiments, the body may comprise a soluble bead which may be porous, or a soluble capsule. In further embodiments, the probe comprises at least one molecule selected from the group consisting of chemical residues, polynucleotides, polypeptides, and carbohydrates, and the molecule may be immobilized. In further embodiments, the mass tag molecule may be a biopolymer or a synthetic polymer.
Another embodiment of the present invention is a set of detection probes comprising: a first detection probe comprising a first body comprising a material that can become soluble upon physical or chemical stimulation and at least one first mass tag molecule, and a first probe attached to the first body; and a second detection probe comprising a second body comprising a material that can become soluble upon physical or chemical stimulation and at least one second mass tag molecule, and a second probe attached to the second body; wherein the mass of the first mass tag molecule is different from the mass of the second mass tag molecule. In further embodiments, the first and second bodies comprise soluble beads, which may be porous, or soluble capsules. In further embodiments, the first and second probes comprise at least one molecule selected from the group consisting of chemical residues, polynucleotides, polypeptides, and carbohydrates, and the molecule may be immobilized. In further embodiments, the first and second mass tag molecules are biopolymers, such as polynucleotides, polypeptides or polysaccharides, synthetic polymers, such as block copolymers, amphiphilic molecules bound to a biopolymer or synthetic polymer, or amphiphilic molecules bound to a polynucleotide, polypeptide, polysaccharide or block copolymer.
Another embodiment of the present invention is a method of simultaneously assaying a plurality of different biological samples, each of said samples comprising a plurality of analytes, the method comprising: immobilizing said analytes from each of said samples on a surface; incubating said surface with the set of detection probes described above; removing unbound detection probe; collecting the first and second mass tag molecules from the bound detection probe; and quantifying the first and second mass tag molecules collected. In further embodiments, the binding of the first and second detection probe results from the binding of molecules such as DNA, RNA, aptamers, proteins, peptides, polysaccharides, chemical residues on a biological molecule, or a small chemical molecule, or from the binding of complementary nucleotide sequences, antigen-antibody binding, protein-protein binding, or the binding of a chemical residue and a biological molecule. In further embodiments, the mass tag molecules are collected after stimulation of the first and second detection probes by a solvent change, chemical addition, pH change, agitation, sonication, heating, laser irradiation, light irradiation or freeze-thaw process. In a further embodiment the mass tag molecules may be quantified by mass spectrometry, electrophoresis or chromatography.
Another embodiment of the present invention is a method of analyzing a plurality of different biological samples, each of said samples comprising a plurality of analytes, said method comprising: labeling each sample with a detection probe comprising a body comprising a material that can become soluble upon physical or chemical stimulation and at least one mass tag molecule, and a probe attached to the body, wherein the mass tag molecule of the detection probe labeling each sample has a different mass; incubating the labeled sample with an immobilized target molecule capable of specifically binding to one of said analytes; removing unbound labeled sample; collecting the mass tag molecules from the bound probe; and quantifying the mass tag molecules collected. In further embodiments, the binding of the detection probe results from the binding of molecules such as DNA, RNA, aptamers, proteins, peptides, polysaccharides, chemical residues on biological molecules, or small chemical molecules, or from the binding of complementary nucleotide sequences, antigen-antibody binding, protein-protein binding, or binding of a chemical residue and a biological molecule. In further embodiments, the mass tag molecules are collected after stimulation of the detection probes.
Another embodiment of the present invention is set of detection probes comprising: a first detection probe comprising a first external vesicle comprising a plurality of amphiphilic molecules forming a first vesicle membrane, a plurality of first mass tag molecules encapsulated within the first external vesicle, within the first vesicle membrane or adsorbed on the first vesicle membrane, and a probe attached to the first external vesicle; and a second detection probe comprising a second external vesicle comprising a plurality of amphiphilic molecules forming a second vesicle membrane, a plurality of second mass tag molecules encapsulated within the second external vesicle, within the second vesicle membrane or adsorbed on the second vesicle membrane, and a probe attached to the second external vesicle; wherein the mass of the first mass tag molecules is different from the mass of the second mass tag molecules. In further embodiments, the first and second external vesicles are easily disrupted to release the mass tag molecules. In further embodiments, each of the first and second mass tag molecules is encapsulated within each of the first and second external vesicles, or within each of the first and second vesicle membranes, or is adsorbed on each of the first and second vesicle membranes, respectively. In further embodiments, the mass tag molecules comprise at least a part of the vesicle membranes. In further embodiments, each of the first and second external vesicles further comprise at least one encapsulated vesicle, at least a part of the external and encapsulated vesicles comprising the mass tag molecule, and the external and encapsulated vesicles may be easily disrupted to release the mass tag molecules. In further embodiments, the external vesicles are liposomes, polymerosomes, or emulsions such as oil-in-water (O/W) emulsions, water-in-oil-in-water (W/O/W) emulsions or solid-in-oil-in-water (S/O/W) emulsions. In further embodiments, the probes each comprise at least one molecule selected from the group consisting of chemical residues, polynucleotides, polypeptides, and carbohydrates, and the molecule may be immobilized. In further embodiments, the first and second mass tag molecules may be biopolymers such as polynucleotides, polypeptides or polysaccharides, synthetic polymers such as block copolymers, amphiphilic molecules bound to a biopolymer such as a a polynucleotide, polypeptide, or polysaccharide, or a synthetic polymer such as a block copolymer.
Another embodiment of the present invention is a method of simultaneously assaying a plurality of different biological samples, each of said samples comprising a plurality of analytes, said method comprising: immobilizing said analytes from each of said samples on a surface; incubating said surface with a set of detection probes comprising: a first detection probe comprising a first external vesicle comprising a plurality of amphiphilic molecules forming a first vesicle membrane, a plurality of first mass tag molecules encapsulated within the first external vesicle, within the first vesicle membrane or adsorbed on the first vesicle membrane, and a probe attached to the first external vesicle; and a second detection probe comprising a second external vesicle comprising a plurality of amphiphilic molecules forming a second vesicle membrane, a plurality of second mass tag molecules encapsulated within the second external vesicle, within the second vesicle membrane or adsorbed on the second vesicle membrane, and a probe attached to the second external vesicle; wherein the mass of the first mass tag molecules is different from the mass of the second mass tag molecules; removing unbound detection probe; collecting the first and second mass tag molecules from the bound detection probe; and quantifying the first and second mass tag molecules collected. In further embodiments, the binding of the detection probe results from the binding of molecules such as DNA, RNA, aptamers, proteins, peptides, polysaccharides, chemical residues on biological molecules, or small chemical molecules, or from the binding of complementary nucleotide sequences, antigen-antibody binding, protein-protein binding, or binding of chemical residues and biological molecules. In further embodiments, the mass tag molecules are collected after stimulation of the detection probes by a solvent change, chemical addition, pH change, agitation, sonication, heating, laser irradiation, light irradiation or freeze-thaw process. In further embodiments, the mass tag molecules are quantified by mass spectrometry, electrophoresis or chromatography.
Another embodiment of the present invention is a method of analyzing a plurality of different biological samples, each of said samples comprising a plurality of analytes, said method comprising: labeling each sample with a detection probe comprising an external vesicle comprising a plurality of amphiphilic molecules forming a vesicle membrane, a plurality of mass tag molecules encapsulated within the vesicle, within the vesicle membrane or adsorbed on the vesicle membrane, and a probe attached to the vesicle, wherein the mass tag molecules of the detection probe labeling each sample have a different mass; incubating the labeled sample with an immobilized target molecule capable of specifically binding to one of said analytes; removing unbound labeled sample; collecting the mass tag molecules from the bound probe; and quantifying the mass tag molecules collected. In further embodiments, the binding of the detection probe results from the binding of molecules such as DNA, RNA, aptamers, proteins, peptides, polysaccharides, chemical residues on biological molecules, or small chemical molecules, or the binding of complementary nucleotide sequences, antigen-antibody binding, protein-protein binding, or the binding of chemical residues and biological molecules. In further embodiments, the mass tag molecules are collected after stimulation of the detection probes by a solvent change, chemical addition, pH change, agitation, sonication, heating, laser irradiation, light irradiation or freeze-thaw process. In further embodiments, the mass tag molecules are quantified by mass spectrometry, electrophoresis or chromatography.
Another embodiment of the present invention is a method of simultaneously assaying a plurality of different biological samples, each of said samples comprising a plurality of analytes, said method comprising: immobilizing said analytes from each of said samples on a surface; incubating said surface with a set of detection probes comprising: a first detection probe comprising a first external vesicle comprising a plurality of first mass tag molecules forming a first vesicle membrane, and a probe attached to the first external vesicle; and a second detection probe comprising a second external vesicle comprising a plurality of second mass tag molecules forming a second vesicle membrane, and a probe attached to the second external vesicle; removing unbound detection probe; collecting the first and second mass tag molecules from the bound detection probe; and quantifying the first and second mass tag molecules collected. In further embodiments, the binding of the detection probe results from the binding of molecules such as DNA, RNA, aptamers, proteins, peptides, polysaccharides, chemical residues on biological molecules, or small chemical molecules, or the binding of complementary nucleotide sequences, antigen-antibody binding, protein-protein binding, or the binding of chemical residues and biological molecules. In further embodiments, the mass tag molecules are collected after stimulation of the detection probes by a solvent change, chemical addition, pH change, agitation, sonication, heating, laser irradiation, light irradiation or freeze-thaw process. In further embodiments, the mass tag molecules are quantified by mass spectrometry, electrophoresis or chromatography.
Another embodiment of the present invention is a method of analyzing a plurality of different biological samples, each of said samples comprising a plurality of analytes, said method comprising: labeling each sample with a detection probe comprising an external vesicle comprising a plurality of mass tag molecules forming a vesicle membrane and a probe attached to the vesicle, wherein the mass tag molecules of the detection probe labeling each sample have a different mass; incubating the labeled sample with an immobilized target molecule capable of specifically binding to one of said analytes; removing unbound labeled sample; collecting the mass tag molecules from the bound probe; and quantifying the mass tag molecules collected. In further embodiments, the binding of the detection probe results from the binding of molecules such as DNA, RNA, aptamers, proteins, peptides, polysaccharides, chemical residues on biological molecules, or small chemical molecules, or from the binding of complementary nucleotide sequences, antigen-antibody binding, protein-protein binding, or the binding of chemical residues and biological molecules. In further embodiments, the mass tag molecules are collected after stimulation of the detection probes by a solvent change, chemical addition, pH change, agitation, sonication, heating, laser irradiation, light irradiation or freeze-thaw process. In further embodiments, the mass tag molecules are quantified by mass spectrometry, electrophoresis or chromatography.
BRIEF DESCRIPTION OF THE DRAWINGS
FIGS. 1A-1C are schematic representations of various types of mass tag-containing vesicles.
FIG. 2 is a graph showing hybridization assay results for various vesicle types.
FIG. 3 is a schematic depiction of a multiplex microarray process with mass tag molecules.
FIG. 4 is a schematic depiction of a multiplex immunoassay with mass tag molecules.
FIG. 5 is a schematic depiction of a multiplex hybridization with mass tag molecules.
FIG. 6 is a schematic depiction of a capillary assay with mass tag molecules.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
Embodiments of the present invention comprise detection probes utilizing various forms of vesicles to retain multiple mass tag molecules. Mass tag molecules are disclosed in U.S. Pat. No. 6,635,452, which is hereby incorporated in its entirety by reference. Mass tag molecules may also be referred to as labels or signals. Examples of the types of mass tag molecules used in the present invention include a repertoire of compounds, preferably ones that share similar mass spectrometric desorption properties and have similar or identical coupling chemistries in order to streamline synthesis of multiple mass label variants. A mass tag molecule of the present invention is detectable by mass spectrometry. Representative types of mass spectrometric techniques include matrix-assisted laser desorption ionization, direct laser-desorption, electrospray ionization, secondary neutral, and secondary ion mass spectrometry, with laser-desorption ionization being preferred. The dynamic range of mass spectral measurements can generally be extended by use of a logarithmic amplifier and/or variable attenuation in the processing and analysis of the signal.
Mass tag molecules may include a vast array of different types of compounds including biopolymers and synthetic polymers. Representative biological monomer units that may be used as mass tag molecules, either singly or in polymeric form, include amino acids, nonnatural amino acids, nucleic acids, saccharides, carbohydrates, peptide mimics and nucleic acid mimics. Preferred amino acids include those with simple aliphatic side chains (e.g., glycine, alanine, valine, leucine and isoleucine), amino acids with aromatic side chains (e.g., phenylalanine, tryptophan, tyrosine, and histidine), amino acids with oxygen and sulfur containing side chains (e.g., serine, threonine, methionine and cysteine), amino acids with side chains containing carboxylic or amide groups (e.g., aspartic acid, glutamic acid, asparagine and glutamine), and amino acids with side chains containing strongly basic groups (e.g., lysine and arginine), and proline. Derivatives of the above described amino acids are also contemplated as monomer units. An amino acid derivative as used herein is any compound that contains within its structure the basic amino acid core of an amino-substituted carboxylic acid, with representative examples including but not limited to azaserine, fluoroalanine, GABA, ornithine, norleucine and cycloserine. Peptides derived from the above described amino acids can also be used as monomer units. Representative examples include both naturally occurring and synthetic peptides with molecular weight above about 500 Daltons, with peptides from about 500-5000 Daltons being preferred. Representative examples of saccharides include ribose, arabinose, xylose, glucose, galactose and other sugar derivatives composed of chains from 2-7 carbons. Representative polysaccharides include combinations of the saccharide units listed above linked via a glycosidic bond. The sequence of the polymeric units within any one mass tag molecule is not critical; the total mass is the key feature of the tag molecules.
The monomer units according to the present invention also may be composed of nucleobase compounds. As used herein, the term nucleobase refers to any moiety that includes within its structure a purine, a pyrimidine, a nucleic acid, nucleoside, nucleotide or derivative of any of these, such as a protected nucleobase, purine analog, pyrimidine analog, folinic acid analog, methyl phosphonate derivatives, phosphotriester derivatives, borano phosphate derivatives or phosphorothioate derivatives.
Mass tag molecules according to the present invention may also include any organic or inorganic polymer that has a defined mass value, remains water soluble during bioassays and is detectable by mass spectrometry. Representative synthetic monomer units that may be used as mass units in polymeric form include polyethylene glycols, polyvinyl phenols, polymethyl methacrylates, polypropylene glycol, polypyroles, and derivatives thereof. A wide variety of polymers would be readily available to one of skill in the art based on references such as Allcock (Contemporary Polymer Chemistry, Prentice-Hall, Inc., Englewood Cliffs, N.J., 1981), which describes the properties of many additional polymers contemplated for use in the present invention. The polymers may be composed of a single type of monomer unit or combinations of monomer units to create a mixed polymer. The sequence of the polymeric units within any one mass tag molecule is not critical; the total mass is the key feature of the tag molecule.
For nonvolatile mass tag molecules having a mass below about 500 Da, usually significant ionic character is required; representative examples include polyethylene glycol oligomers of quaternary ammonium salts (e.g., R—(O—CH 2 —CH 2 ) n —N(CH 3 ) 3 + Cl − ) and polyethylene glycol oligomers of carboxylic acids and salts (e.g., R—(O—CH 2 —CH 2 ) n —CO 2 —Na + ).
Examples of involatile mass tag molecules typically include small oligomers of polyethylene glycol and small peptides (natural or modified) less than about 500 Da in molecular weight. In these instances, as for all of the cases considered herein, mass analysis is not by electron attachment.
Mass tag molecules of the present invention may also include a variety of nonvolatile and involatile organic compounds which are nonpolymeric. Representative examples of nonvolatile organic compounds include heme groups, dyes, organometallic compounds, steroids, fullerenes, retinoids, carotenoids and polyaromatic hydrocarbons.
Mass tag molecules of the present invention comprise molecules with a specific molecular mass or mobility detectable by various analytical methods and systems including, but not limited to: hybridization assays, multiplex microarray assays, multiplex immunoassays, multiplex hybridization assays, multiplex CpG methylation assays, capillary assays, mass spectrometry, electrophoresis, and other analytical methods known to those skilled in the art.
The embodiment illustrated in FIG. 1A shows a number of detection probes 20 comprising an encapsulation vesicle 22 having at least one mass tag molecule 24 preferably located within the vesicle 22 . The vesicle preferably comprises at least one interaction site 26 on its surface. In each probe, the vesicle encapsulates at least one mass tag molecule 24 with a specific molecular mass.
The embodiment illustrated in FIG. 1B shows a detection probe 30 comprising a uni-lamellar vesicle 32 . The membrane 38 of the vesicle 32 preferably comprises mass tag molecules 34 with a specific molecular mass. Further embodiments of the uni-lamellar vesicles 32 comprise at least one mass tag molecule 34 preferably located within the uni-lamellar vesicle 32 . The mass tags 34 located within the vesicle 32 are preferably the same type of mass tags 34 as those comprising the membrane 38 . The vesicle preferably comprises at least one interaction site 36 on its surface.
FIG. 1C shows another preferred embodiment of the present invention which comprises a detection probe 40 , further comprising a multi-lamellar vesicle 42 . The membrane 48 of the vesicle preferably comprises mass tag molecules 44 with a specific molecular mass. Further embodiments of the multi-lamellar vesicles 42 comprise at least one mass tag molecule 44 preferably located within the multi-lamellar vesicle 42 . The vesicle 42 preferably encapsulates at least one smaller vesicle 49 which preferably contains the same type of mass tags 44 as those comprising the membrane 48 . The mass tags 44 located within the vesicle 42 are preferably the same type of mass tags 44 as those comprising the membrane 48 . The vesicle 42 preferably comprises at least one interaction site 46 on its surface.
Embodiments of the detection probes 20 , 30 , and 40 of FIGS. 1A-1C utilize vesicles comprising liposomes, which can carry and release mass tag molecules. In order to release the mass tag molecules for detection, these carriers are preferably easily disrupted by physical stimulation, including but not limited to: heat, centrifugation, laser irradiation, sonication, electricity, evaporation, freeze-thaw process, or other methods known to those skilled in the art. Disruption may also be preferably achieved by chemical stimulation including, but not limited to: addition of organic solvent, detergent, acid, alkaline, enzyme, chaotropic reagents (urea, guanidium chloride, etc.), change of buffer, change of salt, change of concentration, change of pH, change of osmotic pressure, and other methods known to those skilled in the art.
In preferred embodiments, the probes 20 , 30 , and 40 have interaction sites 26 , 36 , and 46 on their outer surface comprising chemical residues, polynucleotides, proteins, peptides, carbohydrate or other small compounds known to those skilled of the art. In preferred embodiments, the molecules of the interaction sites 26 , 36 , and 46 are immobilized. The interaction sites 26 , 36 , and 46 of the probes 20 , 30 , and 40 can preferably be used to analyze various intermolecular interactions such as nucleotide-nucleotide interactions (hybridization), antigen-antibody interactions (immunoassay), protein-protein interactions, small compound-protein interactions, small compound-cell interactions, and other interactions known to those skilled in the art.
As defined herein, the term “interaction site” refers to a group capable of reacting with the molecule whose presence is to be detected. For example, the interaction site may be a biomolecule capable of specific molecular recognition. Biomolecules capable of specific molecular recognition may typically be any molecule capable of specific binding interactions with unique molecules or classes of molecules, such as peptides, proteins, polynucleic acids, carbohydrate, and other chemical molecules, etc.
Thus, interaction sites disclosed herein for use with the disclosed methods encompass polypeptides and polynucleic acids. As used herein, polypeptides refer to molecules containing more than one amino acid (which include native and non-native amino acid monomers). Thus, polypeptides includes peptides comprising 2 or more amino acids; native proteins; enzymes; gene products; antibodies; protein conjugates; mutant or polymorphic polypeptides; post-translationally modified proteins; genetically engineered gene products including products of chemical synthesis, in vitro translation, cell-based expression systems, including fast evolution systems involving vector shuffling, random or directed mutagenesis, and peptide sequence randomization. In preferred embodiments polypeptides may be oligopeptides, antibodies, enzymes, receptors, regulatory proteins, nucleic acid-binding proteins, honnones, or protein product of a display method, such as a phage display method or a bacterial display method. More preferred polypeptide interaction sites are antibodies and enzymes. As used herein, the phrase “product of a display method” refers to any polypeptide resulting from the performance of a display method which are well known in the art. It is contemplated that any display method known in the art may be used to produce the polypeptides for use in conjunction with the present invention.
Similarly, “polynucleic acids” refer to molecules containing more than one nucleic acid. Polynucleic acids include lengths of 2 or more nucleotide monomers and encompass nucleic acids, oligonucleotides, oligos, polynucleotides, DNA, genomic DNA, mitochondrial DNA (mtDNA), copy DNA (cDNA), bacterial DNA, viral DNA, viral RNA, RNA, message RNA (mRNA), transfer RNA (tRNA), ribosomal RNA (rRNA), catalytic RNA, clones, plasmids, M13, P1, cosmid, bacteria artificial chromosome (BAC), yeast artificial chromosome (YAC), amplified nucleic acid, amplicon, PCR product and other types of amplified nucleic acid. In preferred embodiments, the polynucleic acid may be an oligonucleotide.
Additional embodiments of detection probes of the present invention include emulsions. Particularly preferred embodiments comprise oil/water (O/W) emulsions, water/oil/water (W/O/W) emulsions, and solid/oil/water (S/O/W) emulsions, which comprise vesicles with interaction sites on their outer surfaces. The mass tag molecules are preferably encapsulated in the vesicles. In alternative embodiments, the detergents, which comprise the interface between oil and water or oil and solid phases, works as a mass tag.
Additional embodiments of detection probes of the present invention include soluble bead probes, which comprise beads with interaction sites on their outer surface. The beads preferably comprise a material that can become soluble upon physical or chemical stimulation. The mass tag molecules are preferably solidified with the material. In alternative embodiments, the bead material can preferably work as a mass tag.
Further embodiments of detection probes comprise soluble capsules comprising interaction sites on their surface. The capsules preferably comprise a material that becomes soluble upon physical or chemical stimulation. In order to release the mass tag molecules for detection, these carriers are preferably easily disrupted by physical stimulation, including but not limited to: heat, centrifugation, laser irradiation, sonication, electricity, evaporation, freeze-thaw process, or other methods known to those skilled in the art. Disruption may also be preferably achieved by chemical stimulation including, but not limited to: addition of organic solvent, detergent, acid, alkaline, enzyme, chaotropic reagents (urea, guanidium chloride, etc.), change of buffer, change of salt, change of concentration, change of pH, change of osmotic pressure, and other methods known to those skilled in the art. The mass tag molecules are preferably encapsulated within the soluble capsule. In alternative embodiments, the bead material can preferably work as a mass tag.
Additional embodiments of detection probes of the present invention include soluble porous bead probes, which comprise beads with interaction sites on their outer surface. The beads preferably comprise multiple probes, which can preferably be filled or covered with a material that can become soluble upon physical or chemical stimulation. The mass tag molecules are preferably incorporated into the pores. In alternative embodiments, the bead material can preferably work as a mass tag.
The soluble bead probes, soluble capsule probes, and soluble porous bead probes preferably utilize a material that changes its solubility or shape upon physical (heat, centrifugation, laser irradiation, sonication, electricity, evaporation, freeze-thaw process, etc.) or chemical stimulation (addition of organic solvent, detergent, acid, alkaline, enzyme, chaotropic reagent (urea, guanidium chloride, etc.), change of buffer/salt concentration, pH, osmotic pressure, etc.). These materials work as “mass tags”, or “mass tags” can be solidified, polymerized or encapsulated with them.
For example, beads or capsules made of nucleotides, peptides, saccharides or polymers can preferably become soluble by degrading these components by enzymatic or chemical reactions, or can be deformed by other means of physical or chemical stimulation. Probes made of sol-gel material (collagen, agarose, pectin, etc.) are also preferably deformed through sol-gel transformation upon heating, pH change or other forms of stimulation known to those skilled in the art. Dendrimer, sugar balls, or other forms of drug delivery carriers can also be preferably utilized for multiplex probes as such materials can typically release incorporated mass tag molecules upon stimulation.
The use of mass tag molecules in various embodiments of the present invention allows highly multiplexed assays because the mass tag molecules can be identified by their molecular mass and various analytical methods as mentioned above. Analytical methods, including but not limited to mass spectrometry, can detect even one-mass differences. For example, sixty-three fluorescent dyes of Table 1 (below) and twenty-two phospholipids of Table 2 (below) have at least five mass differences between each other, so they can be identified and quantified by mass spectrometry simultaneously.
TABLE 1
Fluorescent Dyes (cited from Synthegen Catalog)
Catalog
Chemical Name
M.W.
Number
7-methoxycoumarin-3-carboxylic acid
202.0
1307
Pacific Blue
224.2
1304
7-diethylaminocoumarin-3-carboxylic acid
243.0
1306
Marina Blue
252.3
1303
NBD-X
276.3
1720
Alexa Fluor 350
295.4
1730
BODIPY 493/503
302.0
1117
EDANS
307.1
1500
BODIPY R6G
322.0
1106
AMCA-X (Coumarin)
328.0
1300
BODIPY 564/570
348.0
1108
5-Carboxyfluorescein (FAM)
358.0
1001
BODIPY 581/591
374.0
1109
BODIPY FL-X
387.0
1104
Rhodamine Green-X
394.0
1305
6-Carboxytetramethylrhodamine (TAMRA)
413.0
1202
Oregon Green 500
431.0
1102
MAX
441.0
1118
Cascade Yellow
448.5
1706
Carboxynapthofluorescein
458.5
1725
PyMPO
467.4
1710
JOE
487.0
1009
Oregon Green 514
494.0
1103
Cy3
508.6
1401
BODIPY TR-X
519.0
1110
BODIPY 650/665
529.5
1107
5-Fluorescein (FITC)
537.6
1000
BODIPY 630/650
545.5
1113
3′6-Carboxyfluorescein (FAM)
569.5
1007
Cascade Blue
580.0
1705
Alexa Fluor 430
586.8
1731
Lucifer Yellow
605.5
1715
WellRED D2-PA
611.0
1600
DY-555
636.2
1410
WellRED D3-PA
645.0
1601
Rhodamine Red-X
654.0
1302
DY-782
660.9
1421
DY-700
668.9
1417
Alexa Fluor 568
676.8
1736
5(6)-Carboxyeosin
689.0
3310
Texas Red-X
702.0
1301
DY-675
706.9
1416
DY-750
713.0
1420
DY-681
736.9
1423
6-Hexachlorofluorescein (HEX)
744.1
1005
LightCycler Red 705
753.0
1011
DY-636
760.9
1414
DY-701
770.9
1424
FAR-Fuchsia (5′-Amidite)
776.0
1020
DY-676
808.0
1422
Erythrosin
814.0
3311
FAR-Blue (SE)
824.0
1023
Oyster 556
850.0
1800
Oyster 656
900.0
1802
Alexa Fluor 546
964.4
1734
FAR-Green One (SE)
976.0
1024
Alexa Fluor 660
985.0
1740
Oyster 645
1000.0
1801
Alexa Fluor 680
1035.0
1741
Alexa Fluor 633
1085.0
1738
Alexa Fluor 555
1135.0
1735
Alexa Fluor 750
1185.0
1743
Alexa Fluor 700
1285.0
1742
TABLE 2
1,2-Diacyl-sn-Glycero-3-Phosphocholine Saturated Series
(Symmetric Fatty Acid) (cited from Avanti Polar Lipid Catalog)
Carbon
Number
Trivial
IUPAC
M.W.
Catalog Number
3:00
Propionoyl
Trianoic
369.4
850302
4:00
Butanoyl
Tetranoic
397.4
850303
5:00
Pentanoyl
Pentanoic
425.5
850304
6:00
Caproyl
Hexanoic
453.5
850305
7:00
Heptanoyl
Heptanoic
481.6
850306
8:00
Capryloyl
Octanoic
509.6
850315
9:00
Nonanoyl
Nonanoic
537.7
850320
10:00
Capryl
Decanoic
565.7
850325
11:00
Undecanoyl
Undecanoic
593.8
850330
12:00
Lauroyl
Dodecanoic
621.9
850335
13:00
Tridecanoyl
Tridecanoic
649.9
850340
14:00
Myristoyl
Tetradecanoic
678.0
850345
15:00
Pentadecanoyl
Pentadecanoic
706.0
850350
16:00
Palmitoyl
Hexadecanoic
734.1
850355
17:00
Heptadecanoyl
Heptadecanoic
762.2
850360
18:00
Stearoyl
Octadecanoic
790.2
850365
19:00
Nonadecanoyl
Nonadecanoic
818.2
850367
20:00
Arachidoyl
Eicosanoic
846.3
850368
21:00
Heniecosanoyl
Heneicosanoic
874.3
850370
22:00
Behenoyl
Docosanoic
902.4
850371
23:00
Trucisanoyl
Trocosanoic
930.4
850372
24:00
Lignoceroyl
Tetracosanoic
958.4
850373
The molecules of Tables 1 and 2 can be used as mass tags in the vesicle or vesicle components, respectively. If more probes are necessary, polynucleotides or peptides with different sequences can be utilized as mass tags or attached to mass tags because the combination of four nucleotides or twenty-one amino acids with different molecular mass can constitute hundreds of molecules with different molecular weights. This idea can be expanded to combinatorial chemistry, so hundreds, thousands, or millions of “mass tag” molecules can be prepared.
In some embodiments, the mass label may generally be any compound that may be detected by mass spectrometry. In particular embodiments, the mass label may be a biopolymer comprising monomer units, wherein each monomer unit is separately and independently selected from the group consisting essentially of an amino acid, a nucleic acid, and a saccharine with amino acids and nucleic acids being preferred monomer units. Because each monomer unit may be separately and independently selected, biopolymer mass labels may be polynucleic acids, peptides, peptide nucleic acids, oligonucleotides, and so on.
As defined herein “nucleic acids” refer to standard or naturally-occurring as well as modified/non-natural nucleic acids, often known as nucleic acid mimics. Thus, the term “nucleotides” refers to both naturally-occurring and modified/nonnaturally-occurring nucleotides, including nucleoside tri-, di-, and monophosphates as well as monophosphate monomers present within polynucleic acid or oligonucleotide. A nucleotide may also be a ribo; 2′-deoxy; 2′,3′-deoxy as well as a vast array of other nucleotide mimics that are well-known in the art. Mimics include chain-terminating nucleotides, such as 3′-O-methyl, halogenated base or sugar substitutions; alternative sugar structures including nonsugar, alkyl ring structures; alternative bases including inosine; deaza-modified; chi, and psi, linker-modified; mass label-modified; phosphodiester modifications or replacements including phosphorothioate, methylphosphonate, boranophosphate, amide, ester, ether; and a basic or complete internucleotide replacements, including cleavage linkages such a photocleavable nitrophenyl moieties. These modifications are well known by those of skill in the art and based on fundamental principles as described in Sanger (1983), incorporated herein by reference.
Similarly, the term “amino acid” refers to a naturally-occurring amino acid as well as any modified amino acid that may be synthesized or obtained by methods that are well known in the art.
In another embodiment, the mass label may be a synthetic polymer, such as polyethylene glycol, polyvinyl phenol, polypropylene glycol, polymethyl methacrylate, and derivatives thereof. Synthetic polymers may typically contain monomer units selected from the group consisting essentially of ethylene glycol, vinyl phenol, propylene glycol, methyl methacrylate, and derivatives thereof. More typically the mass label may be a polymer containing polyethylene glycol units. Alternatively, the amphiphilic molecules that make up the vesicle may themselves be used as mass tag molecules. For example, vesicles could be created from amphiphilic molecules having differing masses.
The mass label is typically detectable by a method of mass spectrometry. While it is envisioned that any known mass spectrometry method may be used to detect the mass labels of the present invention, methods such as matrix-assisted laser-desorption ionization mass spectrometry, direct laser-desorption ionization mass spectrometry (with no matrix), electrospray ionization mass spectrometry, secondary neutral mass spectrometry, and secondary ion mass spectrometry are preferred.
In certain embodiments the mass label has a molecular weight greater than, but not limited to, about 500 Daltons. For some embodiments, it may be preferred to have nonvolatile (including involatile) mass labels; however, for other embodiments volatile mass labels are also contemplated.
The probes of the present invention have advantages not only in multiplex capability, but also in sensitivity. According to the calculation shown in the Table 3, a 100-nm vesicle can retain 315 mass tag molecules in its inside, 62,800 molecules in its membrane, or 6,342,800 molecules in its membrane and inner vesicles. Moreover, these vesicles can preferably encapsulate more molecules by encapsulating their solid forms (powder, crystal, and other forms known to those skilled in the art) in S/O/W emulsion, soluble beads, soluble capsule. When a single detection probe retains more mass tag molecules, more sensitive detection can be accomplished. For example, Table 3 (below) indicates that a probe containing 6,342,800 mass tag molecules can increase the sensitivity 10 6 ˜10 7 times more than without the probe.
TABLE 3
“mass tag” molecules in a Vesicle [-]
Diameter
Encapsulated
Multi-lamellar
of Vesicle [nm]
Vesicle (*1)
Uni-lamellar Vesicle (*2)
Vesicle (*3)
1
0.00
6.28
634
10
0.32
628
63,428
100
315
62,800
6,342,800
500
39,381
1,570,000
158,570,000
(*1): Assuming that 1M “mass tag” molecules are encapsulated in vesicles.
(*2): Assuming that the vesicle membrane consists of 100% “mass tag” molecules and their density in the membrane is set as 0.5 nm 2 /molecule (Faraday Discuss, 1998, 111, 79-94).
(*3): Assuming that the vesicle membrane consists of 100% “mass tag” molecules and the vesicle encapsulates 1,000,000 of 100-times smaller vesicles whose membrane also consists of 100% “mass tag” molecules.
In addition, in preferred embodiments reproducible detection can be achieved because the number of the mass tag molecules in a single probe can preferably be determined by the size of the vesicle, which can be controlled by size exclusion chromatography or membrane filtration. The size of these vesicles can be measured by several methods, including but not limited to: size exclusion chromatography, coulter counter, light scattering, centrifugation, electron microscopy and atomic force microscopy.
These probes can preferably be applied to simultaneously analyze multiple samples (different source, different time, different stimulation, sample duplication or others known to those skilled in the art) or multiple targets (different genes, proteins, small compounds, and other targets known to those skilled in the art).
When multiple samples are to be analyzed, detection of these interactions in accordance with a preferred embodiment of the present invention can preferably be performed by the following steps: label each sample with different probes, mix the labeled samples, allow interaction with a target molecule immobilized on a surface, wash and remove unbound samples, collect the mass tag molecules from the vesicle, and quantify the mass tag molecules.
When multiple targets are to be analyzed, detection in accordance with a preferred embodiment of the present invention can preferably be performed by the following steps: combine multiple target-tethered vesicle probes, allow interaction with a sample immobilized on a surface, wash and remove unbound probes, collect the mass tag molecules from the vesicle, and quantify the mass tag molecules.
To collect the mass tag molecules, physical stimulation (including, but not limited to heat, centrifugation, laser irradiation, sonication, electricity, and other methods known to those skilled in the art) and/or chemical stimulation (including, but not limited to addition of organic solvent, detergent, acid, alkaline, chaotropic reagents, change of buffer/salt concentration, pH, osmotic pressure, and other methods known to those skilled in the art) can preferably be used to disrupt the vesicles and collect the mass tag molecules for the following analysis. Also, to analyze the “mass tag” molecules, mass spectrometry, electrophoresis or chromatography can preferably by use to identify the molecular weight (or mobility) of each mass tag. In preferred embodiments, the concentration of mass tag molecules can be simultaneously quantified. Also, these vesicle probes may preferably carry other compound tags such as raman-active compounds, fluorescent dyes and luminescent dyes
EXAMPLES
Hybridization Assay
The above encapsulated, uni-lamellar, and multi-lamellar vesicle probes were tested using a hybridization assay.
Oligo(dA) 20 and oligo(dT) 20 -tethered vesicles were prepared. The encapsulated and uni-lamellar vesicles were prepared in the following steps: 20 μmol of 1,2-dipalmitoyl-sn-glycero-3-phosphocholine (DPPC), 20 μmol of cholesterol, 2 μmol of 1,2-dipalmitoyl-sn-glycero-3-[phosphor-rac-(1-glycerol)] (DPPG) and 1 μmol of 1,2-dipalmitoyl-sn-glycero-3-phosphoethanolamine-N-(glutaryl) (glutaryl-DPPE) were dried off in chloroform under a vacuum. The dried lipids were swelled in 1 ml of 50 mM Tris-HCl, pH 7.4, 500 mM NaCl and 100 mM sulforhodamine B (SRB) at 45° C. for 1 hour. The vesicles were prepared by filtering the mixture thirty times with a 2.0-μm-pore membrane and thirty times with a 0.2-μm-pore membrane. The vesicles were purified from unincorporated SRB by G-25 column.
The multi-lamellar vesicle was prepared in several steps. For the “inside liposome,” 10 μmol of 1,2-dipalmitoyl-sn-glycero-3-phosphocholine (DPPC), 10 μmol of cholesterol and 1.5 μmol of 1,2-dipalmitoyl-sn-glycero-3-[phosphor-rac-(1-glycerol)] (DPPG) were dried off in chloroform under a vacuum. The dried lipids were swelled in 0.5 ml of 50 mM Tris-HCl, pH 7.4, 500 mM NaCl at 45° C. for 1 hour. The “small vesicles” were prepared by sonication for 30 minutes at 45° C. The liposome encapsulated inside of the liposome was prepared by drying off 10 μmol of 1,2-dipalmitoyl-sn-glycero-3-phosphocholine (DPPC), 10 μmol of cholesterol, 1 μmol of 1,2-dipalmitoyl-sn-glycero-3-[phosphor-rac-(1-glycerol)] (DPPG) and 0.5 μmol of 1,2-dipalmitoyl-sn-glycero-3-phosphoethanolamine-N-(glutaryl) (glutaryl-DPPE) in chloroform under a vacuum. The dried lipids were swelled in 0.5 ml of the “inside liposome” solution (described above) at 45° C. for 1 hour. The mixture was filtered 30 times with a 2.0-μm-pore membrane and 30 times with a 0.2-μm-pore membrane.
Immobilization of oligonucleotide onto the vesicles was performed in the following steps: 1 nmol oligo(dA) 20 or oligo(dT) 20 was activated with thiol modification at its 5′ end by incubation in 10 mM DTT for 15 min at 45° C. The activated oligonucleotide was purified by G-25 column. The oligonucleotide was mixed with 50 μl vesicle solution at room temperature overnight.
The mass tag of the encapsulated vesicle was sulforhodamine B (SRB) encapsulated in the vesicles, and that of the uni- and multi-lamellar vesicle was 1,2-dipalmitoyl-sn-glycero-3-phosphocholine (DPPC) that accounts for approximately 50% of the membrane components. The vesicles in the hybridization buffer (10 mM Tris, pH 7.4, 500 mM NaCl) were incubated in an oligo(dT) 20 -immobilized microplate (RNAture, CA) for 1 hour at room temperature. After three washes with the hybridization buffer, the hybridized vesicles on the well surfaces were disrupted by addition of 100% methanol. The mass tag molecules were collected into methanol and were analyzed by ESI-TOF mass spectrometry (Waters, Mass.), and quantified by the mass intensities of the corresponding mass peaks. As shown in FIG. 2 , The results indicated that the vesicles with complemented oligo(dA) 20 were captured specifically in the oligo(dT) 20 microplate in comparison with those with non-complemented oligo(dT) 20 or without oligonucleotide. In FIG. 2 , “Oligo(dA)” and “oligo(dT)” are the oligo(dA) 20 - and oligo(dT) 20 -tethered vesicles captured by the oligo(dT) 20 -immobilized microplate, respectively. “W/o oligo” is the vesicle without oligonucleotide captured by the oligo(dT) 20 microplate, and “blank” is 100% methanol. In the encapsulated vesicle, the “mass tag” is sulforhodamine B and quantified by the mass peak at m/z=580.60. In the uni- and multi-lamellar vesicles, “mass tag” is DPPC and quantified by the mass peak at m/z=756.05.
Multiplex Microarray Assay
The messenger RNA or their transcribed cDNA (gene A, B, C, etc.) from Sample P1, P2, P3, etc. of FIG. 3 are labeled with the mass tag probes (p1, p2, p3, etc., which correspond to P1, P2, P3, etc., respectively) to identify their respective sample sources. Labeling is accomplished by several methods such as chemical reaction with active residues on the probe, incorporation of the DNTP attached with the probes and cDNA synthesis using the oligo(dT) or specific sequence primer tethered on the probes. These labeled genes are combined together and applied to a surface with multiple spots where specific sequence polynucleotides (gene a, b, c, etc., which are complement with gene A, B, C, etc., respectively) are immobilized. After hybridization and several washes, each gene spot captures its respective complement gene from multiple samples. Laser irradiation onto each spot disrupts the probes on the spot and ionizes the mass tag molecules for mass spectrometry (MALDI, etc.). Alternatively, addition of organic solvent disrupts the probes and collects the mass tag molecules for mass spectrometry (ESI, etc.) or other analytical methods. The mass peaks of the mass tag molecules obtained from each gene spot simultaneously give the amounts of its complement gene expressed in different samples.
Multiplex Immunoassay
Antibodies (A, B, C, etc.) from sample P1, P2, P3, etc. of FIG. 4 are labeled with the mass tag probes (p1, p2, p3, etc., which corresponds to P1, P2, P3, etc., respectively). The labeled antibodies are combined together and applied to a microplate where each well has a different antigen (a, b, c, etc., which specifically bind to Antibody A, B, C, etc., respectively). After incubation and several washes, each well captures its respective antibody from multiple samples. Laser irradiation onto each well disrupts the probes on the spot and ionizes the mass tag molecules for mass spectrometry (MALDI, etc.) or addition of organic solvent disrupts the probes and collects the mass tag molecules for mass spectrometry (ESI, etc.). The mass peaks of the mass tag molecules obtained from each well simultaneously give the amounts of the corresponding antibody expressed in different samples.
Multiplex Hybridization Assay
Multiple hybridization probes (Probe P1, P2, P3, etc.) tethered with their corresponding sequence-specific oligonucleotides (Oligo A, B, C, etc., which are complement to target genes, Gene a, b, c, etc., respectively) are prepared, as illustrated in FIG. 5 . These probes are combined together and applied to a sample DNA or RNA immobilized on a solid surface by hybridization (mRNA captured by oligo(dT)-coated surface, etc.), physical adsorption (DNA/RNA captured on a glass-fiber surface, etc.), synthesis (DNA/RNA synthesis by polymerase or chemical reaction, etc.) or other methods known to those skilled in the art. After hybridization and several washes, only the probes corresponding to the genes expressed in the sample are captured on the surface. Therefore, analyzing the concentrations of the mass tag molecules on the surface simultaneously gives the multiple gene profiles in the sample DNA/RNA.
Multiplex CpG Methylation Assay
Multiple oligonucleotide-tethered probes are prepared to hybridize against specific sequences of their corresponding CpG methylation sites on genomic DNA. These probes are combined together and applied to fragmented sample DNA captured on a surface coated with CpG-methyl-specific antibody or chemical residue. After incubation and several washes, only the probes corresponding to the CpG methyls expressed in the sample are captured on the surface. Therefore, analyzing the concentrations of the “mass tag” molecules on the surface gives the expression profiles of multiple CpG methylation sites in the sample simultaneously.
Capillary Assay
As illustrated in FIG. 6 , biological samples (DNA, RNA, protein, small compound, etc.) labeled with the probes or target-specific probes (hybridization probe, antibody probe, etc.) are prepared, combined and applied to a capillary 61 . On the inside wall of the capillary 61 , specific target molecules or samples (DNA, RNA, protein, small compound, etc.) are immobilized. After incubation and several washes, specifically bound molecules are captured on the inside wall of the capillary by intermolecular interaction such as hybridization, protein-protein interaction or antigen-antibody interaction. A limited amount of organic solvent 62 disrupts the probe 64 on the wall and collects the “mass tag” molecules 63 in the limited volume when it passes through the capillary 61 , therefore the collected “mass tag” molecules 63 are analyzed at higher concentration. | The present invention comprises detection probes utilizing vesicles or soluble bodies to retain multiple mass tag molecules. The detection probes may be used to simultaneously assay a plurality of different biological samples, each comprising a plurality of analytes, by immobilizing the analytes from each of the samples on a surface incubating the surface with a set of the detection probes, each having mass tag molecules with different masses, removing the unbound detection probe, collecting the first and second mass tag molecules from the bound detection probe, and quantifying the first and second mass tag molecules collected. | 2 |
BACKGROUND OF THE INVENTION
A general description of the thermodynamic and aerodynamic theory underlying the design of the gas turbine engine is presented by H. Cohen, et. al., Gas Turbine Theory, Second Edition, John Wiley & Sons, 1973. On page 232, the reference discusses "cooled turbines" which involves the application of substantial quantity of coolant to the nozzle and rotor blades. This permits an increase in the turbine inlet temperature and thereby increasing the specific power output. The reference mentions that apart from the use of spray cooling for thrust boosting in turbojet engines, the liquid systems have not proved to be practical. A discussion of some of the materials and processes used in the General Electric heavy duty gas turbines is presented in a paper by F. D. Lordi, Gas Turbine Materials and Coatings, GER-2182J, General Electric Co., 1976. This paper gives a detailed description of the processing techniques for casting turbine buckets and nozzles, the alloys from which they are made, and the application of corrosion resistant coatings.
Structural arrangements for the open-circuit liquid cooling of gas turbine buckets are shown by Kydd, U.S. Pat. No. 3,445,481 and 3,446,482. The first patent discloses a bucket having cooling passages open at both ends which are defined by a series of ribs forming part of the core portion of the bucket and a sheet metal skin covering the core and welded to the ribs. The second patent discloses squirting liquid under pressure into hollow forged or cast turbine buckets. Another patent issued to Kydd, U.S. Pat. No. 3,619,076 describes an open circuit cooling system wherein a turbine blade construction consists of a central airfoil-shaped spar which is clad with a sheet of metal having a very high thermal conductivity, e.g. copper. The cladding sheet has grooves recessed in the sheet face adjacent to the spar, which grooves together with the smooth surface of the spar define coolant passages distributed over the surface of the turbine blade. There are numerous disadvantages in forming liquid cooling passages by bonding a sheet to a core in either of the configurations shown in U.S. Pat. Nos. 3,445,481 or 3,619,076. Thus, when a braze is used to bond the skin, some channels of the turbine buckets become plugged and obstructed with braze material. Excellant bonds are required between the core and the skin to contain the water in full channel flow under the extremely high hydraulic pressures which result from the centrifugal forces during operation of the turbine. In addition, any cracks in the skin can cause leakage of the coolant and result in vane failure.
SUMMARY OF THE INVENTION
In accordance with my invention, I have discovered a liquid cooled gas turbine bucket having a pressurized water cooling system flowing in tubes located beneath a protective skin. The bucket is comprised of a body having radial grooves located therein near the surface of the body, thermally conductive tubing is fitted and bonded into the grooves through which the cooling liquid flows, and a protective skin is bonded to the outer surface of the body to provide corrosion resistance against the hot corrosive environment of the gas turbine. The skin is preferrably a composite of an inner skin which provides high thermal conductivity and an outer skin which provides protection from hot corrosion. Pressurization of the system to about 1500 psi allows the cooling water to go through a large temperature rise without encountering vigorous boiling.
BRIEF DESCRIPTION OF DRAWING
The invention is more clearly understood from the following description taken in conjunction with the accompanying drawing in which:
FIG. 1 is a perspective view, with portions broken away, of a turbine bucket having the novel features of the present invention.
FIG. 2 is a transverse sectional view of the airfoil portion of a turbine bucket as shown in FIG. 1 illustrating an embodiment of the invention.
FIG. 3 is an enlarged fragmental view of the airfoil of FIG. 2 showing the location of the cooling tubes.
FIG. 4 is a transverse sectional view of the airfoil portion of a turbine bucket illustrating another embodiment of the invention.
FIG. 5 is an enlarged fragmental view of the airfoil of FIG. 4 showing the location of the cooling tubes.
FIG. 6 is a longitudinal sectional view illustrating the path of the cooling fluid in full channel flow.
FIG. 7 is a longitudinal sectional view illustrating the path of the cooling fluid in partial channel flow.
DESCRIPTION OF PREFERRED EMBODIMENT
Referring to FIG. 1, turbine bucket 10 consists of a shank 12 and a water cooled airfoil 14 constructed from a core 16, having a multiplicity of radial grooves 18 either cast or machined into the surface thereof. The number of these grooves 18 depends on the size and the cooling requirements of the bucket 10. Into these grooves 18 are fitted preformed cooling tubes 20 which are bonded to the core 16 such as by brazing and preferrably have a portion exposed to and in contact with a composite skin 22 which covers and envelopes the outer surface of the core 16. This composite skin 22 is composed of an inner layer or skin 23 which is highly heat conducting to maintain substantially uniform temperature over the surface of the bucket during operation of the turbine, resulting from exposure with the hot gases on the outside of the bucket and the internal water cooling. The preferred inner skin material is copper or a copper containing material which, however, is not resistant to the corrosive atmosphere of the hot gases present during operation of the gas turbine. Therefore, an outer corrosion resistant skin 24 is required to cover and protect the inner skin 23.
The cooling tubes 20 are shown to connect the root plenum 26 and 26a to the tip shroud plenum 30. Some of the cooling tubes 20 continue on to the underside of the tip shroud 28 and serpentine back and forth before emptying into the tip shroud plenum 30. This cools the shroud and aids in the manufacturing process since the shroud cooling channel is a continuation of the airfoil cooling tubes 20. No critical joining is necessary. The core 16 is cast along with the tip shroud 28 and the shank 12 and carries the centrifugal load of the tubes 20, the composite skin 22 and the tip shroud 28.
FIG. 2 shows a cross-sectional of the airfoil section 14 of the turbine bucket 10 and FIG. 3 is an enlargement of the structure in the proximity of one of the tubes 20. As is shown, the cooling tubes 20 are fitted into and bonded to grooves 18 within the core 16 of the airfoil by means of braze 32. The composite skin 22, consisting of an inner skin 23 and an outer skin 24, overlays the tubes 20 and the core 16.
FIG. 4 is a modification of the design of FIG. 2. An enlargement of the structure in the proximity of one of the tubes 20 is shown in FIG. 5. In this embodiment of the invention, the core 16 is cast having a smooth surface without grooves. The cooling tubes 20 are now embedded, such as by powder metallurgy techniques, in a thermally conductive copper layer 23A which acts as a heat exchanger. Again a protective skin 24 covers and provides corrosion protection for the sublayer 23A.
FIG. 6 illustrates a cooling design in which the water is in full channel flow, i.e., the cooling tubes 20 are completely filled with water under pressure, and the arrows indicate the direction of cooling water flow. The water initially travels outwardly from a channel within the shank 12 into the root plenum 26 which is connected to the tubes 20 on the convex side of the airfoil 14. The water then travels through the tubes 20 first cooling the convex side of the airfoil 14 and then serpentines back and forth before discharging into the tip shroud plenum. The water then continues by another serpentine path into the concave side of the airfoil 14 through cooling tubes 20 and empties into the root plenum 26A. Subsequently, the water is discharged through exiting tube 34.
Another embodiment is shown in FIG. 7, wherein the cooling design is such that the water is in partial channel flow i.e., the cooling tubes 20 are only partially filled with water in the liquid form. In this design the water flows outwardly from a channel in the shank 12 into both root plenums 26 and 26A which supply the tubes 20 on the convex and concave sides of the airfoil 14 respectfully. The water then travels outwardly through the tubes 20 into the tip shroud plenum 30 by means of a serpentine path in the tip shroud 28 and out of an exiting port 36.
The formation of mineral deposits or any other material on the inside of the cooling tubes should be avoided. Thus, it is important to use substantially pure water, such as demineralized water.
The outer skin material should exhibit a relatively high thermal conductivity so that the surface temperatures and the thermal gradients can be reduced. The thermal expansion of the outer skin must be equivalent to or preferably less than the subskin in order to reduce the thermal strains. Optimization of these physical properties, maximizes low cycle fatigue and creep-rupture life.
Because of the direct exposure of the skin to the hot-gas stream, material selection becomes more complex. The primary operating requirements for the outer skin are resistance to low cycle fatigue damage, corrosion, hot-gas erosion, foreign object damage, and metallurgical instability. Creep and high cycle fatigue may also be important. Each of these are necessary to achieve long operationg life. Metallurgical instability may result in severe mechanical property degradation.
Fabrication requirements of the outer skin include formability, weldability, brazeability, and material compatability within all the processing steps. Formability is required to successfully wrap the material in sheet form having a thickness of about 5-20 mils around the bucket airfoils and about a 20 percent ductility is considered to be adequate. Weldability and brazeability are required to join the skin sections to themselves and the inner skin. Because of the involved processing, (forming, heat treatments, joining cycles, etc.), the properties must be stable, or at least controllable and predictable, as a result of these operations.
Useful outer skin alloys are described in Table 1. IN617 is shown to have the most desirable properties. The next best alloys are IN671 (Ni-50Cr), Hastelloy-S, Incoloy 825, and Carpenter 20Cb-3 stainless steel. Other materials considered are Nickel 201, the high chromium ferrities (Type 430, Type 446, and FeCrAlY as defined by U.S. Pat. No. 3,528,861), Incoloys 800 and 801, Hastelloy-X, and HS188. Low temperature hot corrosion testing revealed that the IN671 (Ni-50Cr) alloy was the best material of those tested, whereas FeCrAlY, Hastelloy-X and HS188 exhibited significant increases in corrosion rate between 1050° and 1175° F. The Ni-Cr outer skin compositions, as represented by IN671, consist essentially of 50-80% by weight of nickel and 20-50% by weight of chromium.
The water-cooled nozzle and bucket designs require the use of a highly conductive inner skin in order to reduce peak temperatures and minimize thermal gradients. Table 2 lists some useful subskin materials. The need for a high thermal conductivity restricts the number of choices. Because of its high thermal conductivity, copper is preferred. Silver, equally conductive as copper, has not been considered because of its cost and lower melting point. Because of its poor resistance to water erosion and lack of resistance to environmental degradation (corrosion/erosion) by the hot gas, protection of the copper is an absolute requirement; hence, the need for an outer skin. The outer skin materials to protect the copper from the hot gas have been discussed hereinabove.
Table 1__________________________________________________________________________OUTER SKIN MATERIALS Thermal Conductivity Expected Low Expansion 1000° F. Room Tolerance Long Cycle RI-1000° F. (BTU/hr ft.sup.2 Temperature.sup.b) to Time.sup.f) FatigueMaterial (in/in/° F. × 10.sup.-6) ° F./ft Formability Weldability Brazeability.sup.e) Processing Stability Resistance__________________________________________________________________________Hastelloy-S 7.3 11.6 Good Very Good Good Good Excellent.sup.g) Good.sup.j)INo17 7.7 12.4 Good Good.sup.c) Good Good Good.sup.h) Good.sup.j)HS188 8.2 11.5 Good Good.sup.c) Good Good Poor.sup.h) Good.sup.i)Hastelloy-X 8.2 11.3 Good Fair-Good Good Good Poor.sup.h) Good.sup.j)IN671 7.7 -- Marginal Acceptable Acceptable Good Good.sup.i) Fair.sup.i)(Ni-50Cr)Nickel 201 7.4(200° F.) 34.2 Very Good Good Good Good Good.sup.i) Poor.sup.j)FeCrAlY 6.3(Est) 15.2(Est) Marginal Acceptable Acceptable Good Good.sup.i) Poor.sup.j)(25-4-1)Type 446 6.2 13.5 Marginal Poor Acceptable Poor Very Poor.sup.g) Good.sup.j)Type 430 6.3 15.2 Good Poor Acceptable Poor-Fair Poor-Fair.sup.g) Fair.sup.i)Incoley 800 9.4 11.6 Good Good.sup.d) Good Poor Good.sup.g) Good.sup.i)Incoley 801 9.6 11.9 Good Good.sup.d) Good Fair-Good Good.sup.i) Good.sup.i)Incoley 825 8.8 10.9 Good Good.sup.d) Good Good Good.sup.i) Good.sup.i)Carpenter 9.5(Est) 10.5(752° F.) Good Good.sup.d) Good Good Good.sup.i) Good.sup.i)200b-3__________________________________________________________________________ .sup.a) FeCrAlY developmental; all others commercial .sup.b) Formability assessments based upon forming at room temperature. However, improvements can generally be made by either in-process anneals or forming at elevated temperatures. .sup.c) Cobalt-based (e.g., HS188) and nickel-based alloys containing hig Co(e.g., IN617) may exhibit weld cracking in presence of copper. .sup.d) Depending upon preweld condition and/or post-weld heat treatment, this alloy may be destabilized during welding thereby leading to possible aqueous corrosion. .sup.e) Although all alloys considered can be brazed, further effort is essential to identify compatible, ductile, corrosion resistant, and inexpensive braze alloy(s). .sup.f) Stability refers to a materials resistance to structural changes that results in mechanical property degradation such as toughness (FOD) resistance). .sup.g) Based upon data in the expected skin operating range (750 to 950° F.). .sup.h) Based upon the lowest temperature data available (1100 to 1200° F.). .sup.i) Estimated. .sup.j) Calculated.
Table 2__________________________________________________________________________SUBSKIN MATERIALS Water ErosionConductivity Expansion Creep Strength Threshold Elevated Temperature Expected ToleranceMaterial(BTU/hr ft.sup.2 ° F./ft (in/in/° F. × 10.sup.-6) 800° F. (ft/sec) Corrosion Resistance to Processing__________________________________________________________________________ StepsCopper226(68° F.) 9.8(68°- Poor 2.sup.a Poor Poor(OFHC) 572° F.)Glidcop204(68° F.) 10.6(100°- Good 5.sup.a Poor GoodA120 600° F.)Nickel 20142.7(200° F.) 7.4(200° F.) Good 2-5 (Est) Poor Good__________________________________________________________________________ .sup.a) Pure soft water at room temperature, approximate values
Pure copper will not provide sufficient strength (creep and yield) at the bucket trailing edges. Strengthening by cold work will not be effective because of rapid annealing during the processing thermal cycles. A commercially available oxide (Al 2 O 3 ) dispersion strengthened (ODS) copper (Glidcop) is being considered for application at the trailing edges. Glidcop exhibits greater strength with enhanced elevated temperature stability than OFHC copper while retaining a high conductivity.
Small diameter, thin wall (i.e., 100-mil o.d. x 10- to 20- mil wall) corrosion-resistant tubing is required in the bucket designs to isolate the copper subskin from the cooling water since the copper is subject to corrosion. Ideally, the tubing material should exhibit a relatively high thermal conductivity with an equivalent or greater thermal expansion relative to copper. With respect to the latter, most materials investigated exhibit a slightly lower thermal expansion than copper, but the mismatch is not sufficiently large to cause alarm, either during processing or service. In a preferred system, the tubing is fabricated from A286 alloy which has good corrosion resistance and ideally matches the bucket also cast from the same alloy.
The bucket core material does not need the very high-temperature strength required by conventional gas turbine bucket materials (superalloys), since operation would be in the 300° to 600° F. range vs conventional buckets with airfoils at 1200° to 1800° F. and dovetail/shanks at 600° to 1200° F. Although these temperatures suggest a greatly expanded field of materials, a high thermal expansion requirement relative to the outer/inner skin materials narrows this field. A higher tensile strength material is also required for the bucket spar compared with the nozzle spar. Good low cycle and high cycle fatigue resistance is required. Hot-gas corrosion resistance is not required for bucket core materials where protection is provided by the outer skin. However, direct contact with the environment by the spar may present problems. Therefore, the spar materials should have intrinsic corrosion resistance and provide resistance to water erosion.
For good results in fabrication, the core materials must possess good castability (or forgeability), machinability, weldability, and brazeability. Also, any processing of the composite part must also be compatible with the required core material heat treatment in order to maintain the critical strength properties.
Representative bucket core materials include chromium-nickel-iron alloys as represented by A286 and nickel-base alloys as represented by IN718 and U500, the compositions of which are shown in Table 3. The terminology used and compositions are disclosed by W. F. Simmons, Compilations of Chemical Compositions and Rupture Strengths of Superalloys, ASTM Data Series Publication No. DS9E.
The physical properties of these alloys are shown in Table 4. In view of its thermal expansion characteristics, A286 is preferred compared with IN718. However, the weldability of A286 is poor and in large sizes may have to be forged rather than cast.
It will be appreciated that the invention is not limited to the specific details shown in the examples and illustrations and that various modifications may be made within the ordinary skill in the art without departing from the spirit and scope of the invention.
Table 3______________________________________NOMINAL COMPOSITIONS, % A286 IN718 U500______________________________________C 0.05 0.04 0.08Mn 1.40 0.18 0.75.sup.aSi 0.40 0.18 0.75.sup.aCr 15.0 19.0 19.0Ni 26.0 52.5 BalCo -- -- 18.0Mo 1.25 3.05 4.0Cb -- 5.13.sup.b --Ti 2.15 0.90 2.9Al 0.20 0.50 2.9B 0.003 -- 0.005Fe Bal 18.5 4.0.sup.aOther 0.3V -- --______________________________________ .sup.a maximum .sup.b Ta included
Table 4__________________________________________________________________________BUCKET SPAR (CORE) MATERIALSThermal Expansion.sup.b) Room Temperature Expected.sup.d) RI-700° F. 0.2% YS(ksi) Castability Tolerance toMaterial.sup.a) (in/in° F. × 10.sup.-6) Cast Forged Forgeability Machineability Brazeability Weldability Processing__________________________________________________________________________U500 7.0 115 125 Good/Good Acceptable Acceptable Poor PoorA286 9.6 78 118 Poor/Good Acceptable Acceptable Poor GoodIN718 8.1 123 162 Good/Good Acceptable Acceptable Acceptable Good__________________________________________________________________________ .sup.a) All commercially available .sup.b) OFHC Copper: 9.8(RT-672° F.); IN617: 7.5(RT-700° F. .sup.c) Wrought Type 304SS: 35 to 45 ksi; above properties reflect fully heat-treated material per specification .sup.d) Essentially depends on the melting point of copper and the coolin rate from the autoclave processing temperature. Fully heat-treated properties may not be realized. | Turbine buckets are designed for use in an environment of ultra-high temperatures by incorporating therein water cooling channels using preformed tubes which are located beneath an outer protective layer. This layer is preferably composed of an inner skin which provides high thermal conductivity and an outer skin which provides protection from hot corrosion. | 5 |
The invention described herein may be manufactured and used by or for the Government of the United States of America for governmental purposes without the payment of any royalties thereon or therefor.
BACKGROUND OF THE INVENTION
The present invention relates to methods and constructions for attaching cylinders to each other, more particularly to methods and constructions for attaching hollow cylinders at the ends of the cylinders wherein at least one cylinder )is made of composite material.
Conventional approaches to attaching composite cylinders either to other composite cylinders or to metallic cylinders implement bonded/bolted-joint or bolted-joint attachment schemes. The most common conventional methodology for cylinder attachment utilizes a scarf joint.
A significant limitation of these conventional attachment schemes is that the joint is permanent. If disassembly is required, the material is necessarily destroyed. Additionally, the use of a fastener creates some problems for either the bonded/bolted-joint attachment scheme or the bolted-joint attachment scheme. The mechanical fastener typically requires machining of the composite, which removes part of the material. This creates a weak point in the material, a site for stress concentrations, and a site for water migration or penetration from outside to inside.
One described approach accomplishes attachment of a composite cylinder to an aluminum end frame through a double-tapered joint that is machined into the composite shell after cure. See Harruff, P., Tsuchiyama T., and Spicola, F. C., "Filament Wound Torpedo Hull Structures," Fabricating Composites '86 Proceedings, Society of Manufacturing Engineers, Sep. 814 11, 1986, Baltimore, Md., incorporated herein by reference, esp. page 3. Although in this case the joint was detachable, i .t was still of greater stiffness than the bulk material and hence vulnerable. The machining and adhesive were critical to the viability of the joint.
For the B-1B composite Rotary Launch Tube, The U.S. Air Force attached composite cylinders together by adhesively bonding the composite cylinder to an aluminum forging; this method utilized a scarf or single-tapered joint. The composite was mechanically fastened to the metal with Hi-Lok fasteners in addition to the adhesive. Although the joint was thus also mechanically attached, the composite material was drilled and hence still compromised. With the removal of material and cutting of the fibers, this site not only manifested potential for reduced mechanical properties but for vulnerability to damage initiation and propagation.
OBJECTS OF THE INVENTION
In view of the foregoing, it is an object of the present invention to provide a method for composite-cylinder-to-composite-cylinder attachment or composite-cylinder-to-metal-cylinder attachment which creates a mechanically sounder and stronger joint which is less susceptible to damage or breakage at the site of the joint.
It is a further object of the present invention to provide such a method for attachment which creates an easily and nondestructively detachable joint.
Another object of this invention is to provide such a method for attachment which creates a joint which is less susceptible to stress concentrations at the site of the joint.
A further object of this invention is to provide such a method for attachment which creates a joint which is less susceptible to fluid infiltration at the site of the joint.
Other objects of this invention will become apparent from the following detailed description of the invention when considered in conjunction with the accompanying drawings.
SUMMARY OF THE INVENTION
The present invention provides cylinder-to-cylinder attachment method and construction which feature nonutilization of either mechanical fasteners or bonding. This invention is perhaps most markedly advantageous for embodiments wherein at least one of the cylinders is composite and hence the aforediscussed drawbacks of conventional attachment methods are most manifest and appreciably avoided by practice of this invention; however, it is emphasized that this invention is applicable, as appropriate, to attachment assemblies of cylinders having any and all material compositions, and in any and all combinations, e.g., metal-cylinder-to-metal-cylinder attachment.
The present invention provides a method for attaching hollow cylinders at the axial ends of the cylinders, comprising: engaging a fastening ring with a first flanged axial end of a first cylinder whereby a plurality of first teeth mesh with the fastening ring at the locations of intersection of a first circumferential channel with a plurality of axial channels; engaging the fastening ring with a second flanged axial end of a second cylinder whereby a plurality of second teeth mesh with the fastening ring at the locations of intersection of a second circumferential channel with a plurality of axial channels; and, rotating the fastening ring so as to align the first teeth and the second teeth with the axial rows, the first teeth meshing with the recessed faces of the axial rows and interposed between the raised faces of the first lateral circumferential row and the raised faces of the intermediate circumferential row, the second teeth meshing with the recessed faces of the axial rows and interposed between the raised faces of the second lateral circumferential row and the raised faces of the intermediate circumferential row.
The first flanged axial end has a first radially inwardly planar flange which is normal to the axis of the first cylinder. The first radially inwardly planar flange has the plurality of first teeth selectively distributed around the inner perimeter of the first radially inwardly planar flange.
The second flanged axial end has a second radially inwardly planar flange which is normal to the axis of the second cylinder. The second radially inwardly planar flange has the plurality of second teeth selectively distributed, correspondingly with the first teeth, around the inner perimeter of the second radially inwardly planar flange.
The outer circumferential surface of the fastening ring has the first circumferential channel, the second circumferential channel and the plurality of axial channels. The axial channels perpendicularly intersect the first circumferential channel and the second circumferential channel. The first circumferential channel, the second circumferential channel and the axial channels form three parallel circumferential rows of alternating raised and recessed faces and a plurality of parallel axial rows of alternating raised and recessed faces.
The three circumferential rows are a first lateral circumferential row, a second lateral circumferential row and an intermediate circumferential row. The first circumferential channel is interposed between the first lateral circumferential row and the intermediate row. The second circumferential channel is interposed between the second lateral circumferential row and the intermediate row. The axial channels are selectively distributed correspondingly with the first teeth of the first radially inwardly planar flange and with the second teeth of the second radially inwardly planar flange.
Accordingly, the present invention also provides a hollow cylinder assembly of two axially attached hollow cylinders, comprising: a first cylinder having the first flanged axial end, the first flanged axial end having the plurality of first teeth; the second cylinder having the second flanged axial end, the second flanged axial end having the plurality of second teeth which are distributed correspondingly with the first teeth; and, the fastening ring, the outer circumferential surface of the fastening ring having the two parallel circumferential channels and the plurality of parallel axial channels perpendicularly intersecting the circumferential channels, the circumferential channels and the axial channels forming the three parallel circumferential rows of uniformly raised and recessed faces and the plurality of parallel axial rows of uniformly raised and recessed faces. The fastening ring is rotatively aligned and engaged with the first flanged axial end and the second flanged axial end, the first teeth meshing with the fastening ring at the locations of intersection of the first circumferential channel with the axial rows, the second teeth meshing with the fastening ring at the locations of intersection of the second circumferential channel with the axial rows.
Many embodiments of the present invention utilize at least one tooth ring for toothed engagement with the fastening ring, rather than utilizing the radially inwardly planar flange of the flanged axial end of the cylinder for toothed engagement with the fastening ring. For some of these embodiments both the first cylinder and second cylinder utilize tooth rings, viz., a first tooth ring having a plurality of first teeth and a second tooth ring having a plurality of second teeth, respectively. For such embodiments of this invention a method is provided by this invention for attaching hollow cylinders at the axial ends of the cylinders, comprising: engaging a fastening ring with the first tooth ring of the first cylinder whereby the plurality of first teeth mesh with the fastening ring at the locations of intersection of the first circumferential channel with the plurality of axial channels; engaging the fastening ring with the second tooth ring of the second cylinder whereby the plurality of second teeth mesh with the fastening ring at the locations of intersection of the second circumferential channel with the plurality of axial channels; and, rotating the fastening ring so as to align the first teeth and the second teeth with the axial rows, the first teeth meshing with the recessed faces of the axial rows and interposed between the raised faces of the first lateral circumferential row and the raised faces of the intermediate circumferential row, the second teeth meshing with the recessed faces of the axial rows and interposed between the raised faces of the second lateral circumferential row and the raised faces of the intermediate circumferential row.
The first tooth ring is mated within the first flanged axial end of the first cylinder; the second tooth ring is mated within the second flanged axial end of the second cylinder. The first tooth ring has a first circumferentially contoured portion and a first radially inwardly planar portion, the first radially inwardly planar portion having the first teeth selectively distributed around the perimeter of the first radially inwardly planar portion. The second tooth ring has a second circumferentially contoured portion and a second radially inwardly planar portion, the second radially inwardly planar portion having the second teeth selectively distributed, correspondingly with the first teeth, around the perimeter of the second radially inwardly planar portion.
Accordingly, the present invention also provides a hollow cylinder assembly of two axially attached hollow cylinders, comprising: a first cylinder having the first flanged axial end; the first tooth ring having the plurality of first teeth; the second cylinder having the second flanged axial end; the second tooth ring having the plurality of second teeth which are distributed correspondingly with the first teeth; and, the fastening ring, the outer circumferential surface of the fastening ring having the two parallel circumferential channels and the plurality of parallel axial channels perpendicularly intersecting the circumferential channels, the circumferential channels and the axial channels forming the three parallel circumferential rows of uniformly raised and recessed faces and the plurality of parallel axial rows of uniformly raised and recessed faces. The fastening ring is rotatively aligned and engaged with the first tooth ring and the second tooth ring, the first teeth meshing with the fastening ring at the locations of intersection of the first circumferential channel with the axial rows, the second teeth meshing with the fastening ring at the locations of intersection of the second circumferential channel with the axial rows.
The cylinder attachment methodology which is provided in accordance with the present invention features solid and dependable cylinder attachment without degradation to either cylinder material, such as ensues when holes are drilled through cylinder material. The fastening ring, for most embodiments a metallic interface, helps to minimize stress concentrations. The attachment joint provided by this invention is easily and harmlessly disassembled and is capable of supporting both tensile and compressive loading without stress concentration fatigue degradation. The attachment arrangement provided by this invention is especially advantageous for composite cylinders which are subjected to hydrostatic pressure and concomitant possible fluid infiltration; hence, the methodology in accordance with this invention has particularly beneficial application for, inter alia, assembly of manned and unmanned submersibles and aircraft fuselage sections and attachment of pipe and shaft sections.
Other objects, advantages and features of this invention will become apparent from the following detailed description of the invention when considered in conjunction with the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
In order that the present invention may be clearly understood, it will now be described, by way of example, with reference to the accompanying drawings, wherein like numbers indicate the same or similar components, and wherein:
FIG. I is a diagrammatic partial perspective view, partially in section, of a cylinder attachment configuration in accordance with the present invention.
FIG. 2 is a diagrammatic perspective view of a tooth ring according to this invention.
FIG. 3 is a diagrammatic enlarged partial plan view of the tooth ring in FIG. 2.
FIG. 4 is a diagrammatic perspective view of two tooth rings and an interposed fastening ring having teeth and raised faces, respectively, with slanted side surfaces.
DETAILED DESCRIPTION OF THE INVENTION
Referring now to FIG. 1, first cylinder 20 has shown first axial end section 22 and second cylinder 28 has shown second axial end section 30. First flanged axial end 24 of first cylinder 20 has first radially inwardly planar flange 26 which is normal to cylindrical axial direction a 1 of first cylinder 20. Second flanged axial end 32 of second cylinder 28 has second radially inwardly planar flange 34 which is normal to cylindrical axial direction a 2 of second cylinder 28.
First tooth ring 36 has first outer circumferentially contoured portion 40 and first radially inwardly planar portion 42. Second tooth ring 46 has second outer circumferentially contoured portion 50 and second radially inwardly planar portion 52. In this example first outer circumferentially contoured portion 40 of first tooth ring 36 has first taper 82 in axial direction a 1 away from fastening ring 56, in furtherance of reduction of stress concentrations under load; similarly, second outer circumferentially contoured portion 50 of second tooth ring 46 has second taper 84 in axial direction a 2 away from fastening ring 56.
With reference to FIG. 2 and FIG. 3, which show a tooth ring configuration in accordance with this invention which is generally illustrative of either first tooth ring 36 or second tooth ring 46 in this example, first tooth ring 36 has a plurality of first teeth 38 uniformly distributed around first inner toothed perimeter 44 of first inwardly radially planar portion 42 of first tooth ring 36. Second tooth ring 46 has a plurality of second teeth 48 uniformly distributed, correspondingly with first teeth 38, around second inner toothed perimeter 54 of second inwardly radially planar portion 52 of second tooth ring 46. First teeth 38 and second teeth 48 are selectively distributed about inner toothed perimeter 44 and second inner toothed perimeter 54, respectively, in accordance with this invention; in this example distribution of teeth 38 and 48 is selected to be uniform.
Referring again to FIG. 1, first tooth ring 36 is flushly mated within first flanged axial end 24 of first cylinder 20. Second tooth ring 46 is flushly mated within second flanged axial end 32 of second cylinder 28. Techniques are well known in the art for securing mating of flanged axial ends 24 and 32 with tooth rings 36 and 46, respectively; most embodiments of this invention use adhesive at the mating surfaces of the tooth ring and the corresponding flanged axial end. For some embodiments, bolts are preferably used in addition to or instead of adhesive for mating a tooth ring within a flanged axial end.
Outer grooved circumferential surface 58 of fastening ring 56 has a plurality of evenly raised faces 60 and a plurality of evenly recessed faces 62. Recessed faces 62 define first circumferential channel 74, second circumferential channel 76 and a plurality of parallel axial channels 64. Raised faces 60 define first lateral circumferential row 68, second lateral circumferential row 70, intermediate circumferential row 72 and a plurality of parallel axial rows 66. First circumferential channel 74 is interposed between first lateral circumferential row 68 and intermediate if circumferential row 72; second circumferential channel 76 is interposed between second lateral circumferential row 70 and intermediate circumferential row 72. Axial channels 64 perpendicularly intersect first circumferential channel 74 and second circumferential channel 76. Axial channels 64 are selectively distributed correspondingly with first teeth 38 of first tooth ring 36 and with second teeth 48 of second tooth ring 46, in this example uniformly distributed. The three parallel circumferential rows 68, 70 and 72 and the plurality of parallel axial rows 66 each have raised faces 60 alternating with recessed faces 62. The two parallel circumferential channels 74 and 76 and the plurality of parallel axial channels 64 each have recessed faces 62 defining a continuous recessed surface.
The tooth ring in accordance with this invention can be made of any appropriate material, e.g., metal or composite; however, for most embodiments of this invention the tooth ring is preferably metal because the loads may be expected to be more uniformly distributed when isotropic materials are used. The fastening ring in accordance with this invention is preferably made of metal, with a predetermined or selected stiffness.
Fastening ring 56 is engaged with first tooth ring 36 whereby first teeth 38 mesh with fastening ring 56 at first channel intersection locations 78, the locations of intersection of first circumferential channel 74 with axial channels 64. Similarly, fastening ring 56 is engaged with second tooth ring 46 whereby second teeth 48 mesh with fastening ring 56 at second channel intersection locations 80, the locations of intersection of second circumferential channel 76 with axial channels 64. Cylindrical axial directions a 1 and a 2 are equivalent.
Fastening ring 56 is rotated so as to align first teeth 38 and second teeth 48 with axial rows 66. First teeth 38 mesh with recessed faces 62 of axial rows 66 and are interposed between raised faces 60 of first lateral circumferential row 68 and raised faces 60 of intermediate circumferential row 72. Second teeth 48 mesh with recessed faces 62 of axial rows 66 and are interposed between raised faces 60 of second lateral circumferential row 70 and raised faces 60 of intermediate circumferential row 72.
The assembly is detachable by first rotating fastening ring 56 so as to align first teeth 38 and second teeth 48 with axial channels 64. In this alignment, first teeth 38 oppose recessed faces 62 at first channel intersection locations 78 similarly, second teeth 48 oppose recessed faces 62 at second channel intersection locations 80. First cylinder 20 and second cylinder 28 are then each axially separated from fastening ring 56.
In this example compression ring 86 is set radially outwardly adjacent to fastening ring 56 and between first flanged axial end 24 and second flanged axial end 32. Compression ring 86 is substantially flush with first outer circumferential cylindrical surface 88 of first cylinder 20 and second outer circumferential cylindrical surface 90 of second cylinder 28. Compression ring 86 transfers the axial compressive loads between cylinders 20 and 28, and can be made of any appropriate material, including metal, so long as its modulus is considered during design. In some embodiments of this invention compression ring 86 is a sealing ring of any appropriate type of viscoelastic or deformable material which can be compressed and act as a seal.
For many embodiments of this invention, some teeth and lateral raised faces preferably have side surfaces which are complementarily slanted in furtherance of sound engagement of the tooth rings with the fastening ring. Referring to FIG. 4, first teeth 38 and second teeth 48 have lateral side surface slants 92. Raised faces 60 of first lateral circumferential row 68 and raised faces 60 of second lateral circumferential row 70 have medial side surface slants 94. For most such embodiments the inclinations of slants 92 and 94 depend upon the dimensions and relative stiffnesses of cylinders 20 and 28, tooth rings 36 and 46, fastening ring 56, and compression ring 86.
Two especially noteworthy contradistinctions may be drawn among various embodiments of the present invention. In this example both a first tooth ring 36 and a second tooth ring 46 are utilized for toothed engagement with fastening ring 56. One contradistinction is that between those embodiments which utilize either or both of tooth ring 36 and 46 for toothed engagement with fastening ring 56, and those embodiments which do not utilize a tooth ring 36 or 46, i.e., those which utilize both inwardly radially planar flanges 26 and 34 of both flanged axial ends 24 and 32 of both cylinders 20 and 28 for toothed engagement with fastening ring 56. The latter category most particularly includes embodiments of the present invention wherein tooth ring 36 or 46 is preferably used as being is of a stronger material composition than cylinder 20 or 28, as for example wherein cylinder 20 or 28 is composite and tooth ring 36 or 46 is metallic, tooth ring 36 or 46 thus serving to provide a stronger joint than that which would be provided by toothed inwardly radially planar flange 26 or 34 alone in accordance with this invention. Some embodiments of this invention utilize toothed inwardly radially planar flange 26 or 34 and complementarily toothed tooth ring 36 or 46 which are mutually fortifying and together provide teeth 38 or 48.
A second contradistinction is that between those embodiments which utilize axial end sections 22 and 30 which are both prefabricatedly ready for toothed engagement with fastening ring 56 in accordance with this invention, and those embodiments which entail adaptation of either or both of axial end sections 22 and 30 for readiness for toothed engagement with fastening ring 56 in accordance with this invention. For prefabricative embodiments axial end section 22 or 30 is specially manufactured with a view toward toothed engagement with fastening ring 56. Some of these prefabricative embodiments integrally manufacture tooth ring 36 or 46 with axial end section 22 or 30; for many such embodiments cylinder 20 or 28 is composite and tooth ring 36 or 46 is metallic.
For adaptive embodiments adaptation of axial end section 22 or 30 is accomplished, for embodiments involving at least one engagement-ready toothed axial end without use of a tooth ring 36 or 46, by radially inwardly bending and toothing axial end section 22 or 30 so as to form flanged axial end 24 or 32 having inwardly radially planar flange 26 or 34 which is appropriately toothed for engagement with fastening ring 56 in accordance with this invention. For embodiments of this invention which utilize at least one tooth ring 36 or 46 for toothed engagement with fastening ring 56, axial end section 22 or 30 is radially inwardly bent so as to form flanged axial end 24 or 32 having inwardly radially planar flange 26 or 34, and tooth ring 36 or 46 is mated with flanged axial end 24 or 32. For some of these embodiments tooth ring 36 or 46 is segmented to permit or facilitate mating with flanged axial end 24 or 32. For some embodiments axial end section 22 or 30 has a scarfed outer cylindrical circumferential surface 88 or 90 which permits attachment of a complementary cylindrical piece which has the appropriate inwardly radically planar flange 26 or 34 for mating with tooth ring 36 or 46. For some embodiments tooth ring 36 or 46 is not appropriately configured and/or is untoothed and needs to be appropriately configured and/or toothed prior to engagement with fastening ring 56. Techniques are known in the art for manufacturing cylinders with appropriately configured and toothed end sections, as well as for appropriately adapting cylinders which were not manufactured with the appropriate characteristics, in accordance with this invention.
Other embodiments of this invention will be apparent to those skilled in the art from a consideration of this specification or practice of the invention disclosed herein. Various omissions, modifications and changes to the principles described may be made by one skilled in the art without departing from the true scope and spirit of the invention which is indicated by the following claims. | Cylinder-to-cylinder attachment method and construction featuring nonutilization of mechanical fasteners or bonding, especially advantageous for attachment of cylinders which are composite or to be subjected to hydrostatic pressure. A fastening ring is interpositionally and rotatively engaged and aligned with a toothed axial end of each cylinder whereby the inwardly radial teeth for each cylinder appropriately mesh with the outer grooved circumferential surface of the fastening ring. The resultant joint is easily detachable and less susceptible than conventional joints to damage, breakage, degradation, stress concentrations and fluid infiltration. | 8 |
CROSS REFERENCE TO RELATED APPLICATION
[0001] This application claims the benefit of U.S. Provisional Patent Application Ser. No. 60/589,337, filed Jul. 19, 2004.
BACKGROUND OF THE INVENTION
[0002] 1. Field of the Invention
[0003] The present invention relates to cable television systems, and particularly to splitter/amplifier systems for delivering diverse communication services, including voice over IP (VOIP) telephone services.
[0004] 2. Description of the Related Art
[0005] Cable television operators provide a variety of diverse services to consumers. These services include high speed Internet access, video on demand, pay-per-view services, and VoIP services. Cable operators provide these services multiplexed over a single cable using such techniques as frequency division multiplexing (FDM). These services are characterized by the need to provide forward and reverse communication path. The forward path is used to transmit data to the user, while the reverse path is used to return data to the cable operator. The return data might include orders for video on demand or pay-per-view content or data transmitted by the user for destinations on the Internet.
[0006] Key components of CATV systems are drop amplifiers. These amplifiers are inserted into the cable transmission path to make up for losses in the transmission system. Signals are weakened as they pass through cables and components, such as splitters. Splitters are used to separate the services provided by the cable operator for distribution to the appropriate customer equipment for receiving the service.
[0007] Typically the return signal operates at a comparatively lower frequency than the forward path. For example, in a typical system the return signal is in a bandwidth of 5 MHz to about 40 MHz, while the forward path operates at 50-1000 MHz. Diplex filters are used to separate the combined forward and return signal into separate components for amplification using separate amplifiers. In some cases the signal level in the reverse path may be sufficiently high so that no reverse path amplifier is required. For example, set top boxes and cable modems typical provide high output levels, making the reverse path amplifier unnecessary.
[0008] Among the services provided by the cable provider, it is particularly important that the voice over IP (VoIP) service be reliable. While such services as video on demand or pay-per-view are viewed as luxury or non-essential services, VoIP is used to provide telephone communications. Telephone communication are viewed as vital services, particularly during situations involving medical emergencies or natural disasters where communications may be necessary to make essential reports, such as injuries, life threatening medical conditions, or downed power lines. The VoIP circuits may be viewed as essential services because of the need to maintain the circuits in emergency situations.
[0009] Because the amplifiers used in the systems are active components employing complex circuitry and requiring electrical power to operate, the drop amplifiers are potential failure points for VoIP services. In some situations, an emergency or disaster that requires the use of the VoIP services also results in a loss of electrical power, disabling the drop amplifiers and interrupting vital VoIP communications.
[0010] Several devices have been developed for VoIP systems. A representative device is shown in Japanese Patent No. 2004-80,483, published Mar. 11, 2004, which shows in FIG. 1 a VoIP adapter for telephone communications that switches from a telephone line network, such as a packet switched telephone network, to a VoIP network to maintain communications when a failure in the telephone line network is detected. Another representative device is shown in Japanese Patent No. 2005-5,875, published Jan. 6, 2005, which also shows in FIG. 1 a device for switching from a telephone line network, such as a packet switched telephone network, to a VoIP network to maintain communications when a failure in the power supply for the telephone line network is detected.
[0011] While the above-mentioned patent references describe circuit monitoring and switching to maintain telephone communications, neither describes maintaining VoIP communications despite failure of components in an IP network providing the VoIP infrastructure.
[0012] None of the above inventions and patents, taken either singly or in combination, is seen to describe the instant invention as claimed. Thus, a VOIP drop amplifier solving the aforementioned problems is desired.
SUMMARY OF THE INVENTION
[0013] The VoIP drop amplifier connects end user equipment to a broadband system, such as that provided by a cable provider. The amplifier includes a splitter for connecting the equipment to multiple output connectors, and RF amplifiers compensating for losses in the splitter and other passive components in the drop amplifier. The drop amplifier includes an input connection for accepting a broadband cable signal from a cable system and returning broadband signals to the cable system. The drop amplifier includes an amplification path connecting the input connection to a plurality of output connections through amplifiers and a splitter, and a bypass path that bypasses the splitter and the forward and reverse amplifiers in the amplification path to connect the input connection directly to the output connection for VoIP. A sensing circuit monitors the amplifiers and the supply voltages and selects the bypass path when a failure is detected.
[0014] The amplification path includes a forward amplifier for amplifying the forward signals, which are signals originating at the cable operators system, and a reverse amplifier for amplifying the reverse signals, which are those signals originating at the end user's equipment.
[0015] The VoIP amplifier further includes a switch circuit for selecting between the amplification path and the bypass path. The switching circuit is controlled by a dc current and voltage sensing circuit.
[0016] The dc current and voltage sensing circuit monitors dc voltage supplied to the amplifier circuitry. The sensing circuitry also monitors the current supplied to the forward and reverse amplifiers, or to the forward amplifier alone when the reverse amplifier is not provided in the amplification path. The dc voltage supplied to the VoIP circuitry is compared to a reference value to determine whether the dc voltage is sufficient to operate the VoIP active components. When the dc voltage is insufficient the dc current and voltage sensing circuit operates the switching circuit to select the bypass path.
[0017] The amplifier current is compared to two reference values to determine whether the current is within a range including a lower and an upper current limit. When the amplifier current is outside this range, which corresponds to the normal range of expected amplifier currents, the dc current and voltage circuit operates the switching circuit to select the bypass path.
[0018] Under normal voltage and current conditions, the dc current and voltage sensing circuit controls the switching circuitry to select the amplification path. The bypass path supplies only the VoIP output or other output connections designated as essential, while the amplification path supplies all of the output connections including the essential and non-essential connections. In a typical case, only the VoIP output is designated as essential.
[0019] The forward and reverse amplifiers may provide sufficient gain to compensate for losses in VoIP drop amplifier. Alternatively, these amplifiers may provide additional gain to compensate for losses elsewhere in the cable system, such as losses in the cable connecting the VoIP to the cable operator's system.
[0020] These and other features of the present invention will become readily apparent upon further review of the following specification and drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
[0021] FIG. 1 is a block diagram of a typical CATV system incorporating a VOIP drop amplifier according to the present invention.
[0022] FIG. 2 is a functional block diagram of the VoIP drop amplifier according to the present invention operating under normal operating conditions.
[0023] FIG. 3 is a functional block diagram of the VoIP drop amplifier according to the present invention switched to the bypass operating condition after detecting a fault in the system.
[0024] FIG. 4 is a simplified schematic diagram of an embodiment of current and voltage sensing circuitry that may be used in the VoIP drop amplifier according to the present invention.
[0025] FIG. 5 is a simplified schematic diagram of an embodiment of a VoIP drop amplifier according to the present invention using relays as the bypass switches.
[0026] Similar reference characters denote corresponding features consistently throughout the attached drawings.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0027] The present invention is a drop amplifier designed to reliably maintain the VoIP signal path during a loss of power or a failure of active amplifying components.
[0028] FIG. 1 illustrates a system employing a VoIP drop amplifier according to the invention. The cable operator provides communication services to a multi-tap point 46 . The VoIP drop amplifier is connected to the multi-tap connection via a cable that is connected to the RF signal input connector 44 . The VoIP drop amplifier provides amplification for the forward and return signals and splits the signals, delivering them to the output connectors 38 and 40 a - 40 g.
[0029] Connected by cables to the output connectors are various devices for utilizing broadband cable service. Connected to output connector 40 a is a cable modem 24 supplying an Internet connection for a personal computer 48 . Two integrated digital televisions 26 are connected to output connectors 40 b and 40 c . IDTV sets are television sets with the ability to interface with a broadband network to receive such services as video on demand (VOD) or electronic program guide (EPG), as well as broadcast TV. Output connector 40 d is connected to a set top box 30 , which in turn is connected to a conventional television set 28 . Output connector 40 d is connected to a set top box 30 that in turn is connected to a conventional (non iDTV capable) television set 28 . A set top box is common for televisions without iDTV capability. The set top box interfaces with broadband networks to deliver such services as VOD and EPG to conventional television sets.
[0030] The VoIP connector 38 is connected via a cable to a second cable modem 32 , which is connected to a multimedia terminal adapter (MTA) 34 . The MTA is connected to one or more VoIP telephones 36 . The remaining output connectors 40 e - 40 g are shown as unused, but may be connected to additional devices. For example, an additional cable modem and MTA may be connected to one of the unused connectors to provide additional VoIP telephone service, or a third cable modem for Internet access may be connected to one of the unused output connectors.
[0031] The VoIP drop amplifier 20 is shown powered by an uninterruptible power supply (UPS) 22 , which provides power to the VoIP drop amplifier 20 via the input connector 42 . Alternatively, power may be provided to the VoIP drop amplifier 20 from a simple wall transformer.
[0032] FIGS. 2 and 3 are block diagrams by which the basic operating principles of the VoIP drop amplifier 20 may be understood. FIG. 2 shows the amplifier in the normal condition, while FIG. 3 shows the amplifier in a bypass condition.
[0033] As shown in FIG. 2 , the RF signal to and from the cable system is routed through the input connector 44 to a first bypass switch 52 . A switch circuit comprises this first bypass switch 52 , as well as a second bypass switch 54 described below. The switch circuit is controlled by dc current and voltage sensing circuitry 66 . When the dc current and voltage sensing circuitry 66 detects that the amplifier and voltage supply is normal, the switch circuit routes the RF signal through the amplification path. To set up the amplification path, the first bypass switch 52 is set to pass the incoming signal to the first diplex filter 60 . The diplex filter separates the signal into the downstream (50-1000 MHz) signal component coming from the cable system and the upstream (5-40 MHz) signal component coming from the customer's equipment, which is directed back to the cable system. A separate upstream amplifier 56 and a downstream amplifier 58 are provided to make up for losses in passive drop amplifier components and provide unity gain. The downstream signal component originates at the cable supplier, passes through the normally open contact of the first bypass switch 52 , the first diplex filter 60 , the high frequency amplifier 56 , the second diplex filter 62 , and into the splitter 64 . After subdividing at the splitter 64 , the signal is routed to the various consumer equipment, as shown in FIG. 1 , with the exception of the VoIP telephone equipment. The path to the VoIP connector, after passing through the splitter 64 , also passes through the second bypass switch 54 . With the second bypass switch 54 in the energized condition, the downstream signal passes through the normally open contacts of the second bypass switch 54 and then to the VoIP output connector 38 .
[0034] The path for the reverse signal, originating at the consumer equipment is into the connectors 40 a - 40 g through the splitter 64 , into the second diplex filter 62 , through the low frequency amplifier 58 , then through the first diplex filter 60 and through the normal open contacts of the first bypass switch 52 . The VoIP reverse signal first passes though the normally open contacts of the second bypass switch 54 before entering the splitter 64 .
[0035] Preferably, the drop amplifier will provide unity gain (0 db), with losses in the passive components, such as connectors, diplex filters and splitters, being compensated for by the amplifier circuitry comprising the forward amplifier 56 and return amplifier 58 . Alternatively, additional gain may be provided by the forward and return amplifiers 56 and 58 to make up for losses external to the VoIP drop amplifier 20 .
[0036] When an abnormal condition, such as a loss of power to the VoIP drop amplifier or an abnormal operating condition of the RF amplifiers 56 and 58 , is encountered, the dc current and voltage sensing circuit 66 switches the bypass switches 52 and 54 to the normally closed condition, as shown in FIG. 3 . In this condition, the path through the diplex filters 60 and 62 , the amplifiers 56 and 58 , and the splitter 64 is opened completely, isolating these components from the signal path. In this condition, the bypass path 68 is activated, connecting only the VoIP output connection to the cable system. If the overall gain in the normal condition was unity (0 dB), isolating the components and connecting the input connector 44 directly to the VoIP output connector 38 will restore an essentially lossless communication path through the VoIP drop amplifier 20 for the VoIP consumer telephone equipment while removing service from the other consumer equipment.
[0037] By referring to the simplified schematic diagram of FIG. 4 , the operation of dc current and voltage sensing circuitry can be understood.
[0038] The dc current and voltage sensing circuit 66 monitors the current provided to the low and high frequency amplifiers 56 and 58 (see FIGS. 2 and 3 ), as well as the dc power supplied to the VoIP drop amplifier. The amplifier voltage is sampled at the VoIP power supply connector 42 via a voltage sensing circuit. The voltage sensing circuit 110 filters the dc voltage and scales the voltage using a voltage divider or other technique known in the art. The voltage at point 118 is then a scaled value representative of the voltage provided to the unit. This voltage is compared to a reference voltage V REF 3 at a first voltage comparator circuit 108 . If the scaled voltage falls below the reference voltage, indicating that the supply power is failing or has failed, the voltage comparator 108 generates a high output signal as its output.
[0039] The power supplied to the RF amplifiers ( 56 and 58 in FIG. 2 and 3 ) passes through a sampling resistor R 1 , also designated 100 in FIG. 4 . The ohmic value of the sampling resistor 100 is small, so that the voltage drop across the resistor 100 does not interfere with proper operation of the RF amplifiers 56 and 58 by lowering the voltage supplied to the amplifiers at path 116 . The resistor 100 is large enough that the voltage drop across the resistor 100 is easily measurable in the current sensing circuitry. The voltage drop across the sampling resistor R 1 is amplified at an amplifying stage 102 , which generates at output 114 a voltage proportional to the combined current drawn by the RF amplifiers, and the amplifier output 114 is provided to a high current limit comparator 106 and a low current limit comparator 104 . In each circuit the RF amplifier supply current, represented by voltage output 114 , is compared to a reference value (V REF 1 or V REF 2 ). If the current exceeds a high current limit value, the high limit comparator 106 generates a high voltage output value, and if the current drops below the low current limit reference value, the low limit comparator 104 generates a high voltage output signal. When the current is between the high and low levels, the high and low limit comparators generate a low voltage output. The high and low current limits are selected so that when the current draw anticipated for the RF amplifiers 56 and 58 is outside normal limits, the respective current comparator 104 or 106 generates a high output signal.
[0040] The outputs from the high limit comparator 106 , low limit comparator 104 , and the voltage comparator 108 are summed at common connection point 120 . If any of the three comparators generates a high-level voltage output, a Schmidt trigger circuit 112 trips to removes the voltage supplied at point 122 . Otherwise the Schmidt trigger circuit 112 generates a dc output signal, V RELAY, at path 122 . The voltage at path 122 is used to control the bypass switches 52 and 54 of the VoIP drop amplifier 20 . The hysteresis of the Schmidt trigger 112 results in the reset point of the Schmidt trigger 112 being appreciably lower than the trigger voltage, which prevents the bypass switches 52 and 54 from cycling between the normal and the bypass condition when the sensed voltage and current values undergo small fluctuations.
[0041] FIG. 5 is a simplified diagram showing an implementation of the bypass circuitry using relays as the bypass switch 52 and 54 components. Each relay is a single pole double throw (SPDT) type with a common pole that is connected to the normally closed contact when the relay coil is de-energized. When the relay coil is energized, the common pole is disconnected from the normally closed contact and connected to the normally opened contact. Alternatively, a single double pole double throw (DPDT) relay can provide the functionality of the pair of SPDT relays.
[0042] As shown in FIG. 5 the voltage V RELAY, which is the output of the voltage sensing circuit 66 as shown in FIG. 4 , is applied to the relay coils of two SPDT relays 202 and 204 . The common pole of the first relay 202 is connected to the cable system input connector 44 of the VoIP drop amplifier 20 . When the voltage sensing circuit 66 provides a high level output voltage for V RELAY, the relay coil of the first relay 202 is energized, connecting the input through the first diplex filter 60 , the high and low frequency amplifiers 56 and 58 , the splitter 64 , and to each of the output connectors 40 a - 40 g . The coil of the second relay 204 is also energized, closing its normally open contact. The second relay 204 completes the path through the splitter 64 and to the VoIP output connector 38 .
[0043] When the sensing circuit 66 detects a loss of power supply voltage or improper amplifier operation, the V RELAY voltage will be deactivated as described above, resulting in the coils of the bypass relays 202 and 204 becoming de-energized. When the relay coils are de-energized, the signal path through the amplifiers 56 and 58 and splitter 64 , or the amplification path, is isolated by opening of the normally open relay contacts. The normally closed contacts of the bypass relays 202 and 204 are then closed to complete a bypass path 68 , connecting the cable system to the VoIP output 38 . Because the splitter 64 is bypassed in this condition, the bypass path 68 is nearly lossless. If the VoIP drop amplifier 20 is designed for unity gain, the VoIP output connector 38 will be supplied with essentially the same signal level in the bypass condition as in the normal condition. Non-essential consumer equipment, such as the PC Internet connection, will be disconnected from the cable signal when the VoIP drop amplifier 20 is in the bypass condition.
[0044] A complete loss of all power supplied to the VoIP drop amplifier 20 will result in disabling the voltage and current sense circuitry 66 . Because the bypass path through the amplifier 20 is selected using the normally closed contacts of the bypass switches 52 and 54 , the loss of power to the VoIP drop amplifier 20 will result in bypassing the de-energized active circuitry and the splitter 64 of the drop amplifier 20 , thus maintaining a loss-free connection to the consumer's VoIP telephone equipment.
[0045] In an example implementation, the reverse amplifier 58 comprises an RF Micro Devices RF2317 integrated circuit based RF amplifier, while the forward amplifier 56 comprises an ANADigics Inc. ADA10000 integrated circuit based broadband RF amplifier. The comparator circuits 104 , 106 , and 108 are implemented using conventional operational amplifier circuits, such as the LM2900. The current supplied to the two RF amplifier circuits passes through a 1-ohm resistor 100 , developing a voltage across the resistor 100 proportional to total amplifier current. This voltage is compared to reference voltage supplied to the current comparators 104 and 106 to implement the high and low current limits described above. The low current limit is approximately 180 milliamps (mA), while the high current limit is at approximately 300 mA. The nominal expected current draw for the amplifier circuitry is 250 mA. The current limit values are chosen to be consistent with the range of expected currents for the particular amplifier circuits used in the VoIP drop amplifier 20 . When amplifier current is outside of the expected range of values, the dc current and voltage sensing circuit 66 removes the voltage to the coils of the bypass relays 52 and 54 , switching the circuit into the bypass condition described above. After a trip due to an out-of-range current, the VoIP resets when the current increases to 200 mA or decreases below 280 mA due to the hysteresis of the Schmidt trigger 112 circuitry. The voltage sensing circuitry conditions the incoming voltage using filters and surge suppressors, and then employs a voltage divider network to provide a voltage proportional to the supply voltage. This voltage is compared to a reference voltage developed from an integrated circuit voltage regulator to establish the low voltage trip point. The low voltage limit is approximately 13 volts, with the normal supply voltage for the VoIP being 15-volts dc. When the supply voltage drops below the low voltage limit, the voltage and current sensing circuit 66 removes the voltage to the coils of the bypass relays 52 and 54 , switching the circuit into the bypass condition described above. After a trip due to a low supply voltage, the VoIP resets to use the amplification path when the voltage increases to at least 14 volts due to the hysteresis of the Schmidt trigger 112 circuitry. The circuit components, voltages and currents described above are by way of example and do not limit the invention to the particular components and circuit values detailed.
[0046] The dc current and voltage sensing circuit may use other means of detecting faults in the drop amplifier circuitry. For example, the integrated circuit amplifiers used to implement the forward and reverse amplifiers may include an output signal indicating normal operation of the amplifier. The dc current and voltage sensing circuitry could detect the loss of the normal operation signal and trigger the selection of the bypass path. In addition to sensing the dc voltage supplied to the unit, the dc voltage and sensing circuit may sample an ac supply voltage by rectifying and filtering the ac voltage to obtain a dc voltage representative of the ac supply voltage. The representative dc voltage may be compared to a reference and the results of the comparison may be used to control the bypass circuit.
[0047] Separate sensing resistors may be provided in the respective current paths supplying the forward and reverse amplifiers. By providing separate sensing resistors, and separate pairs of low and high current comparator circuits, the currents provided to the forward and reverse amplifiers can be monitored separately rather than as a combined value. The current set points of set of low and high current comparators are chosen based on the expected operating currents for the respective amplifier.
[0048] In another variation of the VoIP drop amplifier, the amplifier circuitry may include a forward amplifier but no reverse amplifier. This configuration is useful when user components such as a set top box or a cable modem generate reverse signals at sufficiently high levels so that amplification of the return signal from these user components.
[0049] It is to be understood that the present invention is not limited to the embodiments described above, but encompasses any and all embodiments within the scope of the following claims. | The VOIP drop amplifier connects end user equipment to a broadband system, such as that provided by a cable provider. The amplifier includes a splitter for connecting the cable signal to multiple output connectors, and RF amplifiers compensating for losses in the splitter and other passive components in the amplifier. The drop amplifier includes an input connection for accepting a broadband cable signal from a cable system and returning broadband signals to the cable system. The drop amplifier includes an amplification path connecting the input connection to the plurality of output connections through RF amplifiers and a splitter, and a bypass path that bypass the splitter and forward and reverse amplifiers in the amplification path to connect the input connection directly to the output connection for the essential circuits. A sensing circuit monitors the amplifiers and the supply voltages, and selects the bypass path when a failure is detected. | 7 |
CROSS REFERENCE TO RELATED APPLICATION
This application is a National Stage of International Application No. PCT/CH2010/000127 filed May 11, 2010, claiming priority based on Swiss Patent Application No. 00867/09, filed Jun. 5, 2009, the contents of all of which are incorporated herein by reference in their entirety.
TECHNICAL FIELD
The present invention relates to a mixing device, to a discharge device equipped with such a mixing device, and to a method for producing a mixture of flowable components.
PRIOR ART
An objective in many applications is to produce and discharge a mixture of several flowable components in a predefined mixing ratio. An example is the production of an adhesive for technical or medical uses, e.g. an epoxy resin adhesive or a medical glue based on fibrin, from two or more components. Another example is the production of a bone cement from several components. In systems of this kind, the curing time can be very short, and the product therefore has to be discharged immediately after being mixed.
To this end, the prior art discloses discharge devices in which two components that are to be mixed are stored in a double syringe with two syringe containers, two outlets and two interconnected syringe pistons, or are sucked into such a double syringe shortly before application. A mixing device with two inlet channels is then fitted onto the double syringe, said inlet channels adjoining the outlets of the double syringe. The inlet channels open into a mixing channel, in which a static mixing element is located, in most cases in the form of a mixing helix with helically arranged mixing blades. When the interconnected syringe pistons are then pushed into the double syringe, the two components are fed from the syringe containers into the mixing device, where they are mixed with each other and discharged immediately thereafter. A discharge device of this kind is known, e.g., from WO 2006/005205.
GB 1 423 933 discloses a mixing device for industrial applications, in which the mixing action for two components that are to be mixed is improved by means of two mixing channels, with mixing elements arranged therein, being routed in parallel in pairs. The outlets of the two mixing channels are brought together in a chamber. This chamber opens in turn into two parallel mixing channels which, with respect to the direction of flow, are offset by 90° in relation to the previous two mixing channels. This arrangement is repeated a number of times.
In certain applications, however, instead of just two components it may be necessary for three or more components to be mixed and then immediately discharged.
SUMMARY OF THE INVENTION
It is therefore an object of the present invention to make available a mixing device that permits the production and subsequent discharging of a mixture composed of at least three components.
It is thus proposed to carry out a sequential or serial mixing procedure in which the first two components are first of all mixed and then other components (which can optionally be a mixture themselves) are admixed. To this end, a through-flow mixing device for producing a mixture of flowable components is proposed which comprises:
at least a first and a second inlet channel for the components to be mixed; an outlet channel for the mixture to be produced therefrom; and a first mixing channel arranged, in the direction of flow, between the inlet channels and the outlet channel and accommodating at least one mixing element, wherein the first and second inlet channels open directly or indirectly into the first mixing channel; a second mixing channel arranged, in the direction of flow, between the first mixing channel and the outlet channel and accommodating at least one mixing element, wherein the first mixing channel opens directly or indirectly into the second mixing channel, and at least a third inlet channel, which opens directly or indirectly into the second mixing channel.
The second mixing channel then opens directly or indirectly into the outlet channel of the mixing device.
In other words, a through-flow mixing device is thus proposed which, viewed in the direction of flow, has at least two flow mixers connected in series. At least two components are delivered to the first flow mixer and are mixed together in this flow mixer. Thereafter, in the second flow mixer, the resulting intermediate product has added to it at least one further component (which itself can also be an intermediate product). The terms “directly” and “indirectly” are to be understood as follows. A channel opens “directly” into another channel when there is no further mixer located between these channels. A channel opens “indirectly” into another channel when a further mixer is located between the channels, and in particular if further components are admixed in the further mixer.
The components should generally be flowable. This includes liquid, viscous and powdery components, if appropriate also gaseous components. The components can all be different, although it is also possible for two or more components to be identical. In particular, it is conceivable that the components delivered through the second and third inlet channels are identical, such that only the mixing ratio is changed between the first and second mixers. In this case, the third inlet channel can branch off from the second inlet channel.
At least the first and second inlet channels, preferably also the third inlet channel, preferably each have a connector element for a container. This connector element can be designed in any known way, e.g. as a male or female Luer connector. It is also conceivable to design a common connector element for all three or more channels. In this case, each inlet channel has a connection portion designed for connection to a container. To make connection easier, at least the first and second inlet channels, preferably also the third inlet channel, can extend parallel to one another in the area of the connector elements. The first, second and third inlet channels can be arranged substantially in a common plane in the area of the connector elements, although they can also form a triangle, for example. The connectors can be coded, i.e. differently designed, such that each connector can only be connected to a corresponding complementary connector of a matching container, or they can be designed and arranged such that the mixing device can be connected only in a well-defined position to a matching container arrangement.
The mixing elements in the mixing channels can be any desired static or dynamic mixing elements, as are known per se. In a preferred embodiment, the first and/or second mixing elements are static mixing elements. Mixing elements of this kind have long been known. They can, for example, comprise a helix with a plurality of helical blades or vanes arranged thereon.
In a particular embodiment, the mixing device also comprises a third mixing channel accommodating at least one mixing element, and a fourth inlet channel. The third inlet channel and the fourth inlet channel then open into the third mixing channel, and the third mixing channel opens directly or indirectly into the second mixing channel.
The invention also relates to a discharge device that comprises a mixing device of the type described above. The discharge device further comprises at least a first and a second container, wherein each container has a container outlet, and wherein the container outlet of the first container can be connected to the first inlet channel, and the container outlet of the second container can be connected to the second inlet channel. Preferably, a third container with a container outlet is also present, wherein this container outlet can be connected to the third inlet channel. Any desired containers can be used, e.g. syringes, carpules (i.e. containers that have a cylindrical wall portion and are closed at one end by a septum and at the other end by a movable piston), bags, tubes, etc. The containers can be accommodated in a common cartridge or can be connected to one another in some other way and form a single container unit. The container unit is then designed to be connected as a whole to the mixing device.
For this purpose, the inlet channels of the mixing device and the container outlets of the containers preferably have mutually corresponding connector elements or connection portions, which are designed and/or arranged in such a way that the container outlet of the first container can be connected only to the first inlet channel, and the container outlet of the second container can be connected only to the second inlet channel.
The discharge device preferably further comprises at least one discharge element in order to discharge the components from the containers and dispense said components through the container outlets. The discharge element can then usually be actuated manually. If the containers have a syringe-shaped or carpule-shaped design for example, the discharge element is, for example, a piston rod for each container. By contrast, if the containers are bag-shaped or collapsible tube-shaped for example, the discharge elements can also have completely different shapes. If several discharge elements are present, these are preferably connected to a common actuating element, so as to permit, by manual actuation of the actuating element, simultaneous dispensing of the components from the containers.
In a simple embodiment, each of the containers has a syringe-shaped design, with a syringe body having a cylindrical wall portion, and with a piston movable in the syringe body. The syringe bodies can then be rigidly interconnected in order to form a multiple syringe, and the pistons can be rigidly interconnected in order to ensure joint discharging from the syringes.
The quantities that are processed with a mixing and discharge device of this kind are normally small and vary within the range of about one to a few hundred milliliters. In other words, the containers normally have a volume of in each case less than about 300 ml. The sizes of the mixing device in each dimension usually reach at most about 30 cm, typically even less than 15 cm. The cross section of the mixing channels is typically less than about 5 cm 2 .
According to a further aspect, the present invention relates to a method for producing a mixture of flowable components, said method comprising:
feeding a first and a second component through a first mixing channel accommodating at least one mixing element, in order to mix the first and the second component with each other to form a first intermediate product; feeding the first intermediate product, together with a further component, through a second mixing channel accommodating at least one mixing element, in order to mix the first intermediate product together with the further component.
This method can be set up as an operating method for a device of the type described above, but it can also be carried out using other types of devices.
BRIEF DESCRIPTION OF THE DRAWINGS
Preferred embodiments of the invention are described below with reference to the drawings, which are provided only for illustration and are not to be interpreted as limiting the invention. In the drawings:
FIG. 1 a shows, in longitudinal section, a highly schematic view of a discharge device with mixing device according to a first embodiment;
FIG. 1 b shows an enlarged view of the mixing device from FIG. 1 a; and
FIG. 2 shows a highly schematic view of a mixing device according to a second embodiment.
DESCRIPTION OF PREFERRED EMBODIMENTS
FIGS. 1 a and 1 b show highly schematic views of a discharge device in longitudinal section. The discharge device comprises a container unit in the form of a multiple syringe 200 (here a triple syringe) with three rigidly interconnected containers 210 , 220 and 230 in the form of syringe bodies, which are closed by pistons 214 , 224 , 234 . In the present example, the containers are arranged next to one another in a common plane, but they can also have another arrangement. The containers can have identical cross sections or, as in the present example, different cross sections and, therefore, also different volumes. Each syringe body has a cylindrical jacket wall 211 , 221 , 231 , and a top wall 212 , 222 , 232 which delimits the syringe body in the distal direction and in each of which a container outlet 213 , 223 , 233 is formed. A piston 214 , 224 , 234 is inserted from the proximal direction into each syringe body and provides a seal with the jacket wall. A piston rod 215 , 225 , 235 is connected to each piston. At their proximal end, the piston rods are rigidly interconnected by a common actuating element 240 , here in the form of an actuating flange.
A mixing device 100 is mounted on the container outlets 213 , 223 , 233 . The mixing device has three inlet channels 110 , 120 , 130 , of which the proximal end portions extend parallel to one another and, in the present example, are designed as connectors 111 , 121 , 131 ( FIG. 1 b ) for fitting onto the multiple syringe 200 . The connectors are only shown very schematically here. Many different types of connectors are conceivable here, e.g. standardized Luer connectors with the customary frustoconical contact surfaces and with or without a securing nut (Luer lock). The connectors are preferably coded, i.e. designed such that the mixing device can be fitted only in a well-defined position onto the multiple syringe, e.g. by choosing different diameters of the connectors or defined combinations of male and female connectors. Of course, completely different types of connectors and codings are also possible that permit a defined connection between the outlet of each container and the associated inlet channel.
The first inlet channel 110 and the second inlet channel 120 open into a first mixing channel 141 . Before the inlet portion 143 of the mixing channel 141 , the two inlet channels 110 , 120 run toward each other at an acute angle. However, it is also possible for the two inlet channels to be brought together in another way, e.g. parallel to each other or one surrounding the other in a ring shape, etc. The exact way in which the inlet channels are merged is not essential to the basic mode of operation of the mixing device.
The mixing channel 141 accommodates a static mixing element 142 which, together with the mixing channel 141 , forms a first flow mixer 140 . The mixing element is designed in the usual way as a mixing helix, wherein the helix has a plurality of successively disposed helical mixing blades by means of which the volume flow passing through the mixing channel is divided up, diverted and recombined a number of times in order to achieve thorough and optimally homogeneous mixing together of the mixing material. Mixing helices of this kind have long been known per se, and the exact nature of the mixing element is not essential to the basic mode of operation of the mixing device. Instead of a static mixer, it is also possible in principle to consider using a movable, externally driven mixing element, e.g. a rotatable mixing element.
At its outlet portion 144 , the first mixing channel 141 opens into the inlet portion 153 of a second mixing channel 151 with a static mixing element 152 . The second mixing channel 151 and the second mixing element 152 together form a second flow mixer 150 . The latter can be constructed in the same manner as or in a different manner than the first mixer 140 and have the same or different dimensions, in particular length; the exact structure is once again not essential to the basic mode of operation of the mixing device.
The third inlet channel 130 extends, in a delivery section 132 , parallel to the first mixing channel 141 and opens with a distal mouth portion 133 likewise into the inlet portion 153 of the second mixing channel 151 . Once again, the outlet portion 144 of the first mixing channel 140 and the mouth portion 133 of the third inlet channel 130 can be brought together in any desired manner known per se.
In the present example, the outlet portion 154 of the second mixing channel 151 is adjoined directly by the outlet channel 101 of the mixing device 100 , or this outlet channel is formed by the outlet portion 154 . The outlet channel 101 can be provided with fastening means for attachment of an accessory, e.g. with a Luer cone for attachment of a spray device or of another accessory, or can itself be designed in any desired form, e.g. fan-shaped for a planar discharging of the mixing product. The exact configuration of the outlet portion is also not essential to the basic mode of operation of the mixing device.
In operation, the containers 210 , 220 , 230 are first of all filled with the components to be mixed and are vented, if this has not yet been done. Then the mixing device 100 is mounted on the multiple syringe. By manual pressure on the actuating element, the three pistons 214 , 224 and 234 are pushed forward to the same extent, such that the components located in the containers pass through the outlets 213 , 223 , 233 of the containers into the inlet channels 110 , 120 , 130 of the mixing device. Here, the components from the first two containers 210 , 220 are first of all brought together and mixed in the first mixer 140 . The resulting intermediate product emerges from the first mixer 140 and is brought together with the third component from the container 230 and mixed in the second mixer 150 . The resulting product is then discharged through the outlet channel 101 . The components thus undergo sequential or serial mixing.
A mixing device of this kind can be advantageously used wherever a plurality of components are intended to be mixed together in succession. An example is the production of a bone cement from two components known per se, to which an active substance, e.g. a growth factor or an antibiotic, is to be admixed. The two cement components are in this case delivered through the first and second inlet channel and mixed in the first mixer, while the active substance is delivered through the second inlet channel and admixed in the second mixer. Another example involves two components of an adhesive system (e.g. two monomers), which are first of all mixed together in the first mixer and are then mixed together with a catalyst and/or promoter in the second mixer. Another possible application is one in which the viscosity of a mixture is intentionally influenced by admixture of a component through the third inlet channel. Many other applications are conceivable in which, for chemical or physical reasons, a defined sequence of mixing is necessary or desirable.
Although the three components to be mixed will be different in many applications, it is nonetheless also conceivable that the components in the second container and third container are identical, such that the component from the first container is first of all mixed in the first mixer with a smaller quantity of the other component, before the final mixing ratio is fixed in the second mixer. In this case, embodiments are also conceivable in which, instead of the third inlet channel being connected to a separate container, the second container opens with its outlet both into the second inlet channel and also into the third inlet channel, and these inlet channels are thus connected in the area of their proximal ends or branch off from a common inlet. This results in some of the component from the second container bypassing the first mixer.
It is also not strictly necessary for the components to be delivered from the three containers in a fixed and predetermined ratio, and instead the three pistons can also be advanced independently of one another or in an adjustable ratio of advance.
The mixing device can of course also be used with containers of other designs. Possible examples of such containers are: a cartridge which contains a plurality of containers and from which material is discharged via an integrated or independent actuating element; a tube arrangement; a bag system with flexible bags as containers, etc. The essential point is simply that each container has an outlet and that at least one discharge element is present that can be actuated in such a way that, upon actuation, the content is discharged from the container through the outlet. All the containers advantageously form a common unit.
Another embodiment of a mixing device is shown in FIG. 2 . Identical or corresponding parts are designated by the same reference numbers as in FIGS. 1 a and 1 b. This mixing device 100 ′ has four inlet channels 110 , 120 , 130 and 170 . The first two channels 110 , 120 open into a first mixer 140 . As in the previous illustrative embodiment, this mixer is followed downstream by a second mixer. The other two channels 130 , 170 open into a third mixer 160 with mixing channel 161 and mixing element 162 . The outlet portions of the first and third mixers open jointly into the second mixer.
In operation, the components from the first two inlet channels are fed through the first mixer 140 , in order to mix these components together to form a first intermediate product, while the components from the other two inlet channels are fed through the third mixer, in order to mix these components together to form a second intermediate product. The first and second intermediate products are then fed through the second mixer 150 and mixed with each other. As before in the first illustrative embodiment, each mixer comprises a mixing channel and a mixing element arranged in the latter.
In the second illustrative embodiment too, many variations and modifications are once again possible.
Thus, in this case too, it is once again possible for two components to be identical, e.g. the components that pass through the inlet channels 120 and 130 . These channels can accordingly also branch off from a common inlet. While a linear arrangement of the connectors of the mixing device is shown here, any other desired arrangement is also possible. Here too, the connectors can be designed such that they can be connected only in a very specific manner to a corresponding multiple container.
It is clear from the abovementioned examples that there are also many possible variations in respect of the arrangement of the individual mixers in the mixing device. Thus, instead of a two-stage sequential mixing procedure, it is also possible to provide a three-stage sequential mixing procedure in which at least three mixers are present, arranged one after another in the direction of flow, and in which a further component (which itself can once again be the intermediate product from a preceding mixing procedure) is admixed after each mixer. Thus, individual mixers can be combined with one another in substantially any desired topologies. Each individual mixer can also be designed to mix together not just two components but also three or more components in a single step.
LIST OF REFERENCE SIGNS
100 , 100 ′ mixing device
101 outlet channel
110 first inlet channel
111 first connector
120 second inlet channel
121 second connector
130 third inlet channel
131 third connector
132 delivery section
133 mouth portion
140 first mixer
141 first mixing channel
142 first mixing element
143 inlet portion
144 outlet portion
150 second mixer
151 second mixing channel
152 second mixing element
153 inlet portion
154 outlet portion
160 third mixer
161 third mixing channel
162 third mixing element
170 fourth inlet channel
171 fourth connector
200 multiple syringe
210 first container
211 jacket wall
212 top wall
213 outlet
214 piston
215 piston rod
220 second container
221 jacket wall
222 top wall
223 outlet
224 piston
225 piston rod
230 third container
231 jacket wall
232 top wall
233 outlet
234 piston
235 piston rod
240 actuating element | A mixing apparatus for producing a mixture of flowable components is provided. Two inlet channels for the components to be mixed open into a first mixing channel having at least one mixing element disposed therein. A second mixing channel having at least one mixing element disposed therein is connected downstream of the first mixing channel. A third inlet channel opens directly or indirectly into the second mixing channel in order to admix a third component. In further embodiments, three or more mixing channels are present. In addition, a discharge comprising such a mixing apparatus and corresponding containers and a method for mixing at least three components are provided. | 1 |
REFERENCE TO PRIOR APPLICATIONS
[0001] This application is a continuation of: (i) U.S. Design patent application Ser. No. 07/745,995 filed Aug. 9, 1991, which is a continuation of Design patent application Ser. No. 07/292,742 filed Jan. 3, 1989; and (ii) U.S. patent application Ser. No. 07/763,870 filed Sep. 19, 1991, which is a continuation of application Ser. No. 07/507,002 filed Apr. 10, 1990, which is a continuation of application Ser. No. 07/319,852 filed Mar. 3, 1989, which is a continuation of application Ser. No. 07/101,832 filed Sep. 28, 1987, which is a continuation-in-part of application Ser. No. 07/926,291, filed Nov. 3, 1986, and now issued as U.S. Pat. No. 4,724,642. The disclosure of U.S. Pat. No. 4,724,624 is hereby incorporated by reference.
BACKGROUND OF THE INVENTION
[0002] This invention relates to outdoor residential constructions, and is particularly concerned with support devices for use in deck construction.
[0003] Various types of devices have heretofore been used for supporting and/or connecting building elements, such as horizontal beams, joists, stringers, posts and pillars, to a base slab, footing, foundation or block member. For example, such devices include anchor studs, metal brackets, or other supports or devices which are permanently embedded in the concrete in the manufacturing process of the blocks and which are required to make them functional. Such devices or additional components are used to provide vertical and lateral mechanical connection of building elements to a base or as components to other elements but do not have an individual identity or non-mechanical application which facilitates the inexpensive and convenient construction of a simple deck, such as a deck that may be built by the average home owner on unprepared and unleveled ground typical to a residential backyard.
SUMMARY OF THE INVENTION
[0004] According to the present invention and forming a primary objective thereof, a deck construction is provided including a novel construction support device, which amounts to an improvement over prior structures.
[0005] A more particular object of the invention is to provide a construction support device of the type described having a novel arrangement of recesses, walls, and sockets for receiving horizontal beams and the like, and also capable of receiving vertical pillars or posts, all in a variety of selected support connections not heretofore available.
[0006] Another object of the invention is to provide an embodiment of the invention comprising a plurality of integrated wall portions disposed in a zig zag pattern and forming one or more full width slots for receiving horizontal beams and the like and also forming a rectangular central socket for receiving a vertical pillar or post.
[0007] Another object of the invention is to provide a pier block of the type described having a novel arrangement of recesses and central socket for receiving horizontal two-inch thick (1½-inch nominal) surface supports, and also capable of receiving vertical wood posts without mechanical connections or additional components, all in a variety of selected support configurations not heretofore available.
[0008] In carrying out these objectives, a construction support device is provided for anchoring a beam or other element to the ground or other building site. The device includes a body having upper and lower portions. The lower portion rests on the building site, and the upper portion includes an open slot for holding a beam edgewise. The slot is formed by spaced-apart side walls. The side walls themselves include connected wall portions, which are integrally joined at right angles.
[0009] The slot includes a center socket portion that is adapted for securely holding the bottom end of a vertically oriented post. The center socket portion is formed by the side walls extending at right angles away from each other to form corner sections. The corner sections are spaced apart substantially further than the width of the open slot to provide substantial corner support to the post.
[0010] In some cases, the side walls which define the slot are part of spaced-apart projections which extend from the upper portion of the body. These projections can be integrally molded with the body to form a single-cast, one-piece block or pier. Alternatively, they may be formed of plastic or metal and suitably attached to a base.
[0011] The invention may be practiced with a pair of recesses emanating from the central socket portion to form a single slot which extends unobstructed across the entire breadth of the body. Alternatively, a second pair of recesses may be employed to form a total of two mutually perpendicular slots.
[0012] Support devices in accordance with the invention are particularly suited to the construction of residential decks. Horizontal, coplanar deck support members may be carried by a plurality of the foregoing support devices arranged in rows and columns. The horizontal deck support members are securely seated in the slots defined by the spaced apart side walls.
[0013] Where the deck is to be built on uneven ground, the horizontal members can be supported in a level attitude by a plurality of vertical support pillars. The bottom ends of the vertical support pillars are securely seated in one of the center socket portion, while their respective top ends bear the horizontal members in supporting engagement. The height of the vertical support pillars can vary to span the vertical distance between the uneven ground and the desired plane in which the horizontal support members reside.
[0014] In one embodiment, the construction support device of the invention comprises a body member having a lower surface which serves as a support on a base such as a slab, footing, or pier block. The body member has one or more recess means arranged to receive horizontal beams and the like. The body member also has a central socket for receiving a vertical pillar or post. The recess means are disposed on each of four sides of the body member at 90 degrees apart and communicate with the central socket and the exterior, the pairs of recesses opposite from each other being aligned whereby construction beams or the like can be laid therein in edge and/or end relation. Also, in such embodiment, the construction device has fastener-receiving means therein for attaching a beam or beams and a pillar together, and also for attaching the assembly to the base. In another embodiment, side edges of the body member at the recess openings have downturned projections shaped on a rear portion thereof to frictionally fit on top of pier blocks for anchoring the body member against lateral shifting.
[0015] In another embodiment, the construction support device of the invention is a single cast, one-piece pier block which comprises a body member serving as a capable support on unprepared and unleveled building sites, having localized dips, slopes and random level areas therein. The body member has a single recess means molded into the top surface capable receiving horizontal deck surface support members and also capable of receiving the bottom end of a vertical wood post or pillar. The recess means can have particular dimensions for using conventional, existing lumber sizes and also such dimensions are such that the required integral strength of the block is maintained due to the manufacturing process and application without the necessity of using reinforcing bar steel or additional integral components. All of these features combine in a structural arrangement which automates and standardizes the manufacture and facilitates marketing, at a lower unit and resale cost, a deck that can be preplanned and pre-cut. Such a deck is simplified and inexpensive, and capable of construction by the average do-it-yourself homeowner who desires a deck on the unprepared and unleveled ground of a typical backyard.
[0016] The invention will be better understood and additional objects and advantages will become apparent from the following description taken in connection with the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
[0017] [0017]FIG. 1 is a top perspective view of a support device in accordance with a first embodiment of the invention;
[0018] [0018]FIG. 2 is a bottom perspective view of the device shown in FIG. 1;
[0019] [0019]FIG. 3 is a bottom perspective view of a construction support device in accordance with another embodiment of the invention.
[0020] [0020]FIG. 4 is a bottom perspective view of a construction support device in accordance with yet another embodiment of the invention.
[0021] [0021]FIGS. 5, 6, 7 and 8 are perspective views showing various applications of the device of FIG. 1 in association with structural building elements;
[0022] [0022]FIG. 9 is a perspective view of a construction support device which includes lateral stabilizing elements in accordance with a another embodiment of the invention.
[0023] [0023]FIG. 10 is a bottom perspective view of the construction support device of FIG. 9;
[0024] [0024]FIGS. 11 and 12 are perspective views showing various applications of the device of FIG. 9 in association with structural building elements;
[0025] [0025]FIG. 13 is a perspective view of a construction support device in accordance with another embodiment of the invention;
[0026] [0026]FIG. 14 is bottom perspective view of the construction support device shown in FIG. 13;
[0027] [0027]FIG. 15 is a top perspective view of the construction support device shown in FIG. 13;
[0028] [0028]FIG. 16 is a top plan view of the construction support device shown in FIG. 13;
[0029] [0029]FIG. 17 is a perspective view a construction support device in accordance with another embodiment of the invention;
[0030] [0030]FIG. 18 is a top perspective view of the construction support device shown in FIG. 17;
[0031] [0031]FIG. 19 is a top plan view of the construction support device shown in FIG. 17;
[0032] [0032]FIGS. 20 and 21 are perspective views showing various applications of the device of FIG. 17 in association with structural building elements;
[0033] [0033]FIG. 22 is a perspective view of a deck construction in accordance with the invention employing the construction support device shown in FIG. 17; and
[0034] [0034]FIG. 23 is a perspective view of another deck construction in accordance with the invention employing the construction support device shown in FIG. 17.
DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS
[0035] According to the present invention, a construction support device is provided which conveniently provides anchoring of a building element to a building site. As illustrated herein, the invention may be practiced in accordance with a first embodiment of FIG. 1, wherein the construction support device is securely attached to a concrete base or pier. The device of FIG. 1 can be inexpensively molded from plastic or stamped from metal and is simplified in its use and constructions.
[0036] Alternatively, the invention may be practiced in accordance with other embodiments, such as shown in FIGS. 13 and 17. There, the device is inexpensively poured from concrete together with a pier block to form a single cast, one-piece body. In either type of embodiment, the invention provides a new and advantageous support for securely seating construction members in either a horizontal or vertical orientation.
[0037] With reference first to FIGS. 5 through 8, the numeral 10 represents a base or pier block of conventional structure which is commonly used to support decks, carports, etc. This block is generally constructed of concrete and assumes different shapes. In most cases, the block is tapered to a lesser dimension toward the top. The top and bottom surfaces 12 and 13 , respectively, are flat.
[0038] FIGS. 1 - 8 illustrate a construction support device 14 in accordance with a first embodiment of the invention. Construction support device 14 which may be molded, stamped, or otherwise formed from a tough plastic or metal. The body member of the device 14 includes a flat bottom wall 16 and four identically shaped or symmetrical upright quarter sections 18 . Each of the sections 18 comprises four zig zag panels 18 a joined integrally at right angles. These symmetrical quarter sections are shaped to form a recess or opening 20 on each side, with oppositely located recesses being laterally aligned. Also, with this quarter section construction, a square central socket 22 is formed. Laterally aligned recesses 20 provide a pair of full width slots open at the sides.
[0039] Each of the panel sections 18 a has one or more apertures 24 therein provided to receive fasteners, to be seen hereinafter, for securement of building elements to the device 14 . As seen in FIG. 2, cutouts 26 are provided in the bottom wall 16 for reducing the weight of the member as well as for conserving material. Also, apertures 28 are provided in the wall 16 for secured attachment of the member 14 to a base, such as to a block 10 , a concrete slab, or other support means.
[0040] [0040]FIGS. 5, 6, 7 and 8 show various applications of the construction device 14 with building elements such as support members and pillars. FIG. 5 for example shows a horizontal decking surface support member 30 seated edgewise on the bottom wall 16 and extending fully through the device and out both side recesses 20 . FIG. 6 shows a support member 30 similarly supported as in FIG. 5 but also showing a right angle support member 32 extending through. a 90 degree side recess 20 and abutted against the support member 30 . FIG. 7 shows a vertical pillar 34 supported on the device 14 and fitted in the central socket 22 . FIG. 8 shows a pillar 34 similarly fitted in the socket 22 as in FIG. 7 but also showing side beams 32 extending in from all four of the side recesses. These members may simply be fitted in the respective recesses 20 or socket 22 . Preferably, however, secured attachment to the member 14 is accomplished by fasteners 36 extending through the apertures 24 . Also, device 14 can first be secured to the base member 10 by fasteners extending through the apertures 28 .
[0041] [0041]FIG. 3 is a bottom perspective view of a construction device 14 ′ having a bottom wall 16 and side walls 18 in an arrangement similar to that shown in FIGS. 1 and 2. This structure, however, is formed (such as by integral molding) with a plurality of depending foot members 38 . Four of such foot members are shown, as well as a central foot member, but any number of such foot members may be provided. In the FIG. 3 embodiment, the foot members 38 are hollow whereby long fasteners can be inserted down from the top through the wall 16 and into a base for secured attachment of the construction device 14 ′ to the base. FIG. 4 shows a structure similar to FIG. 3 except that the outer foot members 38 ′ are solid and not hollow. This embodiment may be employed in circumstances where it is not necessary to use vertical fasteners around an outer portion of the member.
[0042] FIGS. 9 - 12 illustrate an embodiment of the invention employing means for anchoring the body member against lateral shifting. In this embodiment, the body member 14 ″ is the same as that shown in FIG. 1 with respect to quarter panel sections 18 a and their formation of aligned recesses 20 and central socket 22 . To accomplish the lateral anchoring feature, the outermost panel section 18 a of each quarter section has a depending projection or lip 40 defined by a bottom wall portion 42 integral with side extensions 44 and a rear wall portion 46 . Rear wall portion 46 preferably angles outwardly toward the bottom to coincide with the angle of the side surfaces of pier block 10 . Reel wall portion 46 can extend at a desired angle, so as to have flush engagement with pier block sides of varying shape.
[0043] [0043]FIGS. 11 and 12 show application of the device 14 ″ of FIG. 9 to a pier block. In such arrangement, the device 14 ″ and the building elements therein are anchored or locked against lateral shifting. Fasteners extending through the bottom wall of the device are not necessary, although such fasteners can be used if desired. The cross dimension of the device between rear wall portions 46 can be preselected according to the size of the pier block so that a snug or frictional fit is provided.
[0044] Referring to FIGS. 13 - 21 , it will be seen that the device 14 may be made of concrete and integrally molded into the upper surface 12 ′ of a pier block such as pier block 50 . As shown in FIGS. 13 - 16 , the four upright quarter sections 18 ′ include zig-zag walls 18 a ′ which project from flat bottom wall 16 ′. Recesses 20 ′ define two perpendicular slot portions extending across the full width of upper surface 12 ′. Zig-zag walls 18 a ′ also define the four corners of a square central socket 22 ′.
[0045] With reference to FIGS. 17 - 21 , the concept of the invention can also utilize a pier block 50 ′ having a central socket portion 22 ′ and only two equal narrower recesses 20 ′ which extend inward from outer edges of two opposite sides of the top surface of the block 50 ′ and lead into the central socket portion, as best shown in FIG. 18. The two narrower recesses 20 ′ form but a single slot for receiving a horizontal decking surface support member 30 which also passes through the central socket portion 22 ′, as shown in FIG. 20. The central socket portion 22 ′ is for receiving vertical pillar supports 34 , independent of the two equal narrower recesses 20 ′, as shown by FIG. 21. The horizontal decking surface support members 30 and vertical pillar support members 34 being mutually exclusive to each other in the recess of block 50 ′ and also mutually interchangeable with each other in the same recess of the same block 50 ′.
[0046] The combination of slots and sockets allows a support in accordance with the invention to accommodate both vertical and horizontal beams, and is particularly well-suited for constructing decks on unprepared and unleveled building sites, two examples of those being shown in FIGS. 22 and 23. Such decks, by using the present block, are extremely simplified in their construction and can be supplied in pre-planned, pre-cut units. Other advantages also exist in the structure, as will be apparent hereinafter.
[0047] The deck shown in FIG. 22, designed by the numeral 52 , comprises the pier blocks 50 ′ as the base or ground support for the deck and can have such lumber as two-inch thick (1½ inch thick nominal) horizontal decking surface support member 30 received by the two equal narrower portions 20 ′, also passing through the central socket portion 22 ′ when the vertical pillar support 34 is not in the block 50 ′, those members 30 then supporting the deck surface structure 54 which is nailed in place and those blocks 501 directly receiving member 30 being on localized high or level ground within an unprepared and unleveled building site.
[0048] The deck shown in FIG. 23, designated by the numeral 56 , similarly uses some pier blocks 50 ′ as described above and also illustrates the use of some blocks 50 ′ as the base or ground support for vertical pillar supports 34 set in the central socket 22 ′ when the member 30 is not in block 50 , member 34 then providing support to member 30 when member 30 is not directly received by block 50 due to localized variations of the ground within an unprepared and unleveled building site. A deck support member 30 can also be fastened to a building 60 , as shown in FIG. 23.
[0049] The particular structure of the manufactured pier blocks 50 and 50 ′ makes it possible to construct an extremely simplified deck and one which can be pre-planned and pre-cut if desired. That is, such lumber as 2-inch thick deck support members 30 and vertical wood pillars 34 which can be used therewith comprise conventional existing material, namely, the two-inch thick deck support members 30 can comprise 2×6's or 2×4's and pillars 34 can comprise 4×4's.
[0050] The two equal narrower recesses 20 ′ can be 2 inches deep and have a width of 1¾ inches. This latter dimension would receive conventional finished 2×6's (1½ inches thick) and 2×4's (also 1½ inches thick). 2×6's and 2×4's have finished height dimensions of 5½ and 3½ inches, respectively, whereby the deck support members, whether 2×6's or 2×4's, project to a minimum necessary height above the top surface of the blocks 50 when seated in the recess for supporting the decking thereon.
[0051] The central socket portion 22 ′ can be 2 inches deep, similar to the recess portion 20 ′. Such socket is square, and can have dimensions of 3¾ inches for receiving a conventional finished 4×4 (3½ inches square) lumber support pillar. The vertical pillar becomes sufficiently fixed in socket portion 22 ′ in the block for deck construction purposes, as does the deck horizontal support member in the two narrower portions 20 ′, also being within the central socket portion 22 ′ when the member 34 is not in the block 50 , for lateral stability.
[0052] Pier blocks 50 and 50 ′ are designed to provide support to a deck on unleveled or unprepared building sites with no additional components required. For this purpose, the blocks 50 and 50 ′ are tapered to a larger dimension toward the bottom. The top and bottom surfaces are flat and square. The enlarged bottom surface allows the block to serve as its own footing. When two of such recesses 20 ′ are provided, they are standardly aligned across the block. Furthermore, the width of these recesses is less than one-third the width of the block at the top, thus maintaining lateral integral strength of the block. This arrangement maintains a strong concrete block without the necessity of re-bar reinforcement and thus contributes to manufacture of a pier block and deck structure in a pre-planned and pre-cut unit which is also sufficiently simplified in its use, standardized in its manufacture, and sufficiently inexpensive for deck construction by the average do-it-yourself homeowner.
[0053] Since the recess can be two inches deep, the recesses of the pier blocks 50 and 50 ′ of FIGS. 13 and 17 automatically and non-mechanically center the horizontal decking surface support member 30 and vertical pillars 34 in the pier block (FIGS. 20 and 21) and automates connection and securement of these support members to the pier block for deck constructions 52 and 54 shown in FIGS. 22 and 23. Mounted engagement of the horizontal surface support members and vertical pillars with the block is accomplished without metal-brackets or embedded connectors thus allowing individual blocks of a deck construction on unleveled and unprepared building sites to be adjusted without the need of any disassembly of the deck (i.e. removing bolts, nails or screws). Also, the recess of the pier blocks 50 and 50 ′ maintains horizontal and vertical members in parallel which is critical in construction of the deck.
[0054] It is to be understood that the forms of our invention herein shown and described are to be taken as preferred examples of the same and that other changes in the shape, size and arrangement of parts may be resorted to without departing from the spirit of our invention or the scope of the following claims. | A deck construction including a plurality of supports for anchoring deck construction elements to a building site. The supports include a body (which may be an integrally molded concrete pier) having upper and lower portions. The upper portion includes at least one slot for seating a horizontally oriented construction member. The slot includes a center socket portion having four extended corners for seating the bottom end of a vertically oriented construction member. The slot and center socket are defined by connecting wall portions which may be integral to the body or may be of plastic or metal and suitable secured to the body. In some cases, two mutually perpendicular slots are provided. | 4 |
[0001] This application claims priority to U.S. patent application Ser. No. 61/095,780, filed Sep. 10, 2008.
BACKGROUND OF THE INVENTION
[0002] The invention relates generally to razors and, more specifically, to a razor having an integrated brush for cleaning of the razor during and after use.
[0003] Razors are in wide use for personal grooming. The majority of such razors have a handle to one end of which is attached a head member which holds one or more razor blades. Often, the head member is releasably attached to the handle so that replacement heads with fresh razor blades can be substituted when the existing blades become dull. A problem that exists with these razors is that hair, skin cells, soap or shaving cream used in the shaving process, and other materials that may be present on the skin, become trapped on the razor blades or in the head member resulting in reduced effectiveness of the razor and perhaps shortening the useful life of the razor or head member.
[0004] One solution to removing the hair and other materials from the head member and razor blades is to displace the hair and other materials by passing a brush over the head member and razor blades. Known brushes are separate articles from the razor and therefore must be purchased separately from the razor, are stored separately so that the brush may not always be accessible when the razor is used, and may become permanently separated, for example if the brush is misplaced or forgotten.
SUMMARY OF THE INVENTION
[0005] The present invention consists of a combination razor and brush personal care product wherein the brush is retained when not in use inside the handle of the razor component. The brush component consists of a handle on one end of which is mounted a brush head. The handle of the razor component is hollow and the brush component is sized to slide longitudinally inside the handle of the razor component where it is releasably retained until withdrawn by a user to clean the razor component after use with the brush component. In a preferred embodiment, the brush component is releasably secured to a base member that has screw threads for engagement corresponding screw threads on the end of the handle of the razor component opposite the end with the razor head member so that the brush component can be extracted from the razor component by unscrewing of the base member.
[0006] Another aspect of the invention is to provide a replacement product packaging that includes new razor head member and/or blades combined together with a new brush component so that a user can easily and conveniently maintain the razor and brush combination product of the present invention.
BRIEF DESCRIPTION OF THE DRAWINGS
[0007] FIG. 1 is an elevational view of an embodiment of the razor and brush combination of the present invention.
[0008] FIG. 2 is a cross-sectional view taken along line 2 - 2 of FIG. 1 .
[0009] FIG. 3 is an enlarged, detail cross-sectional view showing the structure of a preferred embodiment for releasably attaching the brush component to a base member.
[0010] FIG. 4 is a plan view of a package of replacement blades and brush component of the present invention.
DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS
[0011] Illustrated in FIG. 1 , generally at 10 , is a razor and brush combination product of a preferred embodiment of the present invention. The combination product 10 includes a handle 12 , a razor head member 14 attached to a first end of the handle 12 , and a base member 16 releasably attached to a second end of the handle 12 . Preferably, the exterior of the handle 12 has a plurality of recesses 18 to provide for comfortable and secure grasping of the combination product 10 by a user.
[0012] A brush component 20 is releasably retained inside the handle 12 ( FIG. 2 ). The brush component 20 includes a brush handle 22 and a brush head 24 mounted on a first end of the brush handle 22 . The base member 16 is removable attached to the handle 16 by a cooperating set of screw threads 26 and 28 on the interior or the base member and the exterior of the handle 16 , respectively. The brush component 20 is releasably secured to the base member 16 . In a preferred embodiment, the main, central section of the brush handle 22 has a round profile for comfortable grasping by a user. The second end of the brush handle 22 includes a reduced profile, generally at 30 ( FIG. 3 ). A corresponding recess 32 is formed in the base member 16 so that the second end 30 of the brush handle 22 can be inserted and retracted from the base member 16 . In a preferred embodiment, a detent ridge 34 is formed in the recess 32 and a corresponding detent depression 36 is formed in the second end 30 of the brush handle 22 . The detent ridge 34 and detent depression 36 cooperate to allow a user to push the brush handle 22 into the base member 16 , forcing the detent ridge 34 into the detent depression 36 whereupon the brush handle 22 is releasably attached to the base member 16 , but can be readily detached by a user by forcefully separating the brush handle 22 from the base member 16 . In a preferred embodiment, the second end 20 may have a non-circular profile so that it does not rotate inside the base member 16 .
[0013] In use, a user will shave with the combination product 10 and then use the brush component 20 to clean the razor component. Access to the brush component 20 is made by unscrewing the base member 16 from the handle 12 and then retracting the brush component 20 from inside the handle 12 by withdrawing it longitudinally. Once the cleaning process in complete, the brush component is returned inside the razor handle 12 by inserting it longitudinally and then screwing the base member 16 onto the handle 12 . It is preferred that the bush head 24 be received inside the handle 12 in a close fit so as to limit movement and rattling of the brush component 20 inside the handle 12 . Obviously, the fit should not be so close that the brush component 20 is difficult to insert or withdraw and also should not be so close that the force required to withdraw the brush component is greater that the force required to retract the brush handle 22 from the base member 16 .
[0014] The brush head 24 , as well as the razor head member 14 , will wear with use and need to be replaced. A convenient package for maintaining the combination product 10 is illustrated generally at 38 in FIG. 4 . It includes in a single package replacement razor head member 40 and a replacement brush component 42 .
[0015] The foregoing description and drawings comprise illustrative embodiments of the present inventions. The foregoing embodiments and the methods described herein may vary based on the ability, experience, and preference of those skilled in the art. Merely listing the steps of the method in a certain order does not constitute any limitation on the order of the steps of the method. The foregoing description and drawings merely explain and illustrate the invention, and the invention is not limited thereto, except insofar as the claims are so limited. Those skilled in the art that have the disclosure before them will be able to make modifications and variations therein without departing from the scope of the invention. | A combination razor and razor brush is disclosed. The brush for cleaning the razor during and after use of the razor is releasably retained inside a hollow handle of the razor so that the brush is always readily accessible. | 1 |
BACKGROUND
[0001] An auxiliary power unit (“APU”) creates pneumatic power or electrical power to run the air conditioning system, start the main engines and run other accessories on an aircraft. An APU is important to use because the aircraft is not required to use ground power for aircraft air conditioning, to provide electrical power or start the main engines.
[0002] APU Fuel Controls Units (FCUs) are typically shaft driven from the APU gearbox and the fuel is metered based on the APU load by a metering device (i.e., servo valve). Some APU FCUs are driven by a variable speed electrical motor that attempts to meter the fuel demanded by the APU by changing the speed of the pump motor.
SUMMARY
[0003] An example control disclosed herein for providing the fuel to an auxiliary power unit (“APU”) includes a constant speed electrical motor, a first pump driven by the motor; and, a second pump driven by the motor wherein the electric motor, the first pump and the second pump provide fuel at sufficient pressure to start the APU.
[0004] According to a further example provided herein a method for providing fuel to an APU includes providing a constant speed electrical motor; providing a first pump driven by the motor; providing a second pump driven by the motor; and driving the electric motor at a constant speed such that the first pump and the second pump provide fuel at sufficient pressure to start and to operate the APU.
[0005] These and other features of the present disclosure can be best understood from the following specification and drawings, the following of which is a brief description.
BRIEF DESCRIPTION OF THE DRAWINGS
[0006] FIG. 1 shows a schematic view of a prior art APU fuel system.
[0007] FIG. 2 is a schematic view of a simple and reliable APU fuel system as described herein.
DETAILED DESCRIPTION
[0008] Referring to FIG. 1 a prior art, fuel control unit (“FCU”) 10 for an APU 15 is shown. Generally, fuel must be pumped from a fuel tank 17 to a first pressure and then a higher pressure for use at APU fuel nozzles 20 . The higher pressure is required to provide proper atomization for fuel entering the nozzles 20 .
[0009] Fuel passes from the fuel tank 17 to a boost stage pump 25 . The boost stage pump 25 is driven off an APU gearbox (not shown) and pressurizes the fuel and sends it to a fuel filter 30 via lines 35 and 40 . After passing through the fuel filter 30 , the fuel is delivered to the high pressure pump 45 via line 50 . The boost stage pump 25 and the high pressure pump 45 are ganged together by shaft 55 . After passing through the high pressure pump 45 , the fuel is at a proper pressure for delivery to the nozzles 20 . The fuel then passes through a servo valve 60 which is controlled by a controller 65 to meter flow through lines 70 and 75 . A valve 67 , also controlled by controller 65 , is disposed downstream of the servo valve 65 and acts as an emergency shut off. The fuel lines 70 and 75 include a flow divider 90 to apportion fuel to a simplex nozzle 80 or duplex nozzle 85 within the APU 15 . The flow divider 90 , as is known in the art, uses a ball valve 97 that gives way according to the fuel pressure against the spring 95 to provide fuel to the simplex nozzle 80 or to the duplex nozzle 85 .
[0010] Fuel passing through the high pressure pump 45 may be diverted if the pressure becomes too high through the pressure relief valve 100 , which again is a standard ball valve to recirculate fuel through the fuel filter 30 . If the fuel filter 30 becomes clogged and pressure backs up there, fuel may be diverted around the fuel filter 30 through a pressure relief valve 105 via lines 40 , 110 and 115 .
[0011] During start up of the APU 15 , the shaft driven FCU 10 needs to generates enough flow capacity with relatively high pressure for good atomization at the nozzles 20 . However, when an FCU 10 is physically sized for the start condition, such an FCU 10 will generate considerably more flow capacity than needed when the APU 15 is running at normal operating speed. This excess fuel flow which is typically about 300%-500% of what is needed, is recirculated back to the high pressure pump 45 and the boost stage pump 25 through the pressure relief valve 100 back through lines 35 , 40 and 50 . The amount of fuel recirculation back into the inlet of the pump increases even more when the APU 15 is operating at no load at high altitude conditions. This in turn may cause fuel overheating that may be difficult to resolve. Shaft driven FCUs also contain seals (not shown) at the gearbox interface. In time due to rubbing action, these seals will wear and can cause external oil and/or fuel leakage that impact the safety and reliability. An FCU 10 with external leakage will then need to be replaced.
[0012] Note that the FCU 10 shown in FIG. 1 may provide fuel flows that are 300% to 500% higher than required by the APU 15 , making it an inefficient design when it comes to power consumption.
[0013] Further, prior art systems (not shown) have been designed with variable speed electrical motors (not shown) that drive pumps (not shown) such that fuel flow is metered by speeding and slowing the motor driving the pump. However, such systems require expensive motors and sophisticated motor controllers for precise motor speed control with very fast response time to be able to manage the rapid required transient response necessary for an APU.
[0014] Referring now to FIG. 2 , instead of driving the shaft 55 off an APU gearbox (not shown), the shaft 55 is now driven by a constant speed electric motor 200 . The motor 200 may be semi-hermetic with no dynamic seals to wear. Since during APU starting, the electric motor 200 of FCU 210 is at 100% speed and independent of the actual APU speed, the physical size of the pump 25 , 45 can be substantially smaller as compared to the shaft driven FCU 10 . The FCU 210 is typically sized to deliver the maximum fuel demanded by the APU 15 plus a slight margin for engine/pump deterioration. This margin may be as high as 20% or more. The electric motor 200 may be AC induction, DC brushless, switch reluctance or other types. The electric motor 200 may be single speed or a multiple speed motor. The electric motor 200 may be low voltage or high voltage and might be powered during the APU 15 start by the aircraft battery or the APU generator and may be designed to have its input power switched to another source such as an APU driven alternator or other external power. Prior to APU 15 cranking for the start, the electric motor 200 starts to full speed within seconds and generates the proper fuel pressure and flow demanded by the APU controller 65 for proper combustion ignition through the nozzles 85 . During the normal operation, the excess flow will be recirculated similar to the existing FCUs. However, this quantity of recirculation is substantially less than the existing mechanically driven pumps 25 and 45 as shown in FIG. 1 . Moreover, this FCU 210 does not require a complicated variable speed motor or a motor controller with very fast response time for precise motor speed control. If the APU 15 is running by using FCU 10 that utilizes the gearbox driven boost stage pump 25 and high pressure pump 45 , the excess fuel flow may be over 300% to 500% of fuel flow needed, which is not only inefficient but also may cause fuel overheating when the fuel demand is low.
[0015] In contrast, the FCU 210 that uses the constant speed electrical motor 200 , the maximum over pumping at the same operating conditions is about 20%. As such, the drain on the APU 15 to drive the electric motor 200 is less than the power required to drive the shaft driven FCUs. The electric motor 200 , which is independent of APU speed, provides higher start reliability, better energy efficiency due to little recirculation during full APU speed, and no dynamic seals for enhanced reliability and safety. There is less drag on the APU gearbox during cold starts which increases APU start torque margin.
[0016] Although preferred embodiments have been disclosed, a worker of ordinary skill in this art would recognize that certain modifications would come within the scope of this disclosure. For that reason, the following claims should be studied to determine the true scope and content of this disclosure. | A control disclosed herein for providing fuel to an auxiliary power unit (“APU”) includes a constant speed electrical motor, a first pump driven by the motor; and, a second pump driven by the motor wherein the electric motor, the first pump and the second pump provide fuel at sufficient pressure/flow capacity to run the APU. | 5 |
CROSS REFERENCE TO RELATED APPLICATIONS
This is a continuation of application Ser. No. 819,507, filed Dec. 12, 1985, now abandoned, which in turn stems from PCT International Application No. PCT/JP85/00227, filed Apr. 23, 1985.
TECHNICAL FIELD
The present invention relates to an improved reaction vessel which is used to carry out an exothermic reaction of a mixed gas consisting of a plurality of elements in the presence of a solid catalyst, as in the case of a synthesis of methanol from hydrogen and a carbon monoxide (and carbon dioxide) gas.
BACKGROUND TECHNOLOGY
As reaction vessels of this type, there have been suggested ones involving means or structures for controlling the rise of a gas temperature resulting from an exothermic reaction during operation. FIG. 1 attached hereto exemplarily shows the effect of a temperature on a methanol equilibrium concentration in a methanol synthesis reaction, and as is definite from it, the methanol equilibrium concentration will be low along with the rise of the temperature, so that an economy of an industrial plant will be impaired. Therefore, the above-mentioned suggested reaction vessels have attempted to eliminate such a disadvantage. FIG. 1 above has been quoted from "Methanol", Nozawa, Vol. 46, No. 9, p. 507 (1982) and calculated values have been obtained by setting, to 4, a ratio of H 2 to CO in the reaction of CO+2H 2 →CH 3 OH. In this reaction, a reaction rate is limited even if a catalyst is employed, but naturally the reaction rate will be low with the fall of the temperature. Therefore, it is industrially preferred that the operation of the reaction vessel is carried out within a certain proper temperature range in view of catalyst performance. In the case of synthesizing methanol from a mixed gas containing hydrogen, carbon monoxide and carbon dioxide as major component materials by the use of a copper catalyst, the inventors of the present application have the understanding that a preferred temperature lies within the range of 220° to 280° C. and a preferred and economical pressure (total pressure) of the gas lies within the range of 50 to 300 kg/cm 2 •G, but these preferred ranges can vary dependent upon any future improvement in the catalysts used.
A known method for adjusting this temperature is disclosed in, for example, Japanese Patent Publication No. 38568/1982.
This known technique, as shown in FIG. 2, comprises causing a pressurized mixed gas, i.e., an unreacted gas A consisting of hydrogen, carbon monoxide, carbon dioxide and the like which has previously been heated to a suitable temperature, to flow through a catalyst filling reaction pipe 2 in a reaction vessel 1 upward from a lower position thereof in order to accomplish a methanol synthesis reaction, and getting rid of the resultant reaction heat via the latent evaporation latent heat of water, having a suitable pressure and a saturated temperature, which is brought into contact with the outer surface of the reaction pipe, whereby a temperature of the mixed gas in the reaction pipe is maintained in a suitable condition range. In FIG. 2, reference symbol B represents a reaction gas, and numerals 3 and 4 are water to be supplied and water vapor to be discharged, respectively. Practically, a number of reaction pipes can be disposed therein, but in FIG. 2, simplification is made for clarity.
In the case of the above known example, however, it is necessary to previously heat, by a heat exchanger, the feed gas which will be forwarded to the reaction vessel, which fact means that it is poor in economy. Further, as is definite from FIG. 3 which is a sectional view of the reaction pipe 2 in FIG. 2, the pipe 2 is packed with a grainy catalyst 4 in the form of a column, therefore the central portion of the catalyst layer 4 is so considerably away from the heat transmitting surface that a sufficient cooling (control of a reaction temperature of the gas, i.e, maintenance of an optimum temperature) is disadvantageously difficult to achieve.
The present inventors have already suggested a double pipe type exothermic reaction vessel by which the above-mentioned drawbacks are eliminated (Japanese Patent Application No 213724/1983), but the present invention intends to provide a further improved reaction vessel.
SUMMARY OF THE INVENTION
The present inventors have invented the following apparatus: A reaction pipe 2 is constructed in the form of a double pipe as shown in FIG. 4, and a circular space between an outer pipe 2' and an inner pipe 2" is packed with a grainy catalyst 4, so that the catalyst layer is thin. An outside surface of the outer tube 2' is cooled with cooling water and an inside surface of the inner tube 2" is cooled with an unreacted feed gas A so as to maintain a temperature of the gas at a proper level within the narrow temperature range in a direction across the catalyst layer and to simultaneously preheat the unreacted feed gas A. It has been found that such a constitution is advantageous for the control of the reaction temperature, leads to the effect of rendering needless a heat exchanger for preheating the unreacted feed gas, permits lowering a temperature at an inlet of the catalyst layer by mixing the unreacted feed gas preheated ascending through a central pipe with a cold unreacted feed gas, and can suitably adjust a temperature of the catalyst layer.
That is to say, the present invention is directed to a reaction vessel for an exothermic reaction which comprises a plurality of reaction pipes, central pipes disposed in the middle of the reaction pipes, and circular catalyst layers formed by packing circular spaces defined between the reaction pipes and the central pipes with a grainy catalyst, whereby an unreacted feed gas can be caused to flow through the central pipes upward from lower positions thereof and can be then caused to flow through the circular catalyst layers downward from upper positions thereof, the central pipes through which the unreacted feed gas flows being connected to one or more mixing chambers defined at an upper portion in the reaction vessel, the mixing chamber being provided with an inlet for allowing a cold unreacted feed gas to pass therethrough, which cold gas having a lower temperature than the unreacted feed gas coming out from the central pipes.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a graph showing a relation of pressure and temperature effect to an equilibrium concentration in a methanol synthesis reaction;
FIG. 2 is a vertical section of a conventional reaction vessel;
FIG. 3 is a horizontal section of the reaction vessel in FIG. 2;
FIG. 4 is a horizontal section of a reaction vessel along line 4--4 of FIG. 5, according to the present invention;
FIG. 5 is a vertical section of the reaction vessel according to the present invention; and
FIGS. 6 to 9 are vertical sections illustrating various embodiments of mixing chambers for the reaction vessel according to the present invention.
DETAILED DESCRIPTION OF THE INVENTION
The present invention will be described in detail in reference to accompanying drawings.
FIG. 5 shows one example of a structure of a reaction vessel according to the present invention. A reaction pipe 1 is fixed at the opposite upper and lower ends thereof by two circular plates 90 and a central pipe 3 is disposed in the middle of each reaction pipe 1. A circular space defined between the reaction pipe 1 and the central pipe 3 is packed with a grainy catalyst to form a circular catalyst layer 13. An unreacted feed gas 40 is delivered from the unreacted feed gas nozzle 5 and reaches lower the central pipes 3 through the branch ducts 6, 7 to a mixing chamber 8 defined at the upper portion in the reaction vessel. Another cold unreacted feed gas 9 is introduced into the mixing chamber 8 through a nozzle 14 and is mixed with the unreacted feed gas coming out through the central pipes 3, and the resultant mixed gas is then guided to the circular catalyst layers 13.
The gas is caused to pass through the circular catalyst layers 13 and then reaches, through outlets 10 of the catalyst layers 13, a gathering chamber 19 defined at a lower portion in the reaction vessel, and the gas is afterward caused to run out through a reaction vessel outlet nozzle 12 as a reaction gas 11 from the reaction vessel.
A boiling liquid 16 for cooling the reaction pipe 1 from the outside surface thereof is introduced into the reaction vessel through an inlet nozzle 15 and discharged therefrom through an outlet nozzle 18 of the reaction vessel.
FIG. 6 shows another embodiment of the mixing chamber regarding the present invention. In this drawing, the unreacted feed gas 41 is heat exchanged with the circular catalyst layers 13 while flowing upward through the central pipes 3 in order to be heated and is then forwarded to the mixing chamber 8 through central pipe outlets 3'. On the other hand, the other cold unreacted feed gas 9 is introduced into the reaction vessel through the nozzle 14 and is hit against a dispersing plate 20 in order to be dispersed, and it is then caused to go into a dispersing chamber 8'. The gas is further forwarded via a dispersing plate 21 to the mixing chamber 8, where it is then mixed with the preheated unreacted feed gas 3'. The resultant mixed gas is caused to pass through a dispersing plate 22 in order to be mixed more uniformly and is guided to the catalyst layers 13 via a dealing chamber 23. In this case, the two dispersing plates 20 and 21 for the unreacted feed gas 9 are exhibited in this drawing, but the only one dispersing plate may be disposed.
FIG. 7 shows still another embodiment of the mixing chamber, and in this embodiment, the unreacted feed gas 41 is heat exchanged with the circular catalyst layers 13 while flowing upward through the central pipes 3 and is then forwarded to the mixing chamber 8 via the central pipe outlets 3'. On the other hand, the other cold unreacted feed gas 9 is introduced into the reaction vessel via the nozzle 14 and is then caused to descend through a mirror plate space 24. Afterward, the gas 9 is guided via a space 26 confronted with a partition 25 to a mixing chamber 8, where it is mixed with the preheated unreacted feed gas 3'. The thus uniformly mixed gas is caused to pass through a mixing pipe 27 in order to be mixed more uniformly during its passage, and the gas is then guided to the dealing chamber 23 and afterward the catalyst layers 13.
FIG. 8 shows a further embodiment of the mixing chamber, and in this embodiment, the unreacted feed gas 4 is heated by heat exchange with the circular catalyst layers 13 while flowing upward through the central pipes 3 and is introduced into the mixing chamber 8 via the central pipe outlets 3'. On the other hand, the other cold unreacted feed gas 9 is introduced into the reaction vessel through the nozzle 14 and is then jetted via a dispersing header 28 into the mixing chamber 8, where it is mixed with the preheated unreacted feed gas 3'. The thus mixed unreacted feed gas is caused to pass through the dispersing plate 20 in order to be mixed more uniformly at this time and is then introduced via the dealing chamber 23 into the catalyst layers 13.
FIG. 9 shows a still further embodiment of the mixing chamber, and in this embodiment, the unreacted feed gas 4 is heated by heat exchange with the circular catalyst layers 13 while flowing upward through the central pipes 3 and is forwarded to the mixing chamber 8 via the central pipe outlets 3'. On the other hand, the other cold unreacted feed gas 9 is introduced into the reaction vessel through the nozzle 14 and is hit against a baffle 6, so that it is dispersed in the mixing chamber 8, where it is mixed with the preheated unreacted feed gas 3'. The thus mixed material gas is caused to pass through a mixing pipe 27 in order to be mixed more uniformly during its passage and is then guided to the dealing chamber 23 divided by a partition 25 and afterward the catalyst layers 13.
As a matter of course, in the one reaction vessel, a plurality of the reaction pipes packed with the catalyst may be disposed, but the one central pipe is disposed to the one reaction pipe. Each central pipe may be connected to one end of a connecting pipe, another end of which may be connected to a header. The connection of the central pipe with the connecting pipe and the connection of the header with the connecting pipe are suitably carried out in an optional manner such as a flange structure (bolt join) so as to be easily detached when needed.
POSSIBILITY OF INDUSTRIAL UTILIZATION
In contrast with the prior application (Japanese Patent Application No. 213724/1983; "double pipe type exothermic reaction vessel"), the present invention permits directly controlling a temperature of the unreacted feed gas at the circular catalyst layer inlets by introducing the cold gas into the upper portion of the reaction vessel, and can accomplish a more effective control particularly even for an abrupt temperature rise at the catalyst layer inlets at an early operation stage in which a catalyst activity is very great.
For this reason, the maximum temperature in the catalyst layer can be caused to fall without lowering a pressure of the boiling liquid which is a cooling medium, and a life span of the used catalyst particularly in the vicinity of the inlets can thus be prolonged.
As is definite from the foregoing, according to the present invention, the reaction temperature can be maintained within the range of proper levels in order to heighten a reaction efficiency, i.e., a concentration of the reaction product at a reaction vessel outlet, which fact is industrially very valuable. In addition thereto, in the reaction vessel of the present invention, the central pipes can be vibrated by means of a vibrator at the time of a catalyst packing operation, whereby the catalyst can be packed closely and firmly without leaving spaces therein and a pressure loss of each catalyst layer can thus be uniformized (uniformization of space velocity), which facts are also great advantages of the present invention.
In the case of "the double pipe type exothermic reaction vessel" of Japanese Patent Application No. 213724/1983 which has already been invented by the present inventors, the unreacted feed gas is introduced into the central pipes from their upper ends and is then discharged from the central pipes through the lower ends and the gas is also caused to flow through the circular catalyst layers downward from their upper ends in order to accomplish the reaction during its flow. Therefore, if a diameter of each catalyst grain is small and a space velocity of the gas is too high, the catalyst grains will be streamed and will consequently undergo mechanical wear. As a result, the pressure loss in each reaction pipe will be ununiformed and the space velocity will also be ununiformed, which fact will tend to deteriorate the performance. However, the present invention has the constitution that the gas is caused to flow through the catalyst-packed portions downward from above, and thus the occurrence of the above-mentioned problem can be restrained perfectly even if the space velocity is high.
As described above, the reaction vessel of the present invention can achieve a gas phase exothermic reaction by the use of the grainy solid catalyst and thus has an industrially great value. Besides, the present invention can be applied to uses other than the synthesis of methanol, and a composition of the gas, a kind and shape of the catalyst, a space velocity, a pressure and a temperature are not particularly restricted.
Although omitted in FIG. 5, there are known a structure of disposing the central pipes in the middle of the reaction pipes and a disposition, at the lower circular plate, of a member for preventing the catalyst from dropping, and the present invention does not intend to limit these constitutions. Also with regard to a diameter and length of each reaction pipe packed with the catalyst, a diameter and length of each central pipe, fins fixed on pipe surfaces to increase a heat transfer area, a formation of grooves, a material of the pipes and a shape of the baffle, they are not specified in the present invention. They are decided in accordance with many factors such as a pressure, a composition of the gas, a temperature, an amount of the reaction heat and a performance of the catalyst, and in the present invention, these factors are not restricted especially.
As described above, in the present invention, a part of the reaction heat of the gas which is reacting in the catalyst layers is given to the unreacted feed gas flowing through the central pipes by a heat transfer via walls of the central pipes in order to preheat the unreacted feed gas and to simultaneously cool the gas in the catalyst layers (temperature control). These effects satisfy the requirement of maintaining a temperature of the gas in the central pipes at a lower level than a reaction temperature. The remaining reaction heat is removed as an evaporation latent heat of water by a heat transfer to the pressurized water having a saturated temperature which is brought into contact with the outer surface of the reaction pipes, and the pressurized water vapor generated is taken out from the reaction vessel and is then used for another application. The heat transfer and the removal function of the reaction heat will not be accomplished naturally, if the temperature of the pressurized water is not set to a lower level than the reaction temperature. Accordingly, a pressure (saturated temperature) of the pressurized water should be decided suitably on the basis of a necessary amount of the heat to be transferred and an aimed reaction temperature.
As understood from the above, the present invention is desirable as a reaction vessel, for example, for methanol synthesis, which carries out the exothermic reaction of the gas by the use of the solid grainy catalyst and which requires the control of the reaction temperature to enhance its performance. Additionally, in the case of the present invention, since the structure is simple, there can be easily carried out design, manufacture, inspection, repair, catalyst filling and catalyst takeout, and the stability of operation is also excellent, and thus it can be believed that the present invention has an industially great value.
TEST FOR COMPARISON
According to the embodiment shown in FIG. 6, an example and comparative examples were carried out. With regard to a composition of a feed material gas, a space velocity of the feed material gas and a reaction pressure, they were common to the example and the comparative examples.
______________________________________Composition of feed material gas (mole %)______________________________________CO.sub.2 5.8CO 9.6H.sub.2 68.4CH.sub.4 15.2N.sub.2 0.6H.sub.2 O 0.0Methanol 0.4Space velocity of feed gas 6500 1/HRReaction pressure 96 kg/cm.sup.2 · G______________________________________ Compar. Compar. Example Example 1 Example 2______________________________________Quench operation Done Not done Not doneRate (%) of quench gas 37 0 0amount to feed gas amountabove inlets of allcatalyst layersTemp. (°C.) of material gas 150 150 150at inlet of central pipeTemp. (°C.) of material gas 272 282 267at outlet of central pipeTemp. (°C.) of quench gas 150 -- --Temp. (°C.) of mixed gas 227 -- --Temp. (°C.) at inlet of 227 282 267catalyst layerMaximum temp. (°C.) in 280 315 280catalyst layerTemp. (°C.) at outlet of 250 250 235catalyst layerTemp. (°C.) of saturated 260 260 245pressurized waterPressure (kg/cm.sup.2 · G) of 47 47 36generated saturatedwater vapor______________________________________
In the example of the present invention, the unreacted feed gas coming out through the central pipes was mixed with a quench gas which was the cold unreacted feed gas in order to lower a temperature of the resultant mixed gas at the inlets of the catalyst layers. The effects thus obtained are set forth in the above table. In this Example, saturated pressurized water was used as a boiling liquid for cooling.
In Comparative Example 1, a temperature of the mixed gas at the inlets of the catalyst layers was 282° C. and a maximum temperature of the mixed gas in the catalyst layers was as high as 315° C. Especially at an early operation stage in which a catalyst activity is good, a temperature of the gas in the catalyst layers preferably is lower on the whole, since a life span of the catalyst can be prolonged. For this reason, in Comparative Example 2, the maximum temperature of the catalyst layers was maintained at 280° C. by lowering a pressure of the pressurized water which was a cooling medium. However, the present invention permits retaining the same maximum temperature as in Comparative Example 2 without lowering the pressure of the pressurized water.
The pressurized water which has been evaporated by a reaction heat is taken out in the form of water vapor from the reaction vessel and can be effectively utilized as a variety of energy sources, but in this case, needless to say, the higher the pressure of the water vapor is, the greater its value as energy is.
Therefore, it is clearly beneficial that the maximum temperature of the catalyst layer can be maintained at a predetermined level or less even at the early stage involving a good catalyst activity by employing the quench gas without lowering the pressure of the vapor to be recovered, as in Example of the present invention. | A reaction vessel has a catalytic core, with an inlet for a first gas and for a second gas. The first and second gasses react in an exothermic reaction during passage through the catalytic core. The first gas passes through conduits which extend through the catalytic core, so as to be preheated and also so as to cool the catalytic core so that the catalyzed reaction proceeds in a preferred temperature range. The gasses are mixed at one end of the vessel in a mixing chamber, and are drawn through the catalytic core into a gathering chamber, from which the reacted gasses exit. A cooling chamber is provided for introduction of a cooling fluid about the periphery of the catalytic core, for drawing away any excess heat during operation. | 1 |
RELATED APPLICATION
[0001] This application claims priority from British Application Number 0122153.0, filed Sep. 13, 2001.
[0002] 1. Field of Invention
[0003] This invention relates to a catalyzed urea formaldehyde binder for use in abrasive articles, a method of making the binder, abrasive articles made therewith and in particular to coated abrasive articles and to a method of making coated abrasive articles.
[0004] 2. Discussion of Related Art
[0005] Coated abrasive articles generally contain an abrasive material, typically in the form of abrasive grains, bonded to a backing via of one or more adhesive layers. Such articles usually take the form of sheets, discs, belts, bands, and the like, which can be adapted to be mounted on pads, wheels or drums. Abrasive articles can be used for sanding, grinding or polishing various surfaces of, for example, steel and other metals, wood, wood-like laminates, plastic, fiberglass, leather or ceramics.
[0006] The backings used in coated abrasive articles are typically made of paper, polymeric materials, cloth, vulcanized fiber or combinations of these materials. A common type of bond system includes a make coat, a size coat, and optionally a supersize coat. The make coat typically includes a tough, resilient polymer binder that adheres the abrasive particles to the backing. The size coat, which also typically includes a tough resilient polymer binder that may be the same as or different from the make coat binder, is applied over the make coat and abrasive particles to further reinforce the particles. The supersize coat, including one or more antiloading ingredients or perhaps grinding aids, may then be applied over the size coat if desired.
[0007] In a typical manufacturing process, a coated abrasive article is made in a continuous web form and then converted into a desired construction, such as a sheet, disc, belt, or the like. Binders for the purpose of adhering the abrasive granules to the backing include the traditional phenolic resins, urea-formaldehyde resins, hide glue, varnish, epoxy resins, and polyurethane resins, or more recently a class of radiation cured crosslinked acrylate binders; see, e.g., in U.S. Pat. No. 4,751,138 (Tumey, et al.) and U.S. Pat. No. 4,828,583 (Oxman, et al.).
[0008] High performance coated abrasive articles have traditionally used phenolic size resins. Such resin systems suffer from the disadvantage that they require high temperatures for a prolonged time for optimum curing. This prevents the use of such resins with some polymeric backings either because they will not withstand the cure temperature or because the high cure temperature may result in dimensional instability of the coated sheet, e.g., curling upon cooling to ambient temperature. Additional disadvantages are that phenolic resins tend to be more expensive and have more undesirable emissions compared to urea-formaldehyde resin systems.
[0009] Urea formaldehyde (UF) was first patented for use as an adhesive for coated abrasives by 3M Company (“3M”) in the mid 1930's (Great Britain Pat. No. 419,812). Since that time a number of different coated abrasive products have been made with acid catalyzed UF resins. Today, the two most common catalysts used with UF resins are aluminum chloride (AlCl 3 ) and ammonium chloride (NH 4 Cl).
[0010] Urea-aldehyde resins have enjoyed great success in coated abrasives. However, the need to reduce the use of solvents and unreacted reactants which contribute to release of volatile organic hydrocarbons (VOC) in the process of making coated abrasives and the need to increase the quality of the abrasives while maintaining or increasing their level of performance are challenging the industry.
[0011] When aluminum chloride is used as the catalyst, a higher temperature than normal must be used to cure the urea-aldehyde resin, which in turn leads to curling of edges of the coated abrasive. Also, the gel time, pot life and peak exotherm temperatures are all dependent on the concentration of the aluminum chloride. Consequently, there is a trade-off between aluminum chloride concentration and curing conditions, especially with low free-aldehyde UF resins.
[0012] Unlike aluminum chloride catalysis, the gel time, pot life and peak exotherm temperatures are all independent of the ammonium chloride concentration. However, the activity (ability of the catalyst to catalyze the reaction) of ammonium chloride is dependent on the free formaldehyde concentration in the binder precursor composition. With low free aldehyde resins, the ammonium chloride does not activate the condensation reaction very readily until a sufficient temperature is reached. However, as mentioned above, increased temperature tends to curl the edges of the coated abrasive and does not render performance improvements.
[0013] U.S. Pat. No. 5,611,825 (Engen, et al.) reports coated abrasives comprising a backing coated on at least one major surface thereof with an abrasive coating comprising a binder and abrasive particles. The binder is comprised of a solidified urea-aldehyde resin, the solidified urea-aldehyde resin being derived from a binder precursor comprising a urea-aldehyde resin having a low free aldehyde content and a co-catalyst. The co-catalyst is a catalyst consisting essentially of a Lewis acid, preferably aluminium chloride or an organic amine salt or an ammonium salt, preferably ammonium chloride. Preferred linear organic amine salts are those selected from the group of compounds having the general formula:
(X 31 ) + H 3 N(CH 2 ) n NH 3 + (Y − )
[0014] wherein X and Y are halide atoms that may be the same or different and n is an integer ranging from about 3 to about 10. An example of such a linear organic amine salt found useful is the dichloride salt of hexamethylene diamine, obtained by the acidification of an aqueous solution of hexamethylene diamine with hydrochloric acid (HCl). One branched chain organic amine salt found useful is that known under the trade designation “DYTEK-A,” available from E. I. duPont de Nemours & Co., Wilmington, Del., which is commonly known as 2-methyl-pentamethylene diamine.
[0015] Although urea-formaldehyde resins have been used as make, size and supersize resins in coated abrasives they are generally not able to match the performance of coated abrasive made with phenol-formaldehyde resins.
SUMMARY OF THE INVENTION
[0016] It has now been found that certain urea formaldehyde resin systems can provide comparable performance to phenol formaldehyde resins when used in the production of coated abrasives. According to the present invention there is provided a coated abrasive article comprising a backing having at least one major surface, a plurality of abrasive grains bonded to at least a portion of the one major surface of the backing by at least one binder, wherein the binder comprises an urea formaldehyde resin precursor cured in the presence of a sole catalyst which consists essentially of at least one salt of an acid with a diamine of the formula:
H 2 N—R—NH 2
[0017] in which R is an alkylene group of 3 to 10 carbon atoms, wherein the acid is selected from the group consisting of hydrochloric, citric, nitric, sulphuric, acetic, phosphoric and combinations thereof.
[0018] In a further aspect, the invention provides a method of making a coated abrasive which comprises coating a major surface of a backing with a plurality of abrasive grains and a binder comprising a urea formaldehyde resin precursor solution and a solution of a sole catalyst which consists essentially of at least one salt of an acid with a diamine of the formula:
H 2 N—R—NH 2
[0019] in which R is an alkylene group of 3 to 10 carbon atoms, wherein the acid is selected from the group consisting of hydrochloric, citric, nitric, sulphuric, acetic, phosphoric and combinations thereof, and curing the urea formaldehyde resin precursor. Curing is typically accomplished by heating at a temperature of at least 60° C., preferably at a temperature in the range of about 75° C. to 140° C., or a temperature in the range of 80° C. to 90° C. for 40 minutes or less, temperature in the range of 115° C. to 125° C. for less than 10 minutes.
[0020] In a further aspect, the invention provides a binder which is useful in abrasive products comprising urea formaldehyde precursor resin cured in the presence of a sole catalyst which consists essentially of at least one salt of an acid with a diamine of the formula:
H 2 N—R—NH 2
[0021] in which R is an alkylene group of 3 to 10 carbon atoms, wherein the acid is selected from the group consisting of hydrochloric, citric, nitric, sulphuric, acetic, phosphoric and combinations thereof
[0022] In a further aspect, the invention provides a method of making a binder comprising mixing components comprising an aqueous solution of a urea-formaldehyde resin precursor; and a sufficient quantity of an aqueous solution of a sole catalyst to initiate cross-linking of said urea-formaldehyde resin precursor of a catalyst consisting essentially of at least one salt of an acid with a diamine of the formula:
H 2 N—R—NH 2
[0023] in which R is an alkylene group of 3 to 10 carbon atoms, wherein the acid is selected from the group consisting of hydrochloric, citric, nitric, sulphuric, acetic, phosphoric and combinations thereof to provide a mixture; and heating said mixture to provide said binder.
[0024] As used herein, the term “sole catalyst” means only one catalyst is employed, that being the diamine salt catalyst as defined above.
[0025] The term “catalyst” refers to the diamine salt defined above and its ability to initiate polymerization of urea-formaldehyde resin precursor to provide a cured urea-formaldehyde resin which is cross-linked.
[0026] It has been found that the use of particular catalysts which are salts of a lower alkaline diamine with an acid in combination with urea formaldehyde resin precursors provide a binder system suitable for use in coated abrasives which may provide comparable and sometimes superior physical properties to the use of phenolic resins systems while allowing low cure temperatures and shorter cure times. The cost of the urea formaldehyde binder system is significantly less than the cost of a phenolic resin system and the urea formaldehyde resin may have in excess of 90% less emissions than a phenolic resin system.
[0027] The catalyst used in the invention is derived from an alkaline diamine containing from 3 to 10 carbon atoms. Preferably, the diamine is 1,2 hexamethylene diamine or octadiamine. The acid is selected from hydrochloric, citric, nitric, sulphuric, acetic and phosphoric acids. Phosphoric acid is preferred. The preferred catalyst is 1,6, hexamethylene diamine phosphate.
DETAILED DESCRIPTION
[0028] The catalysts that are useful to initiate the cure of urea formaldehyde resin precursor in accordance with the present invention are formed by reacting the diamine with an acid to form a salt. The diamines are typically reacted to give a salt solution with a pH in the range of about 10.0 to about 10.5 for the HCl salt and about 6 for the phosphate and other acid salts. The optimum pH depends upon the acid used and is generally about 6, except for the chloride salt. The urea formaldehyde resin precursor, typically available as an aqueous solution, is mixed with an aqueous solution of the diamine salt catalyst and heated to cause the resin precursor to cure.
[0029] The catalysts are typically used in an amount just sufficient to initiate the reaction to cause urea formaldehyde precursor to polymerize to form the urea formaldehyde resin, although additional amounts may also be useful. That amount of diamine catalyst on a dry weight basis is typically in the range of about 1 to about 25% by weight, preferably about 2 to about 10% by weight, most preferably about 3 to about 5% by weight, based upon the total dry weight of the urea formaldehyde resin precursor plus diamine catalyst.
[0030] It has been surprisingly found that these diamine salt catalysts in combination with urea formaldehyde resin precursors provide improved cured urea formaldehyde resin binders compared with those produced by the use of the corresponding triamines or hexamine catalyst systems.
[0031] The above defined diamine salts are the sole catalysts employed in the urea formaldehyde binders of the invention. The diamine salts are latent catalysts and do not catalyze the curing of the resin below temperatures of about 60° C. Thus, the pot life of the resin binder system at ambient temperature is longer which is particularly beneficial in the manufacturing process of the coated abrasives. This is in contrast to a co-catalyst system comprising a Lewis acid, such as aluminium chloride, and an amine salt which begins to cure the resin system at ambient temperature and has a limited pot life.
[0032] The term “urea formaldehyde resin precursor” refers to compounds which may include monomers or oligomers which are curable in the presence of an appropriate catalyst to provide fully cured urea formaldehyde resins which are solid polymeric materials that are cross-linked. Urea-formaldehyde resin precursors compositions useful in the present invention may be prepared by the reaction of urea with formaldehyde. The molar ratio of formaldehyde to urea (“F/U ratio”) of the resin ranges from about 1.4:1.0 to about 1.6:1.0. Urea-formaldehyde resins having low, i.e. less than 1%, free formaldehyde are preferred. The urea formaldehyde resin precursor aqueous solution generally has a viscosity in the range 600 to 1600 cps (0.6 to 1.6 Pascal seconds) measured at 60% by weight solids in aqueous medium using a BROOKFIELD LV viscometer with a number 1 spindle at ambient temperature (e.g., 20° C.). A preferred urea formaldehyde resin has a viscosity of about 860 cps (0.86 Pascal seconds) at ambient temperature.
[0033] Examples of commercially available urea-formaldehyde resin precursor aqueous solutions include those having the trade designations “AL3029R,” commercially available from the Borden Chemical Co., Westchester, Ill., USA, and “CBU UF,” commercially available from Dynochem Limited, Mold, U.K.
[0034] The binder preferably generally additionally comprises at least one of an acid filler or neutral filler. Preferred fillers are of the platelet type having a particle size of less than 10 micrometers. Preferred fillers include mica and clays (e.g., kaolin and silane-treated kaolin). Calcium silicate, magnesium calcium silicate may also be used. Specific materials suitable for use as fillers include those under the trade designations: SX400 mica, VANSIL EW20 (Wollastonite, calcium silicate), NYTAL 200, 400 and 7700 (magnesium calcium silicate, Microfine Minerals Ltd., Derby, U.K.); POLARITE 102A (silane treated calcined kaolin), POLESTAR 200R (calcined kaolin), kaolin grade E-silane treated, Supreme China Clay (Imerys Co., Paris, France).
[0035] The filler is generally employed in an amount from about 5 to about 50% by weight of the dry weight of urea formaldehyde binder (that being the dry weight of the urea formaldehyde precursor plus the dry weight of the diamine catalyst), preferably from about 15 to about 30%, more preferably about 25% by weight of the dry weight of the urea formaldehyde binder. The presence of the filler contributes towards the flexural modulus of the cured binder system.
[0036] The binder preferably comprises a wetting agent to assist in defloculating and dispersing the filler. The particular selection of wetting agent will depend upon the filler present in the binder formulation. Suitable wetting agents include esters of polyethylene glycol, ammonium salt of polyacrylic acid and a methacrylamide functional amine adduct of neopentyl-diallyl-oxy-tridioctyl pyro-phosphato titanate.
[0037] Suitable materials for use as wetting agents for the fillers include those available under the trade designations: DISPEX A40 (ammonium salt of polyacrylic acid, Harcros Chemicals, Inc., Kansas City, Kans.), IRGASTAT 33 (ester of polyethylene glycol, Ciba Specialty Chemicals, Basel, Switzerland), LICA 38J (methacrylamide functional amine adduct of neopentyl-diallyl-oxy tri-dioctyl pyro-phosphato titanate, Kenrich Petrochemicals Inc., Bayonne, N.J.).
[0038] The wetting agent is generally used in the range about 0.1 to about 1.0% by weight based on the total weight of filler, although additional amounts may also be useful.
[0039] The binder formulations used in the invention may preferably additionally comprise a toughening agent. This is preferably a polymer latex selected from vinyl acetate, vinyl chloride, ethylene, styrene butyl acrylate and vinyl ester of versatic acid, polymers and copolymers.
[0040] The glass transition temperature (Tg) of the polymers used as toughening agents is typically in the range 0° C. to 50° C. Typical useful polymers include VINAMUL, e.g., VFNAMUL 3303 (vinyl acetate-ethylene, Tg 0° C.), VINAMUL 3405 (a blend of the monomers vinyl acetate, vinyl chloride and ethylene with nonylphenol ethoxylate surfactant as a dispersant), VINAMUL 3479 (vinyl acetate-vinyl chloride-ethylene, Tg 30° C.), VINAMUL 69223 (vinyl acetate-vinyl ester of versatic acid, Tg 22° C.), VINAMUL 3252 (vinyl acetate-ethylene, Tg 3° C.), VINAMUL 3253 (vinyl acetate-ethylene, Tg 7° C.), VINAMUL 31259 (vinyl acetate-ethylene), VINAMUL 3171 (vinyl acetate-ethylene, Tg 4° C.), VINAMUL 43627 (vinyl acetate-butyl acrylate), and VINAMUL 7139 (Styrene-acrylate, Tg 50° C.), commercially available from Vinamul Polymers, Bridgewater, N.J.
[0041] The toughening agent is generally present in an amount in the range about 1 to about 50% by weight based on the weight of the urea formaldehyde resin (i.e., the resin precursor plus catalyst).
[0042] The binder formulation may additionally comprise other adjuvants, e.g., a defoamer and other conventional adjuvants typically used in coated abrasive binder formulations.
[0043] The urea formaldehyde binder may be present as a make coat, size coat and/or a supersize coat. Preferably, the binder is used as a size coat. The binder may be coated by any of the conventional techniques known in the art. The binder is generally cured at a temperature in the range of 75 to 140° C. Low temperature curing can be effected at a temperature of 80 to 90° C. for 20 to 40 minutes. Alternatively, higher temperatures may be employed (e.g., 115 to 125° C.) for shorter cure time periods (e.g., less than 10 minutes). Resin slabs are typically pre-dried at lower temperatures (e.g., 50° C.) prior to curing.
[0044] When used as a supersize coat, the binder formulation may comprise antiloading agents, fillers, anti-static agents, lubricants, grinding aids, etc. Examples of such additives include salts and soaps of fatty acids such as lauric acid, myristic acid, palmitic acid, stearic acid, arachic acid and behenic acid, stearate salts, particularly calcium, zinc and lithium stearate, fluorinated compounds, e.g., a fluorochemical compound selected from compounds comprising a fluorinated aliphatic group attached to a polar group or moiety and compounds having a molecular weight of at least about 750 and comprising a non-fluorinated polymeric backbone having a plurality of pendant fluorinated aliphatic groups comprising the higher of (a) a minimum of three C—F bonds, or (b) in which 25% of the C—H bonds have been replaced by C—F bonds such that the fluorochemical compounds comprises at least 15% by weight of fluorine, potassium fluoroborate, sodium fluorosilicate, potassium fluoride, iron sulfide, potassium phosphate, molybdenum disulfide and calcium hydrogen phosphate and the anti-loading component disclosed in U.S. Pat. No. 5,704,952 (Law, et al.) incorporated herein by reference.
[0045] The backing substrate used in the coated abrasive articles may be selected from any of a wide range of materials including paper, polymeric materials, cloth, and combinations thereof.
[0046] The abrasive articles can contain 100% of a single abrasive grain mineral composition. Alternatively, the abrasive article may comprise a blend or mixture of different abrasive grain mineral compositions. The mineral may be coated from 1% to 99% blends, preferably 50 to 95%, to form either open or closed coat construction. Useful conventional abrasive grains include fused aluminum oxide, heat treated aluminum oxide, white fused aluminum oxide, silica, silicon carbide, titanium diboride, boron carbide, tungsten carbide, titanium carbide, diamond, cubic boron nitride, garnet, fused alumina zirconia, sol gel abrasive grains and the like. Examples of sol gel abrasive grains can be found in U.S. Pat. No. 4,314,827 (Leitheiser, et al.); U.S. Pat. No. 4,623,364 (Cottringer, et al.); U.S. Pat. No. 4,744,802 (Schwabel); U.S. Pat. No. 4,770,671 (Monroe, et al.) and U.S. Pat. No. 4,881,951 (Wood, et al.), all of which are incorporated herein by reference. The diamond and cubic boron nitride abrasive grains may be monocrystalline or polycrystalline. The particle size of these conventional abrasive grains can range from about 0.01 to 1500 micrometers, typically between 1 to 1000 micrometers. The abrasive grains may also contain an organic or inorganic coating. Such surface coatings are described, for example, in U.S. Pat. No. 5,011,508 (Wald, et al.); U.S. Pat. No. 1,910,444 Nicholson); U.S. Pat. No. 3,041,156 (Rowse, et al.); U.S. Pat. No. 5,009,675 (Kunz, et al.); U.S. Pat. No. 4,997,461 (Markhoff-Metheny); U.S. Pat. No. 5,213,591 (Celikkaya, et al.); U.S. Pat. No. 5,085,671 (Martin, et al.); and U.S. Pat. No. 5,042,991 (Kunz, et al.) all of which are incorporated herein by reference.
[0047] In one embodiment a pressure sensitive adhesive is coated onto the back side of the coated abrasive such that the resulting coated abrasive can be secured to a back up pad. In another embodiment the coated abrasive may contain a hook and loop type attachment system to secure the coated abrasive to the back up pad. The loop fabric may be on the back side of the coated abrasive with hooks on the back up pad. Alternatively, the hooks may be on the back side of the coated abrasive with the loops on the back up pad. This hook and loop type attachment system is further described in U.S. Pat. No. 4,609,581 (Ott); U.S. Pat. No. 5,254,194 (Ott, et al.); and U.S. Pat. No. 5,505,747 (Barry, et al.), all of which are incorporated herein by reference.
EXAMPLES
[0048] Embodiments of this invention are further illustrated by the following examples, but the particular materials and amounts thereof recited in these examples, as well as other conditions and details, should not be construed to unduly limit this invention. All parts and percentages are by weight unless otherwise indicated.
[0049] In the Examples the following materials were used:
CBU UF A urea formaldehyde resin precursor commercially available from Dynochem Limited, Mold, Flintshire, U.K., supplied as a 67-70% solids aqueous solution having a viscosity of 685 to 1600 cps (0.685 to 1.6 Pascal seconds) depending upon the molecular weight of the resin (typically about 790 cps, 0.79 Pascal seconds). SX400 Mica commercially available from Microfine Minerals Limited, Derby, U.K. POLARITE 102A Silane treated calcined kaolin commercially available from Imerys Co., Paris, France. V4305 Vinyl acetate-vinyl chloride-ethylene latex commercially available from National Starch & Chemical Co., Bridgewater, NJ. V3479 Vinyl acetate-vinyl chloride-ethylene latex commercially available from National Starch & Chemical Co. Kaolin Grade E Silane treated kaolin commercially available from Imerys Co., Paris, France. LICA 38J Methacrylamide functional amine adduct of neopentyl- diallyl-oxy-tri-dioctyl pyro-phosphato titanate commercially available from Kenrich Petrochemicals Inc., Bayonne, NJ. IRGASTAT 33 Ester of polyethylene glycol commercially available from Ciba Specialty Chemicals, Basel, Switzerland. 1512M A defoamer commercially available from Hercules Inc., Wilmington, DE.
Examples 1A-1E
[0050] Examples 1A-1E, respectively, show urea formaldehyde resin precursors cured with diamine-based catalysts with different acid salts.
[0051] In Example 1A a diamine phosphate catalyst solution was made by mixing under reflux 47.5 g of 60% weight solution of 1,6-hexamethylene diamine (0.25 mole) in water with 46.6 g of 85% weight solution of phosphoric acid (0.48 mole) and 200 g of water. The resulting mixture generated heat, indicating an exothermic reaction, and the mixture was cooled during manufacture and before use. The resultant solution contained 23% by weight diamine phosphate catalyst.
[0052] The following procedure was used to prepare the Examples:
[0053] 1. Mix the urea formaldehyde resin precursor aqueous solution and the wetting agent, if used, to provide a resin pre-mix smooth paste.
[0054] 2. High-shear mix the filler into the resin pre-mix smooth paste.
[0055] 3. Mix in the latex containing the toughening agent polymer, if used.
[0056] 4. Mix in the defoamer, if used.
[0057] 5. Mix in the diamine salt catalyst solution.
[0058] Examples 1B-1E show the preparation of other catalysts using the same diamine, i.e., 1,6-hexamethylene diamine, reacted with other acids to produce diamine salt catalyst solutions. These were prepared in an analogous manner as described above for Example 1A using the same molar equivalents.
[0059] The resulting catalysts were mixed with the CBU UF urea formaldehyde resin precursor aqueous solution to provide a mixture which was cast to form a 40 mm×20 mm×1 mm slab and cured in an oven for 30 minutes at 50° C., followed by 60 minutes at 75° C., followed by a seven day aging at room temperature.
Example 1A
[0060] [0060] Wet Solids Dry Component Wt. % (g) Wt. % Urea formaldehyde resin precursor solution 65.00 42.25 64.29 (CBU UF) Hexamethylene diamine phosphate salt 15.00 3.47 5.28 1 solution Mica (SX400) 20.00 20.00 30.43
Example 1B
[0061] [0061] Wet Solids Dry Component Wt. % (g) Wt. % Urea formaldehyde resin precursor solution 574.96 373.72 66.64 (CBU UF) Hexamethylene diamine sulphate salt 51.12 25.83 4.61 1 solution Vinyl acetate-vinyl chloride-ethylene latex 14.48 7.24 1.29 (V4305) Mica (SX400) 130.72 130.72 23.31 Methacrylamide functional amine adduct of 0.30 0.30 0.05 neopentyl-diallyl-oxy-tri-dioctyl pyro- phosphato titanate wetting agent (LICA 38J) Wetting agent (IRGASTAT 33) 7.36 7.36 1.31 Defoamer (1512M) 4.48 4.48 0.80 Orange Pigment 16.40 11.15 1.99
Example 1C
[0062] [0062] Wet Solids Dry Component Wt. % (g) Wt. % Urea formaldehyde resin precursor solution 574.96 373.72 67.70 (CBU UF) Hexamethylene diamine acetate salt solution 51.12 17.04 3.09 1 Vinyl acetate-vinyl chloride-ethylene latex 14.48 7.24 1.31 (V4305) Mica (SX400) 130.72 130.72 23.68 Wetting agent (LICA 38J) 0.30 0.30 0.05 Wetting agent (IRGASTAT 33) 7.36 7.36 1.33 Defoamer (1512M) 4.48 4.48 0.81 Orange Pigment 16.40 11.15 2.02
Example 1D
[0063] [0063] Wet Solids Dry Component Wt. % (g) Wt. % Urea formaldehyde resin precursor solution 574.96 373.72 67.56 (CBU UF) Hexamethylene diamine nitrate salt solution 51.12 18.23 3.29 1 Vinyl acetate-vinyl chloride-ethylene latex 14.48 7.24 1.31 (V4305) Mica (SX400) 130.72 130.72 23.63 Wetting agent (LICA 38J) 0.30 0.30 0.05 Wetting agent (IRGASTAT 33) 7.36 7.36 1.33 Defoamer (1512M) 4.48 4.48 0.81 Orange Pigment 16.40 11.15 2.02
Example 1E
[0064] [0064] Wet Solids Dry Component Wt. % (g) Wt. % Urea formaldehyde resin precursor solution 574.96 373.72 66.94 (CBU UF) Hexamethylene diamine citrate salt solution 51.12 23.30 4.17 1 Vinyl acetate-vinyl chloride-ethylene latex 14.48 7.24 1.30 (V4305) Mica (SX400) 130.72 130.72 23.41 Wetting agent (LICA 38J) 0.30 0.30 0.05 Wetting agent (IRGASTAT 33) 7.36 7.36 1.32 Defoamer (1512M) 4.48 4.48 0.80 Orange Pigment 16.40 11.15 2.00
[0065] The flexural modulus and toughness of the slabs were measured at room temperature by 3 point bend using a flexural modulus and toughness testing device commercially available from Instron Corp., Canton, Mass. under the trade designation INSTRON 4301. The summary of the results is reported in the following Table.
Example Flexural Modulus Toughness No. Catalyst (MPa) (MPa) 1A diamine phosphate 10830 0.08 1B diamine sulphate 10960 0.0795 1C diamine acetate 9127 0.0111 1D diamine nitrate 9542 0.0724 1E diamine citrate 8635 0.0645
[0066] The surfaces of the diamine-sulphate and nitrate diamine-catalyzed slabs were not as smooth as the diamine phosphate-catalyzed slabs.
Examples 2 to 8
[0067] The following formulations were prepared and tested in accordance with Example 1.
[0068] The formulations were cast into slabs as in Example 1. The resin formulations were cured as described in Example 1.
Example 2
[0069] [0069] Wet Solids Dry Component Wt. % (g) Wt. % Urea formaldehyde resin precursor solution 65.00 42.25 55.92 (CBU UF) 4.7 molar hexamethylene diamine hydro- 15.00 13.31 17.62 1 chloride solution Mica (SX400) 20.00 20.0 26.47
Example 3
[0070] [0070] Wet Solids Dry Component Wt. % (g) Wt. % Urea formaldehyde resin precursor solution 69.78 45.38 79.40 (CBU UF) Vinyl acetate-vinyl chloride-ethylene latex 19.77 10.00 17.51 (V4305) 4.7 molar hexamethylene diamine hydro- 1.99 1.77 3.09 1 chloride solution Water 8.46
Example 4
[0071] [0071] Wet Solids Dry Component Wt. % (g) Wt. % Urea formaldehyde resin precursor solution 80.41 52.27 82.69 (CBU UF) Vinyl acetate-vinyl chloride-ethylene latex 1.53 0.76 1.21 (V4305) 4.7 molar hexamethylene diamine phosphate 10.23 2.36 3.73 1 solution Kaolin grade E 6.59 6.59 10.43 Wetting agent (IRGASTAT 33) 0.82 0.82 1.30 Defoamer (1512M) 0.41 0.41 0.65
Example 5
[0072] [0072] Wet Solids Dry Component Wt. % (g) Wt. % Urea formaldehyde resin precursor solution 62.48 40.61 66.75 (CBU UF) Vinyl acetate-vinyl chloride-ethylene latex 17.71 8.86 14.55 (V4305) 4.7 molar hexamethylene diamine hydro- 1.78 1.58 2.60 1 chloride solution Silane treated calcined kaolin 9.62 9.62 15.81 (POLARITE 102A) Defoamer (1512M) 0.18 0.18 0.30 Water 8.22
Example 6
[0073] [0073] Wet Solids Dry Component Wt. % (g) Wt. % Urea formaldehyde resin precursor solution 76.56 49.76 76.79 (CBU UF) Vinyl acetate-vinyl chloride-ethylene latex 15.01 7.51 11.58 (V4305) 4.7 molar hexamethylene diamine hydro- 7.93 7.03 10.86 1 chloride solution Mica (SX400) 0.30 0.30 0.46 Defoamer (1512M) 0.20 0.20 0.31
Example 7
[0074] [0074] Wet Solids Dry Component Wt. % (g) Wt. % Urea formaldehyde resin precursor solution 73.41 46.73 69.79 (CBU UF) (858 cps) Vinyl acetate-vinyl chloride-ethylene latex 1.85 0.91 1.35 (V3479) Hexamethylene diamine phosphate solution 6.50 1.47 2.19 1 (mix of 23.53 g of a 60% solution of 1,6 hexamethylene diamine in water and 23.22 g of an 85% solution of phosphoric acid and 100 g of water) Mica (SX400) 16.69 16.34 24.40 Methacrylamide functional amine adduct of 0.04 0.04 0.06 neopentyl-diallyl-oxy-tri-dioctyl pyro- phosphato titanate wetting agent (LICA 38J) Wetting agent (IRGASTAT 33) 0.94 0.92 1.37 Defoamer (1512M) 0.57 0.56 0.84
Example 8
[0075] [0075] Wet Solids Dry Component Wt. % (g) Wt. % Urea formaldehyde resin precursor solution 77.31 45.77 75.36 (CBU UF) Vinyl acetate-vinyl chloride-ethylene latex 1.94 0.89 1.46 (V4305) Mica filler (SX400) 12.25 11.16 18.38 Defoamer (1512M) 0.60 0.55 0.91 Wetting agent (IRGASTAT 33) 0.99 0.90 1.48 Hexamethylene diamine phosphate solution 6.87 2.38 2.16 1 (pH 5.8 to 6.1) Wetting agent (LICA 38J) 0.02 0.02 0.04
[0076] The flexural modulus and toughness of slabs made from this mix according to the techniques of Example 1 was compared with slabs made from the phenolic resin mix used in the size layer of 775L STIKIT™ abrasive disc commercially available from 3M United Kingdom plc.
Urea Formaldehyde Mix Phenolic Resin Mix Flexural modulus (MPa) 1067 800 Toughness (MPa) 0.127 0.076
[0077] The urea formaldehyde mix was used as a size coat in place of the phenolic resin system on a P180 775L STIKIT™ disc. The cutting performance of each disc was closely matched both in terms of cutting rate and cumulative cut.
Example 9
[0078] The following formulation was prepared:
Wet Solids Dry Component Wt. % (g) Wt. % Methacrylamide functional amine adduct of 0.04 0.04 0.05 neopentyl-diallyl-oxy-tri-dioctyl pyro- phosphato titanate (LICA 38J) Urea formaldehyde resin precursor solution 71.87 46.72 68.35 (CBU UF) Vinyl acetate-vinyl chloride-ethylene latex 1.81 0.91 1.32 (V4305) Mica (SX400) 16.34 16.34 23.91 Defoamer (1512M) 0.56 0.56 0.82 Wetting agent (IRGASTAT 33) 0.92 0.92 1.35 Hexamethylene diamine phosphate solution 6.39 1.47 2.16 1 Orange pigment 2.05 1.39 2.04
[0079] The diamine phosphate was a mix of 23.75 g of a 60% solution of 1,6 hexamethylene diamine in water and 23.22 g of an 85% solution of phosphoric acid and 100 g of water. These components were mixed under reflux, causing an exotherm, heating the solution. The solution was cooled during preparation.
[0080] The mix procedure was as follows:
[0081] 1. Mix the CBU urea formaldehyde resin precursor solution with the wetting agent (LICA 38J) and filler to provide a smooth paste.
[0082] 2. Mix in the SX400 mica filler.
[0083] 3. Mix in the Orange pigment.
[0084] 4. Mix in the latex (V4305) containing the toughening agent polymer.
[0085] 5. Mix in defoamer (1512M).
[0086] 6. Mix in the wetting agent (IRGASTAT 33).
[0087] 7. Mix in the hexamethylene diamine phosphate solution
[0088] The mixture was used as a size coat on coated abrasive web which was converted into 15 cm diameter P80 HOOKIT™ discs (HOOKIT™ is a trade mark of 3M Company). The mixture was used in place of the conventional phenol formaldehyde size coat, normally used on the commercially available product (3M 775L). The disc exhibited closely matched cutting performance to the commercially available disc.
Example 10
[0089] This Example demonstrates use of the urea formaldehyde resin in a supersize layer.
[0090] The urea formaldehyde binder used was the same one described in Example 9 with the exception that the orange pigment was not added. The binder was mixed with a calcium stearate dispersion 1097A commercially available from eChem Ltd., Leeds, U.K., in the following weight ratios:
Binder Stearate 5 95 10 90 20 80 30 70 45 55 70 30
[0091] The supersize was coated over an abrasive sheet equivalent to that which is commercially available under the trade designation 3M618, without its supersize layer. Coated abrasive identified as 3M618 is available from 3M United Kingdom plc and it comprises a paper backing, a urea formaldehyde make coating, a urea formaldehyde size coating and SiC abrasive particles. The supersize coatings were dried and cured for 5 minutes at 105° C.
[0092] Samples were evaluated by hand sanding on medium density fiber board (MDF) panels coated with (a) a water based lacquer or (b) a waxed polyester and compared against the commercial product 3M 618.
[0093] The water based lacquer was that available under the trade designation “WATER BASED LACQUER SEMI-MATT” from Granyte Coatings, Salford, U.K. The wax polyester was that available under the trade designation “SAYERLACK PH6355” from Arch Coatings, Knottingley, U.K.
[0094] Each panel was sanded for 50 strokes (about 20×4 cm 2 ). The abrasive sheet was supported on a rubber block (5×2.5 cm 2 ) but was used by hand. The cut was measured in grams.
[0095] Anti-loading and cut performance of the samples of the invention was similar to that of the 3M618 coated abrasive sheet for the test on water based lacquer for 55% and higher stearate levels.
[0096] Anti-loading and cut performance of the samples of the invention was similar to that of the 3M618 coated abrasive sheet for the test on waxed polyester lacquer for 70% and higher stearate levels.
[0097] Various modifications and alterations of this invention will become apparent to those skilled in the art without departing from the scope and spirit of this invention, and it should be understood that this invention is not to be unduly limited to the illustrative embodiments set forth herein. | A binder for abrasive products, coated abrasive articles and a method of making the same comprising a urea formaldehyde resin precursor cured in the presence of a sole catalyst which consists essentially of at least one salt of an acid with a diamine of the formula H 2 N—R—NH 2 wherein R is an alkylene group of 3 to 10 carbon atoms, and the acid is selected from the group consisting of hydrochloric, citric, nitric, sulphuric, acetic, phosphoric and combinations thereof | 1 |
FIELD OF THE INVENTION
The invention relates to specialized forms of adjustably positioned lighting fixtures, as frequently used in commercial and theatrical lighting, and particularly to features thereof to accommodate and facilitate periodic adjustment.
BACKGROUND OF THE INVENTION
Specialized lighting fixtures, such as theatrical lighting, and various forms of commercial lighting fixtures are constructed to provide for accurate aiming of a light beam. In many cases, after a lighting fixture is initially installed, it may be adjusted one or more times until a desired effect is achieved. At that juncture, it may be desired to tightly lock the adjustments, so that vibrations and other external influences will not, over time, result in undesired movements in the adjusted position of the fixture. For effectively tight locking of the adjustments, a tool frequently is required. However, if the workman does not have the correct tool at the proper time, the final locking of the adjustments may not be carried out.
SUMMARY OF THE INVENTION
The invention is directed to an improvement in adjustable lighting fixtures of the type described, particularly for track lighting systems, which include novel and effective facilities for housing a locking tool in the fixture itself in a reliable and secure manner, easily accessible to a workman. Typically a suitable locking tool is an Allen key, of a size to be engageable with one or more Allen screws provided on the fixture, for securely tightening the fixture in an adjusted position when appropriate and desired. The Allen key is mounted in a convenient manner and location, easily accessible to the workman, yet is securely retained against accidental dislodgment and loss, and is easily replaced by the workman when finished with the locking operations.
An advantageous form of track lighting fixture of existing design includes a mounting body arranged to be received within a downwardly opening recess of a bus bar containing conductive elements for operating lighting fixtures positioned anywhere along the bar. The mounting body includes a rotatable element carrying electrical contacts and a clamping element, all operated by a rotatable locking lever accessible at the bottom of the mounting body. After the mounting body is positioned in the bus bar, the locking lever is rotated such that the electrical and the clamping elements are rotated into engagement with the bus bar, securing the fixture in position and engaging its electrical contacts with the conductors of the bus bar. The new fixture incorporates a novel and specialized design of locking lever, which enables it to conveniently house an Allen key in a secure manner which is at the same time easily accessible to a workman for locking an adjusted lighting fixture in a desired orientation and also conveniently restored to its position within the locking lever so as to be available for a future occasion. The proper tool thus always accompanies the fixture and is always available to a workman installing, re-installing and/or adjusting the fixture.
For a more complete understanding of the invention reference should be made to the following detailed description of a preferred embodiment thereof and to the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a perspective view of an advantageous form of track lighting fixture incorporating the features of the invention.
FIG. 2 is an exploded view of a rotatable locking lever, utilized in the fixture of FIG. 1 , incorporating features of the invention.
FIGS. 3 and 4 are top plan views of the locking lever of FIG. 2 , showing features according to the invention for receiving and securely retaining an Allen key for use in setting the lighting fixture in a semi-permanent manner after its initial adjustments have been completed.
DETAILED DESCRIPTION OF THE INVENTION
Referring now to the drawings, the reference numeral 10 designates generally a track lighting fixture which, except for features to be described hereinafter, is of a known type with known features which do not form part of this invention. The illustrated fixture includes a lamp body 11 which is mounted on a transformer housing 12 for rotation with respect to the housing 12 about a horizontal axis. Suitable calibration indices 13 may be provided to assist in properly orienting the housing 11 with respect to its rotational axis. The transformer housing 12 is attached to a mounting body 14 and is arranged for rotation with respect to the mounting body 14 , about a vertical axis. Calibration indices 15 also can be provided to facilitate proper rotational adjustment about the vertical axis.
The mounting body 14 is of an inverted T-shaped cross sectional configuration, suitable to be received within the downwardly opening recess of a typical bus bar (not shown). A flange 16 at the bottom of the mounting body seats against bottom surfaces of the bus bar.
For mounting the fixture 10 in the bus bar, the mounting body 14 houses an internal rotary element (not shown) carrying electrical contacts 17 , 18 and a clamping element 19 . The rotary element is fixed to a rotary locking lever 20 located underneath the flange 16 . For the initial mounting of the fixture, the lever 20 is rotated at right angles to the mounting body 14 , to retract the contacts 17 , 18 and the clamping element 19 into the mounting body. After the mounting body is positioned in the bus bar, the lever 20 is rotated to a position parallel with the mounting body, as shown in FIG. 1 , simultaneously to cause the clamping element 19 to lockingly engage the bus bar and to cause the contacts 17 , 18 to engage linear conductors within the bus bar.
After mounting the fixture on the bus bar, the lamp housing 11 is normally adjusted about its respective horizontal and vertical axes to cause light from the fixture to be properly focused on a desired subject area. Typically, there is sufficient friction in the horizontal and vertical rotational connections to enable the housing 11 to remain in an adjusted position. However, over time, various influences such as vibrations, temperature variations, accidental bumping etc., can cause an initial adjusted position to change. Accordingly, manufacturers frequently provide locking devices, such as Allen screws, for tightly locking the elements in their adjusted positions to largely prevent such undesired movements. One such Allen screw is indicated at 21 in FIG. 1 for the vertical axis adjustment, and a similar such screw (not visible) is provided on the housing 11 for locking the horizontal axis adjustment.
Pursuant to the invention, a locking lever 20 of novel design is provided to enable each lighting fixture to be provided with an Allen key suitable for its components, with the Allen key being inserted and retained in the locking lever so as to be available at all times for securing of the fixture in its adjusted position. With reference to FIGS. 2-4 , the locking lever 20 comprises a molded plastic body 22 formed with a generally flat bottom wall 23 , a surrounding wall 24 and a rounded end 25 to accommodate rotation. At the center of the rounded end, the lever is formed with socket walls 26 forming a hexagonal socket engageable with a correspondingly shaped element (not shown) forming the bottom of the previously mentioned rotary element in the mounting body 14 . A screw fastener 28 is engageable through opening 27 at the center of the socket defined by walls 26 , for fixing the lever 20 to the rotary element.
Locking levers 20 generally are well known devices for use in the mounting of track lighting fixtures and frequently are formed with a bottom opening 29 providing access to an on-off switch (not shown). An associated side recess 30 allows the lever to be rotated to engage or disengage the fixture when the switch is in its “off” position. The locking lever of the invention, however, includes an additional and unique feature for receiving and reliably retaining an Allen key 31 . As shown in FIGS. 2 and 4 , a standard Allen key 31 is of L-shaped configuration comprised of a long leg 32 and a short leg 33 . The locking lever of the invention is formed with an opening 34 in an end portion 35 of the surrounding wall, with one side of the opening being defined by a side wall portion 36 . The side wall portion 36 forms a guide for receiving the long leg of the Allen key 31 and forms one side of a cavity for retaining the key. In this respect, the length of the locking lever 22 is such that the entire long leg of the Allen key can be received within the lever 22 , with the short leg positioned tightly against the end wall portion 35 (see FIG. 4 ).
Spaced inward from the guide wall 36 is an inner confinement wall 37 , which is spaced from the guide wall and defines therewith a confinement space considerably greater than the thickness of the Allen key. In the illustrated and preferred embodiment of the invention, the confinement wall 37 is formed, adjacent to the end wall opening 34 with a short re-entrant wall 38 defining an inwardly facing, open ended recess 39 . The recess 39 is arranged to receive one end 40 of a generally J-shaped strip spring 41 . The spring 41 includes an elongated stem portion 42 , which is received in the confinement space between walls 36 , 37 , and an arcuate portion 43 configured to pass part way around the socket wall 36 . The arcuate portion 43 joins at an apex 44 with a straight portion 45 passing in contact with a facet 46 of the socket wall 26 that lies parallel with the opposite side portions 36 , 47 of the wall 24 . The straight portion 45 of the spring terminates in an outwardly and rearwardly directed end element 48 , which is received in a recess slot 49 on the inside of the wall portion 47 .
The spring 41 is assembled with the molded lever body by inserting the spring downwardly into the open top of the lever body, inserting the opposite ends of the spring into their respective confining slots 39 , 49 . The geometry of the spring 41 is such that, when initially assembled, a portion 50 of the spring, between the straight and arcuate portions 42 , 43 lies close to, and preferably bears resiliently against the inner surface of the side wall 36 , as shown in FIG. 3 . To advantage the arcuate portion 43 of the spring may be pressed outward by corner 51 of the socket wall 46 to help press the spring portion 50 against the wall 36 .
As shown in FIGS. 3 and 4 , the straight portion 42 of the strip spring 41 extends diagonally across the confinement space between the walls 36 , 37 at a small angle thereto. Accordingly, when the long leg 32 of the Allen key is inserted into the end opening 34 , the end of the key is confined between the spring and the wall 36 . As the key is forced inward, it displaces the spring inwardly in the region of the portion 50 . When the Allen key is fully inserted, as shown in FIG. 4 , the long leg 32 of the key is tightly gripped between the spring portion 50 and the wall 36 and is removable only by an intentional withdrawal by a service man or other person.
As shown in FIG. 4 , the Allen key 31 is formed with a generous rounding in the area 53 between the short and long legs 33 , 32 . To accommodate this rounding, the end wall opening 34 is substantially wider than the maximum thickness of the key stock. This allows the key to be inserted into the lever 22 sufficiently that the short leg 33 of the key comes into contact with the end wall 35 . It also stabilizes the key by providing a support surface 54 to position and hold the short leg 33 parallel with the bottom surface 23 of the locking lever. Only the short leg of the key is visible externally, and that is positioned tightly against the end wall of the lever 22 so as to be inconspicuous while being readily available for use.
The key-holding feature of the invention can be incorporated with track lighting fixtures of existing design with minimal cost, consisting of the cost of the spring 41 and its assembly, and minor, one-time mold revisions to accommodate the presence of the spring and to define a recess and an opening for the Allen key.
The new feature has substantial commercial significance in that it makes the overall product substantially more attractive to potential customers. Maintaining the adjustable lighting fixtures in accurate adjustment is a concern of all users thereof, and the improvement of the present invention greatly simplifies such maintenance and, more importantly, makes it more likely that the necessary or desired locking of the fixture adjustment will in fact take place. When “final” adjustments of a fixture have been completed, it is largely assured that the fixture adjustment can and will be properly locked because the required tool is always available to the service person.
It should be understood, of course, that the specific form of the invention herein illustrated and described is intended to be representative only as various changes may be made therein without departing from the clear teachings of the disclosure. Accordingly, reference should be made to the following claims in determining the full scope of the invention. | An adjustable track lighting fixture of a type having rotary locking lever for securing the fixture to a bus bar, where the locking lever is economically formed with an internal confinement facility of removably housing an Allen key to be retained with the fixture and used for locking the adjustments of the fixture when desired. A spring, also housed internally of the locking lever, resiliently but releasably retains the Allen key until purposefully withdrawn by a workman. The key is returned to its confinement after the workman has finished using it for the purposes intended. The key is retained in an inconspicuous manner but nevertheless visible to the workman and readily extracted for use when desired. | 5 |
This application is a Continuation-In-Part of prior U.S. patent application Ser. No. 08/375,520, filed Jan. 18, 1995, U.S. Pat. No. 5,517,815 which is a Continuation of U.S. patent application Ser. No. 08/209,469, filed Mar. 14, 1994 and now abandoned.
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to an apparatus for generating power by use of a gaseous fuel such as gasified coal.
2. Discussion of the Related Art
Coal is of importance as a fuel for power generation now and in the future since there are a lot of coal reserves, and the coal reserves are hardly unevenly distributed over the world. It is required to reduce the emission of the materials such as SOx, NOx, or CO 2 from a power plant which generates power by using coal as a fuel, which adversely affect the global environment, and also to improve the efficiency of power a coal gasification generation. To satisfy such requirements, a coal gasification power generator, a power generator of the pressurized fluidized bed combustion boiler type and the like have been developed in lieu of a conventional pulverized coal boiler. As one of those developing power generators, there has been proposed a power generator using a fluidized bed coal gasifying furnace. One example of the conventional power generator is shown in FIG. 6. This conventional power generator has been proposed by British Coal Corporation in Great Britain, and will be described with reference to FIG. 6.
Coal 100, limestone 400, air 203 and water vapor 300 are supplied to a coal gasifying furnace 1'. The coal 100 is gasified in the coal gasifying furnace 1'. H 2 S and COS in the resultant generated gas are reacted with the limestone 400 and fixed as CaS in the limestone 400.
Dust in a coal gas 500 generated from the coal gasifying furnace 1' is removed by a dust removing unit 3. A coal gas 501 which has been subjected to dust removal is introduced in a combuster 5. Char which has not been gasified in the coal gasifying furnace 1' and particles 60b of the limestone 400 after the above reaction are extracted from the coal gasifying furnace 1' and then transferred to a hopper 17. Particles 60c removed from the coal gas 500 by the dust removing unit are transferred to the hopper 17.
Air 200 is pressurized by an air compressor 6 to produce a pressurized air 201. Pressurized air 204, which is a part of the pressurized air 201, is supplied to the combuster 5. The gas 501 is burned by the combuster 5 by application of the pressurized air 204, thereby generating a gas turbine inlet gas 800. A gas turbine 7 is driven by the gas turbine inlet gas 800 to produce a gas turbine outlet gas 801 having normal pressure. The gas turbine 7 drives the air compressor 6 and the power generator whereby electricity is obtained from the power generator. The heat of the gas turbine outlet gas 801 is retrieved by an exhaust heat recovery boiler 8a to be radiated to the air from a funnel.
The char and particles 60d of a desulfurization agent stored in the hopper 17 are supplied to an atmospheric circulating fluidized bed combustion unit 2'. In the atmospheric circulating fluidized bed combustion unit 2', the char is burned by the aid of air 206 supplied from a blower 18 while CaS contained in the limestone 400 is oxidized into CASO 4 . After the heat of a combustion gas 700 produced from the atmospheric circulating fluidized bed combustion unit 2' is retrieved by an exhaust heat recovery boiler 8b, particles 901 contained in a combustion gas 701 is removed by a dust removing unit 19 so that the gas 700 are radiated to the air from the funnel 9 as a gas 803.
Water vapor 30a which has been heated by heat exchangers 10a and 10b installed in the exhaust heat recovery boilers 8a and 8b and a heat exchanger 10c installed in the atmospheric circulating fluidized bed combustion unit 2' drives a steam turbine 11 which drives the power generator. As a result, electricity is produced from the power generator.
The above-mentioned conventional power generator has a first problem in that the efficiency of power generation is low. Among chemical energy possessed by coal, chemical energy possessed by the char, which has been transferred to the atmospheric circulating fluidized bed combustion unit 2' without being gasified in the coal gasifying furnace 1', is transformed into electrical energy by the steam turbine 11. However, the energy possessed by the char is not used for driving the gas turbine 7. Therefore, there is a disadvantage in that the conversion efficiency of chemical energy into electrical energy is lowered for the condition where the gas turbine 7 is not used.
The conventional power generator has a second problem that lowers the efficiency of desulfurization. The first reason why the efficiency of desulfurization is lowered is that the efficiency of desulfurization of the coal gasifying furnace 1' is lowered. The second reason why the efficiency of desulfurization is that a large amount of SO 2 is emitted from the atmospheric circulating fluidized bed combustion unit 2'.
As described above, in the conventional power generator, limestone and coal are supplied to the coal gasifying furnace 1' so that gasification of coal and desulfurization of H 2 S and COS contained in the gas due to limestone are carried out in the same fluidized bed. In this case, it has been recognized that the rate of desulfurization in the coal gasifying furnace 1' is lowered for three causes stated below.
The first cause is that, in an area where oxygen exists at the bottom of the coal gasifying furnace 1', limestone is reacted with H 2 S and COS contained in the gas to produce CaS which is reacted with oxygen. As a result, there occurs a reaction in which CaS is converted into CaO and SO 2 .
The second cause is that a time required for completing desulfurization is different from that of gasification of coal. In order to complete desulfurization due to the existence of limestone, for example, approximately 120 seconds are required in a gas at 900° C. under the pressure of 12 ata. On the contrary, a time required for gasification of coal is approximately 30 minutes. Therefore, provided that a time necessary for gasification of coal is a particle residence time of coal and limestone in the coal gasifying furnace 1', there is no time sufficient for completion of the desulfurization reaction.
The third cause is that, because H 2 S and CO are produced in the whole furnace due to gasification of coal, H 2 S and COS produced in the upper portion of the furnace have a shorter time to be in contact with limestone in the furnace compared with H 2 S and COS generated at the lower portion of the furnace.
For the above-mentioned reasons, the desulfurization efficiency of coal and limestone in the coal gasifying furnace 1' could not be elevated.
SUMMARY OF THE INVENTION
An object of the present invention is to provide a coal gasification power generator which is capable of improving the efficiency of power generation by efficiently converting chemical energy into electrical energy.
Another object of the present invention is to provide a coal gasification power generator which is capable of reducing sulfur oxide to be emitted by improving the rate of desulfurization to coal gas used as fuel.
In the coal gasification power generator in accordance with the present invention, the following structure is applied for achieving an improvement in the efficiency of power generation and an improvement in the efficiency of desulfurization.
(1) Improvement in the efficiency of power generation
According to the present invention, in order to elevate the efficiency of power generation in a power generator, the following system is used for efficiently distributing coal energy to a gas turbine and a steam turbine.
First, combustion gas generated from an oxidizing furnace which allows char generated in a gasifying furnace to be burned is introduced as a gasifying agent in a gasifying furnace. Then, coal gas supplied from the gasifying furnace is used for driving a gas turbine.
Thus, coal char is burned in the oxidizing furnace, and the combustion gas is used as a gasification agent in the gasifying furnace whereby coal char energy is converted into coal gas energy. The coal gas is used for driving the gas turbine. As a result, coal char energy can be used for gas turbine drive.
Further, according to the present invention, a heat exchanger to heat water vapor is located in a bed of an oxidizing furnace for cooling. This is a system to supply water vapor after overheating water vapor from an exhaust heat recovery boiler to the steam turbine.
To the heat exchanger thus configured for cooling the bed of the oxidizing furnace, water vapor is supplied, and then water vapor whose temperature is increased up in the heat exchanger is used in the steam turbine. As a result, the quantity of water vapor is increased and the temperature of water vapor supplied to the steam turbine is elevated in comparison with the conventional system. Consequently, the quantity of heat exchange with oxidizing furnace emission gas is increased and the efficiency of the steam turbine due to the temperature rise in the water vapor is heightened, and loss of the emission gas caused by making the funnel inlet temperature of the emission gas boiler lowered can be reduced.
(2) An improvement in the efficiency of desulfurization
The present invention has the following structure in order to improve the efficiency of desulfurization.
First, a coal gasifying section and a desulfurizing section are divided into a gasifying furnace and a desulfurization furnace, respectively. A coal gas produced by the gasifying furnace is introduced into the desulfurization furnace, and limestone supply equipment is installed in the desulfurization furnace. A fluidized bed is formed in the desulfurization furnace, which is constituted as a reactor which can adjust the height of the fluidized bed.
Thus, the gasifying furnace and the desulfurization furnace are separated to prevent CaS from being converted due to oxygen, which is the first cause of lowering of the desulfurization efficiency.
Further, with the separation of the gasifying furnace and the desulfurization furnace, the adverse condition of the residence time of limestone within the furnace be shorter than a reaction time necessary for the conversion of limestone into CaS in the conventional system, which is the second cause of lowering the desulfurization efficiency, can be improved. The intended residence time of limestone for completion of the reaction in which limestone is converted into CaS can be ensured by adjusting the height of the fluidized bed.
By separating the gasifying furnace and the desulfurization furnace, the efficiency of contact of H 2 S and COS in the coal gas and limestone, which is the third cause of lowering of the desulfurization efficiency, is improved. The sum of H 2 S in the coal gas and the density of COS becomes maximum at the gasifying furnace outlet, and the coal gas is supplied to the desulfurization furnace with a maximum of H 2 S and the COS density to improve the efficiency of contact of H 2 S with COS.
In addition, according to the present invention, the desulfurization furnace has the following structure with the result that the efficiency of desulfurization can be improved more than the above cases.
That is, a gas dispersion plate for forming the fluidized bed of limestone is installed within a reactor of the desulfurization furnace, and an interior dispersion plate, which is formed of a porous plate for limiting the movement of particles, is installed within the fluidized bed. The fluidized bed is divided into upper and lower fluidized beds by the interior dispersion plate. A cooler (heat exchanger) is located on the upper fluidized bed, and limestone is supplied to the upper fluidized bed. Coal gas is supplied from piping, which is coupled with the gasifying furnace, to the lower fluidized bed through the gas dispersion plate, and the coal gas which has passed through the lower fluidized bed is supplied through the interior dispersion plate to the upper fluidized layer. The coal gas which has passed the upper fluidized bed is sent out to piping coupled with a dust removing unit. The temperature of the upper fluidized bed is regulated by the cooler (heat exchanger) to 800° to 950° C. The temperature of the lower fluidized layer is regulated to 900 to 1100° C.
Thus, the desulfurization furnace is divided into the upper and lower fluidized beds, limestone is supplied to the upper fluidized bed, and the temperature of the upper fluidized bed is regulated to 800° to 950° C., whereby non-reactive limestone is reacted with H 2 S and COS in the vicinity of the surface of limestone particles so that H 2 S and COS in gas are fixed to the surface of limestone. The limestone particles whose surface has been changed into CaS is moved to the lower fluidized bed, and then the temperature of the fluidized bed becomes 950° to 1100° C., whereby there occurs such a reaction that CaCO 3 contained in limestone is converted to CaO and CO 2 . Thereafter, the reaction effective area of limestone is increased when CO 2 is released from the interior of the limestone particles, as the result of which H 2 S and COS are fixed to the interior of limestone as CaS.
Setting the temperature of the lower fluidized bed to 900° to 1100° C. enables the reaction speed at which CACO 3 is converted into CaO and CO 2 to be substantially equal to the speed of desulfurization reaction so that CaS production weight per limestone weight can be increased. Since the above-mentioned reaction speed necessary for converting CaCO 3 to CaO and CO 2 is affected by the divided pressure of CO 2 , the reaction speed necessary for converting CaCO 3 to CaO and CO 2 can be adjusted depending on the temperature.
Although the densities of H 2 S and COS in the coal gas in the lower fluidized bed are lowered, the density of H 2 S in the reaction equilibrium gas is increased from the reaction equilibrium of limestone and H 2 S as the temperature goes up, as shown in FIG. 5. After the density of H 2 S approaches to a value of the H 2 S density in the gas of the lower fluidized bed, it is reacted with limestone which is not reactive in the upper fluidized bed at a temperature lower than that of the lower fluidized bed to further reduce the density of H 2 S.
BRIEF DESCRIPTION OF THE DRAWINGS
Other objects, advantages and features of the invention will be apparent when carefully reading the following detailed description in connection with the accompanying drawings, in which:
FIG. 1 is a system diagram of a first embodiment of a coal gasification power generator in accordance with the present invention;
FIG. 2 is a table showing the temperature of a main unit, a mass balance and gas components in accordance with the first embodiment;
FIG. 3 is a system diagram of a second embodiment of coal gasification power generator in accordance with the present invention;
FIG. 4 is a conceptual diagram showing the structure of a gasifying furnace, a desulfurization furnace, and an oxidizing furnace of the first embodiment of the coal gasification power generator;
FIG. 5 is a diagram showing the density of water in gas and hydrogen sulfide after desulfurization;
FIG. 6 is a system diagram of a conventional coal gasification power generator; and
FIG. 7 is a chart comparing the performance of desulfurization between a mode employing a conventional integrated desulfurization gasifying furnace as shown in FIG. 6 and a preferred mode of the present invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
FIG. 1 shows a first embodiment in accordance with the present invention. The first embodiment will be described with reference to FIG. 1. In the first embodiment, air is used as oxidation gas.
Coal 100 and pressurized air 202 are supplied to a gasifying furnace 1. In the gasifying furnace 1, the coal 100 is gasified by the aid of oxygen in the pressurized air 202 and a combustion gas 700 in an oxidizing furnace 4, thereby being converted into a coal gas 500 and char 60a.
The coal gas 500 is transferred to a desulfurization furnace 2 to which limestone 400 is supplied. In the desulfurization furnace 2, a fluidized bed of the limestone 400 is formed, and the coal gas 500 plays the role of fluidized gas in the fluidized bed. The limestone 400 is reacted with H 2 S and COS in the coal gas 500 in such a manner that a part of the limestone 400 is converted into CaS.
After desulfurization, a coal gas 501 is transferred to a dust removing unit 3 by which particles contained in the coal gas 501 are removed. A purpose of removing the particles by means of the dust removing unit 3 is to prevent those particles from wearing a gas turbine blade of a gas turbine 7 and also from being attached to the gas turbine blade.
After desulfurization, a coal gas 502 is sent to a combuster 5. In the combuster 5, the coal gas 502 is burned with pressurized air 203 to produce a combustion gas 800.
The combustion gas 800 is transmitted to the gas turbine 7 which is driven by the combustion gas 800 so that it drives an air compressor 6 and a power generator from which electricity is generated.
A combustion gas 801 in a gas turbine outlet allows a water vapor 30a to be generated by the aid of the high heat of the combustion gas 801 in an emission gas boiler 8. A combustion gas 802, whose temperature is lowered because it is restored by the emission gas boiler 8, is radiated as a combustion gas 803 from a funnel 9 toward the atmosphere.
The char 60a formed in the gasifying furnace 1 is supplied to,an oxidizing furnace 4 through a char transfer unit 15. Limestone 60b containing CaS formed by the desulfurization furnace 1 is supplied to the oxidizing furnace 4 through a desulfurization transfer unit 16. In the oxidizing furnace 4, particles 60c which have been removed from gas 501 by the dust removing unit 3, the char 60a and CaS contained in the desulfurization agent 60b are burned with oxygen contained in pressurized air 204 so that the CaS of the desulfurization agent 60b is oxidized into CaSO 4 . The heat generated in the oxidizing furnace 4 is used to produce water vapor 30b by a heat exchanger 10. The combustion gas 700 is supplied to the gasifying furnace 1 so as to be used as a gasifying agent.
The water vapor 30a which has received heat from the combustion gas 801 by means of the emission gas boiler 8 further receives oxidation reaction heat of char, thereby forming the water vapor 30b which drives a steam turbine 11. The steam turbine 11 drives the power generator which generates electricity. Water vapor which has driven the steam turbine 11 is cooled by a steam condenser 12 into water 30c to be pressurized by a pressure pump 13 and then transferred to the emission gas boiler 8.
The air compressor 6 takes in air 200 and compresses it to produce pressurized air. The pressurized air is distributed to the pressurized air 203 supplied to the combuster 5 and a pressurized air 201 supplied to a gas booster 14. The pressurized air which has been boosted by the gas booster 14 is distributed to the pressurized air 202 supplied to the gasifying furnace 1 and the pressurized air 204 supplied to the oxidizing furnace.
Ashes in coal and limestone after desulfurization are emitted as emission ashes 900 from the oxidizing furnace 4 toward the exterior of this power generator.
A mass balance, temperature and gas components in the major units of the system according to the above-mentioned embodiment of FIG. 1 are shown in FIG. 2.
FIG. 3 shows a coal gasification power generator in accordance with a second embodiment of the invention, which is a case of using oxidation gas oxygen. Differences from FIG. 1 will be described with reference to FIG. 3.
Oxygen gas from an oxygen manufacturing plant 20 is used for an oxidizing furnace oxidation gas 204' and a gasifying furnace oxidation gas 205'. After the combustion gas 802 containing a large amount of CO 2 is cooled and dehydrated by a combustion gas cooler 21, a resultant gas 803 is compressed by the gas booster 14' and then introduced into the gasifying furnace 1 so that it is introduced as a gasifying agent 205' at coal gasification.
FIG. 4 shows one example of the gasifying furnace 1, a desulfurization furnace 2 and an oxidizing furnace 4 in accordance with the present invention. FIG. 4 will be briefly explained in the following. The coal 100 and the pressurized air 200 are supplied to the gasifying furnace 1. In the gasifying furnace 1, the coal 100 is gasified by the aid of oxygen in the pressurized air 200 and the combustion gas 700 in the oxidizing furnace 4 so as to be converted to a coal gas 500a and the char 60a.
A char transfer unit 15a is supplied with an inert gas 1000 through piping. When the inert gas 1000 is supplied intermittently to the char transfer unit 15a, the particles within the piping are fluidized. When the inert gas 1000 is not supplied thereto, the char transfer unit 15a forms a fixed bed. When the particles are fluidized, they are transferred from the gasifying furnace 1 to a hopper 17a. The char 60a has an emission quantity which is controlled by a supply quantity of the inert gas 1000 and its supply intermittent time so that the quantity of the char 60a extracted to the hopper 17a is controlled. The dust of the coal gas 500a is removed by a cyclone 19a. The particles whose dust has been removed by the cyclone 19a are recycled through the char transfer unit 15b from the lower portion of the cyclone 19a within the gasifying furnace 1 by the aid of an inert gas 1001. The coal gas 500b after being subjected to dust removal treatment is supplied to the desulfurization furnace 2 through a dispersion plate 31.
In the desulfurization furnace 2, a fluidized bed of limestone 400 is formed, and the coal gas 500b plays the role of fluidized gas in the fluidized bed. The desulfurization furnace 2 is divided by an interior dispersion plate 32 into an upper fluidized bed 2B and a lower fluidized bed 2A. The limestone 400 is supplied to the upper fluidized bed 2B. The interior dispersion plate 32 reduces the sectional area of the fluidized bed by 50% or less so that a mixing of the particles between the upper fluidized bed 2B and the lower fluidized bed 2A is limited. In the upper fluidized bed 2B, a cooler (heat exchanger) 33 is installed. The cooler 33 cools the particles and gas, and controls the mixing quantity of the particles in the upper fluidized bed 2B and the particles in the lower fluidized bed 2A so that the temperature of the upper fluidized bed 2B is maintained at 800° to 900° C. and the temperature of the lower fluidized bed 2A is maintained to 950° C. The limestone 400 is reacted with H 2 S and COS contained in the coal gas 500b whereby a part of the limestone 400 is changed into CaS. The coal gas 501 after desulfurization is transferred to a dust removing unit (not shown).
A desulfurization agent 60b is extracted from the desulfurization furnace 2 while the extracted quantity of the agent 60b is adjusted by the desulfurization agent transfer unit 16.
The char 60a produced by the gasifying furnace 1 is received by the hopper 17a. In the case where a hopper 17c is under pressure, the char 60a is stored in the hopper 17a until the pressure in the hopper 17c is identical with that in the hopper 17a. After the hoppers 17a and 17c have- the same pressure, a valve 17b is opened whereby the char 60a drops into a hopper 17e. Subsequently, the valve 17b is shut in such a manner that the hopper 17c is pressurized, as the result of which, when the pressure in the hopper 17c is identical with valve 17d is opened so that the char that in the hopper 17e, a valve 17d is opened so that the char 60a drops into the hopper 17e. The char 60a in the hopper 17e is supplied to the oxidizing furnace 4 through a rotary feeder 17f by a given quantity. The limestone containing CaS produced by the desulfurization furnace 2 is supplied to the oxidizing bed 4 by use of hoppers 17a', 17c' and 17e', valves 17b' and 17d', and a rotary feeder 17f', as in the case of the char 60a.
In the oxidizing furnace 4, a fluidized bed is mainly formed by a desulfurization agent. The char 60a and the particles restored by the desulfurization agent 60b and the cyclone 10b are supplied to the fluidized bed 4A through the char transfer unit 15c. The fluidized bed 4A is fluidized by the aid of the air 204 and a water vapor 300 supplied through the dispersion plate 41 from the bottom of the furnace.
In the fluidized bed 4A, the char is rapidly converted into the gas and ashes according to the combustion reaction whereas CaS in the limestone is slowly converted into CASO 4 , as the result of which the fluidized particles of the fluidized bed 4A mainly contain the desulfurization agent.
A heat exchanger is located on a free board of the oxidizing furnace 4. The heat of the particles and the gas which are whirled up from the fluidized bed 4A is absorbed by the heat exchanger, whereby the temperature of the fluidized bed 4A is controlled in the range of 850° to 1050° C., which allows the reaction in which CaS is changed into CaSO 4 to occur, allows the reaction of SO 2 (produced by an auxiliary reaction) with CaO into CaSO 4 to progress, and prevents the ashes or the desulfurization agent from being softened to generate agrome.
The oxidizing furnace 4 is coupled to the cyclone 19b through two branches of piping, and one of the two branches extends from a position in the vicinity of the top of the oxidizing furnace 4, that is, the upper portion of the heat exchanger 10, and the other branch extends from a position which is at the same level as the lower portion of the heat exchanger 10. This is because the quantity of the combustion gas 700a which is transferred from the upper portion of the heat exchanger 10 to the cyclone 10b and the quantity of the combustion gas 700b which is transferred from the lower portion of the heat exchanger 10 to the cyclone 19b are adjusted by a valve 42 attached to one of these branches so that the temperature of the combustion gas 700 supplied to the gasifying furnace 1 is adjusted.
Ashes contained in the limestone and the limestone after desulfurization treatment are exhausted from the furnace bottom of the oxidizing furnace 4 as emission ashes 900, or from the lower portion of the cyclone 19b as emission ashes 901 toward the exterior of this power generator.
According to the present invention, with the above-mentioned structure, coal energy is effectively distributed to the gas turbine and the steam turbine, thereby enabling power generation with a high efficiency.
Further, coal gas produced by the gasifying furnace passes through the fluidized bed of the limestone according to the present invention, as the result of which the sum of the H 2 S density and the COS density in coal gas can be reduced to the chemical equilibrium represented by the following expression.
CaO+H.sub.2 S=CaS+H.sub.2 O
The relationship between the chemical equilibrium density and the water vapor density of the above-mentioned H 2 S reaction is shown in FIG. 5.
According to the present invention, with the above structure, the SO 2 density produced by the oxidizing furnace can be restrained, and the quantity of SOx which is emitted from the system can be reduced due to the reduction effect of the H 2 S density of the above-mentioned coal gas.
FIG. 7 compares the performance of desulfurization between a mode employing a conventional integrated desulfurization gasifying furnace (reference character 1' in FIG. 6) and a preferred mode, as shown in this example, of this invention, which separates the gasifying furnace 1 from the desulfurization furnace 2. The term "sulfur holding efficiency" in this figure is defined as the percentage of sulfur being fixed in char or limestone to the quantity of sulfur initially contained in the coal. The term Ca/S is defined as the molar ratio of S in coal to Ca in limestone. As seen in the figure, the efficiency of desulfurization for the desulfurization separation type of this embodiment is superior to the conventional integrated desulfurization type by approximately 1:5 times.
The foregoing description of preferred embodiments of the invention has been presented for purposes of illustration and description. It is not intended to be exhaustive or to limit the invention to the precise form disclosed, and modifications and variations are possible in light of the above teachings or may be acquired from practice of the invention. The embodiment was chosen and described in order to explain the principles of the invention and its practical application to enable one skilled in the art to utilize the invention in various embodiments and with various modifications as are suited to the particular use contemplated. It is intended that the scope of the invention be defined by the claims appended hereto, and their equivalents. | In a coal gasification power generator, coal gas 500 obtained by gasifying a coal 100 by a gasifying furnace is introduced into a desulfurization furnace in which the coal gas 500 is desulfurized by limestone 400. A coal gas 501 after desulfurization is burned by a combuster 5 after it has passed through a dust removing unit 3 so that high temperature combustion gas 800 is supplied to a gas turbine. The gas turbine 7 drives a power generating unit. Exhaust gas 801 from the gas turbine is supplied to an exhaust gas boiler 8. Char 60a produced in the gasifying furnace and limestone 60b containing CaS emitted from the desulfurization furnace are burned in an oxidation furnace, and by using the resultant combustion gas, water vapor introduced from the exhaust gas boiler 8 is heated by a heat exchanger, and thereafter it is supplied to the gasifying furnace as a gas. With the above construction, chemical energy possessed by the coal is effectively converted into electric energy, and also the rate of desulfurization of coal gasifying gas is improved thereby reducing emitted sulfur oxide. | 5 |
BACKGROUND OF THE INVENTION
This invention concerns a phase change material which melts and freezes at a temperature below 32 degrees F. and can be utilized to store coolness in ice bank equipment such as that disclosed in co-applicant Calvin MacCracken's U.S. Pat. Nos. 4,294,078 and 4,403,645. In particular it relates to an improved eutectic composition, and its method of use, having a melting-freezing temperature remaining constant at about 28 degrees F. providing optimum neucleation and minimal precipitation during freezing.
Co-applicant Maria Telkes in her U.S. Pat. Nos. 2,667,664 and 2,989,856 disclosed a phase change material rich in anhydrous sodium sulfate (at least one-third by weight) with a small amount of sodium tetraborate decahydrate (i.e. borax) as a neucleating agent, both added to water. That composition was intended for heat storage rather than coolness storage and had a melting-freezing temperature of about 90 degrees F. The salt was not in the solubility range in water so that a substantial amount of it precipitated upon melting unless a strong gel or thixotropic agent was employed, as described in Telkes' U.S. Pat. No. 3,986,969. The heat of fusion of the Telkes' prior art eutectic was in the order of 103 Btu's per pound and its volumetric storage capacity was approximately 7280 Btu's per cubic foot. Another eutectic of anhydrous sodium sulfate decahydrate mixed with chlorides or potassium nitrate having melting-freezing temperatures above 40 degrees F. for coolness storage is disclosed in Telkes' U.S. Pat. No. 2,989,856.
The object of the present invention is to provide a eutectic composition for coolness storage in ice bank equipment such as that described in the aforementioned MacCracken patent. The eutectic is to have a constant melting-freezing temperature of about 28 degrees F, a heat of fusion substantially higher than that of the prior art, improved solubility in water to reduce precipitation, and optimum nucleation during freezing.
SUMMARY OF THE INVENTION
The invention provides a eutectic composition consisting essentially of approximately 3.3% to approximately 4.3% by weight of sodium sulfate, approximately 0.5% to approximately 1.5% by weight of sodium tetraborate decahydrate, and the balance water. A buffering acid may be included to reduce alkalinity, and sodium bisulfate is preferred for that purpose comprising approximately 0.3% to approximately 0.9% by weight of the composition.
In a preferred form of the eutectic of the invention the sodium sulfate is approximately 3.8% by weight and the sodium tetraborate decahydrate is approximately 1.0% by weight of the composition.
The invention also covers a dry particulate mixture consisting essentially of approximately 65% to approximately 90% by weight of anhydrous sodium sulfate, approximately 10% to approximately 25% by weight sodium tetraborate pentahydrate, and approximately 6% by weight to approximately 16% by weight of sodium bisulfate. Preferably these percentages are 75% by weight of anhydrous sodium sulfate and 15% by weight of sodium tetraborate pentahydrate, and 10% by weight of sodium bisulfate.
A method of making a eutectic composition for coolness storage is also provided by the invention. It includes the step of adding to water at ambient temperature sufficient quantities of dry particulate sodium sulfate and sodium tetraborate pentahydrate to produce a mixture consisting essentially of 3.3% to approximately 4.3% by weight of sodium sulfate and approximately 0.5% to approximately 1.5% by weight of sodium tetraborate decahydrate (the pentahydrate becomes decahydrate, or borax, when mixed with the water). During the addition of this dry particulate material to the water, the method of the invention provides that the water is to be stirred. The method also provides for the addition of a buffering acid to reduce alkalinity, preferably sodium bisulfate comprising approximately 0.3% to approximately 0.9% by weight of the solution.
The eutectic composition of the invention, produced by the method of the invention, has a very stable melting and freezing temperature of 28 degrees F. which is ideal for cooling storage. The heat of fusion of the composition is approximately 142 Btu's per pound which is substantially higher than that of the Telkes' prior art eutectic described above. The salt of the eutectic of the invention is entirely within the solubility range of water and consequently little of it precipitates during mixture, so that a gel or thixotropic agent is not required. Any limited amount which may precipitate during freezing is easily remixed and dissolved by the recommended stirring. The sodium tetraborate decahydrate serves as an excellent nucleating agent minimizing subcooling during initial freezing. The high percentage of water in the eutectic solution results in formation of ice crystals of a regular pattern, which due to the high thermal conductivity of ice as compared to water (about 4 to 1), provides higher thermal conductivity during both freezing and melting. This is of great importance in the overall efficiency and economy in a thermal storage ice bank.
The preferred addition of an acid to reduce alkalinity is important because a high pH solution causes carbon dioxide to be absorbed by the air and precipitate carbonates. With water hardness in the range of five to six grains per gallon (i.e. medium-hard) with a pH of 7.5 to 8.0 it is desirable to add approximately 0.3% to 0.9% by weight of sodium bisulfate as a buffering acid. Sodium bisulfate, or NaHSO 4 , which is preferred to reduce alkalinity is sometimes referred to as sodium acid sulfate, sodium hydrogen sulfate or sodium pyrosulfate. Very little of it need be added and therefore its cost and shipping weight is minimal. Since it is mixed with sodium sulfate there are less possible combinations that could be formed between them to precipitate.
The present invention does not utilize sodium tetraborate decahydrate, commonly known as borax, as the nucleating agent. In the initial dry particulate form but rather sodium tetraborate pentahydrate, which turns to borax when mixed with water. Dry sodium tetraborate pentahydrate is cheaper, lighter and more stable than borax and does not cake up in shipment but remains in particulate granular form for easy pouring into the water in the tank.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is an elevation of a thermal storage device in which the eutectic of the invention and its method may be employed; and
FIG. 2 is a top plan view of the tank of FIG. 1.
DESCRIPTION OF PREFERRED EMBODIMENT
The ice bank shown in the drawings includes an outer skin of aluminum foil 10 covering thermal insulation 11 which in turn encloses a cylindrical tank 12 of rigid plastic such as polyethylene. An insulated base 13 defines the bottom of the tank and the top comprises a molded lid 14 with a foam insulation core. The tank 12 may be somewhat more than eight feet high and over seven feet in diameter. Coiled within it are extended lengths of plastic heat exchange tubing, perhaps of five-eights inch outside diameter, laid in a series of flat spirals with the turns in a given spiral and the spirals themselves held apart by spacer strips 15 as described in co-applicant Calvin MacCracken's U.S. Pat. No. 4,671,347. An anti-freeze heat transfer liquid such as ethylene glycol is circulated through the tubing to either melt or freeze a phase change material filling the tank up to a level indicated by the reference numeral 16.
To charge the ice bank water is added through a central port 17 in the lid 14 to rise to the level indicated at 16 in FIG. 1 submerging all of the levels and spirals of the heat exchange tubing. With the use of a funnel 18 a dry particulate mixture as described below is added while the water is stirred. Closed circulation pumping achieves the stirring action during charging, as for example by a suction pump 19 temporarily used to draw water through an outlet pipe 20 from a second port 21 in the lid 14 and returning the water through the central fill port 17 by a fill pipe 22 extending almost to the bottom of the tank and equipped with outlet holes 23 at various levels.
EXAMPLE
The tank of an ice bank was filled to the level 16 with 1620 gallons or 13,328 pounds of water known to have a hardness of between 5 or 6 grains per gallon, which is medium-hard, and a pH of between 7.5 and 8.0. The pump 19 was then activated to circulate the water up through the pipe 20 and down through the pipe 22 so that a gentle stirring was achieved as the additives were introduced into the funnel 18. A dry particulate mixture was prepared of 75% by weight of anhydrous sodium sulfate or Na 2 SO 4 , 15% by weight of sodium tetraborate pentahydrate and 10% by weight of sodium 0185 bisulfate or NaHSO 4 .
Approximately 710 pounds of this dry particulate mixture of sodium sulfate, sodium tetraborate pentahydrate and sodium bisulfate was slowly poured into the gently stirred water to produce a eutectic composition of 3.8% by weight of sodium sulfate, 0.1% by weight of sodium tetraborate decahydrate (the pentahydrate changed to decahydrate upon dissolution in the water) and 0.5% by weight of sodium bisulfate. This addition yields 1620 gallons or 14,038 pounds of eutectic solution with a liquid density of 1.04. Sodium tetraborate pentahydrate is preferred in the initial powdered form over decahydrate because, as noted previously, pentahydrate is less expensive, lighter in weight and does not cake up in shipment. Once the pentahydrate is in the water the ions gradually become the same as if it had been added in the form of decahydrate or borax. The sodium bisulfate acts as a buffering agent to lower the pH of the water to approximately 4.5.
This 28 degree F. eutectic of the invention is distinguishable over the prior art Telkes' 90 degree F. eutectic as follows:
______________________________________ 90 Degree eutectic 28 Degree eutectic______________________________________Btu/lb. capacity 80 142Btu/cu.ft.capacity 7280 8500Density re water 1.46/1.465 1.03/.96liquid/solidExpansion percent <1% 7.5liquid/solidSpecific heat .60/.40 .85/.50liquid/solidSolubility 85% 99% to 100%______________________________________
It should be noted that water has a heat of fusion of 144 Btu/lb. and an expansion percentage of 9%. The cooling storage per unit volume of the eutectic of the invention is 8524 Btu/ft. 3 as compared to that of water which is 8177 Btu/ft. 3 , an increase of 4.2%. | A eutectic composition for coolness storage and its method of making wherein a dry particulate mixture of sodium sulfate and a lesser amount of sodium tetraborate pentahydrate is added to water while the water is stirred, together with a small amount of a buffering acid to reduce alkalinity. | 2 |
CROSS REFERENCE TO RELATED APPLICATIONS
[0001] This application is a divisional of U.S. patent application Ser. No. 10/380,392, pending, which is the National Phase of International Application PCT/EP01/10199 filed Sep. 4, 2001 which designated the U.S and which claims priority to U.S. Pat. App. No. 60/231,596 filed Sep. 11, 2000. The noted applications are incorporated herein by reference.
BACKGROUND OF THE INVENTION
[0002] In the transport industries (for example, the automotive, rail and aerospace industries), it is common practice to produce large, dimensionally accurate master models. These models are used by engineers for conceptual design of the individual component parts of the final product.
[0003] The state-of-the-art often involves a “building block” approach wherein multiple boards are glued together to produce a rough model structure and then are machined to form the desired shape (illustrated in FIG. 1 ). This approach, however, is labor intensive and requires precision operations, leading to high cost, and moreover results in a model having bondlines at the surface, an appearance which is aesthetically undesirable.
[0004] There is thus a need in the industry for a model and method of making a model that is characterized by low cost and a smooth seamless surface free of bondlines. U.S. Pat. Nos. 5,707,477 and 5,773,047 describe a method for making prepreg parts for use in the aerospace industry where pliable solid paddies prepared from syntactic epoxy material are hand-applied to a block made by stacking successive layers of aluminum honeycomb core, which entire resulting structure is heat cured to effect cure of the paddies. However, this approach is labor intensive in that it involves hand application of the pliable solid paddies to the honeycomb core as well as requiring heating of the entire structure in order to cure the applied paddies. The resulting models are also of relatively high density.
[0005] There thus remains continued need in the art for a model and method of producing same where the model is characterized by lower production cost, lower weight and a more uniform surface having improved smoothness and free of bondlines.
SUMMARY OF THE INVENTION
[0006] The present invention is directed to a model and a method of making a model which meets these needs of industry. The method of making a seamless model free of bond lines in accordance with the present invention includes the sequential steps of providing a substructure having an exposed outer surface, applying a modeling paste to the outer surface of the substructure in the form of a continuous layer, curing the continuous layer of applied modeling paste, and machining said cured layer of modeling paste to the desired contour. This method is termed herein as “net size casting” using a “seamless modeling paste” (SMP).
[0007] The modeling paste of the invention is mechanically frothed syntactic foam prepared by injecting inert gas with mechanical stirring into a resin composition, which is preferably a low temperature curable thermoset. Most preferably, the composition is either a formed polyurethane or epoxy froth-forming composition containing microballoons. The polyurethane composition exemplified herein comprises (1) an organic polyisocyanate component; (2) a polyol component comprising (a) greater than 50%, by weight of a high molecular weight polyol and (b) less than 50%, by weight, of a low molecular weight polyol; and (3) a chemical thixotropic agent in an amount sufficient to induce thixotropic properties. The preferred epoxy composition comprises (1) an epoxy resin; (2) a thixotropic agent in an amount sufficient to induce thixotropic properties; and (3) a hardener comprising (a) at least one polyethyleneimine and (b) at least one other amine having at least two amino hydrogen groups, the combined amounts of (a) and (b) being sufficient to effect cure of the epoxy resin.
FIGURES
[0008] FIG. 1 illustrates an example of the prior art “building block” modeling method by gluing multiple boards.
[0009] FIG. 2 illustrates a cross-section of a seamless model free of bond lines produced in accordance with the present invention.
DETAILED DESCRIPTION
[0010] The undersized support structures used in accordance with the present invention, and methods of making said structures, are known in the art and may be of the same type of structure typically produced as a back support for conventional board models. Said structure is used as a core onto which the modeling paste is applied. Examples of materials from which the support structure is made include, but are not limited to, natural wood and low-density foams made for example from polystyrene, polyurethane or epoxy materials. One example of such low-density core is Dow HD 3000, a 0.03 density expanded polystyrene.
[0011] Referring to FIG. 2 , a layer of modeling paste 2 is applied to the outer surface of the substructure 1 . Preferably, the layer of modeling paste is dispensed onto the substructure surface with a high-output meter-mix machine in the form of a continuous layer. The paste is preferably applied at a thickness of from about 0.5 to about 1.5 inch thick, more preferably at about 0.75 inch thick. The paste is then cured.
[0012] Cure of the curable resin composition can be effected in accordance with conventional practice in the particular application. In general, the composition can be allowed to gel (set) at ambient temperature or heated moderately in accordance with conventional practice to accelerate setting. Subsequently, completion of cure may be effected at ambient temperature, moderately elevated temperature or higher temperature as required. Typically, room temperature cure is preferred.
[0013] After curing, the resin layer is machined to the final contour by use of a cutter 3 . Typically, approximately 0.25 inch of material is removed during machining. The surfaces may be sealed with a sealant before the model is put into production.
[0014] The seamless master modeling paste which is dispensed onto the outer surface of the substructure is comprised of mechanically frothed syntactic foam. The foam is prepared by injecting inert gas with mechanical stirring into a formed froth-forming composition comprising the curable resin composition, microballons and any other optional additives.
[0015] The mechanically frothed syntactic foam used in accordance with the present invention is required to exhibit good non-slump and sag resistance properties when laid horizontally oriented on a vertical surface. Typically, a minimum sag resistance of a one inch thickness on a vertical surface is required. It has been found that mechanically frothed syntactic foams made from certain polyurethane, epoxy and polyester froth-forming mixtures particularly meet these criteria.
[0016] Examples of suitable curable polyurethane froth-forming mixtures include, but are not limited to, those comprising (1) an organic polyisocyanate component; (2) a polyol component comprising (a) greater than 50%, by weight, of a high molecular weight polyol and (b) less than 50%, by weight, of a low molecular weight polyol; and (3) a chemical thixotropic agent in an amount sufficient to induce thixotropic properties. Preferably, the low molecular weight polyol (b) is present in an amount of less than 40%, by weight, based on the total weight of the combined polyol component. The polyisocyanate and polyol components are conveniently liquid under ambient temperature and pressure conditions, with the polyisocyanate component having a viscosity in the range of 500-3000 cps and the polyol component having a viscosity of less than 30,000 cps in order to ensure optimal throughput in the mixing and dispensing apparatus. However, both components may have greater viscosity, for example up to 60,000 cps, if proper metering pumps are employed.
[0017] Suitable organic polyisocyanates (1) which are useful in the invention include any of those commonly employed in making polyurethane plastics including polyarylisocyanates such as polymethylene polyphenyl isocyanate, 4,4′-diphenylmethane diisocyanate and modifications thereof, for example, containing carbodiimide linkages, toluene diisocyanate, phenylindane diisocyanate, aliphatic polyisocyanates such as hexamethylene diisocyanate, isophorone diisocyanate, 2,2,4-trimethylhexamethylene diisocyanate, and blends thereof. Polymeric 4,4′-diphenylmethane diisocyanate is preferred.
[0018] Suitable high molecular weight polyols (2a) include those having hydroxyl numbers of less than 300, preferably between 100 and 300. Particularly suitable are polyether triols, including aliphatic alkylene glycol polymers having an alkylene unit composed of at least two carbon atoms. Typical ones are prepared through the polymerization of such alkylene oxides as ethylene oxide, propylene oxide, butylene oxide and tetrahydrofuran, and di- and polyfunctional alcohols such as water, propylene glycol, glycerol, trimethylol propane, hexanetriol, pentaerythritol and sucrose. Applicable materials will generally have molecular weights ranging from 500-7000 preferably between 500 and 1700. A typical polyether triol is available from Olin Corp., under the name POLY-0 30-280.
[0019] The low molecular weight polyols (2b) include those having hydroxyl numbers of at least 300, preferably between 300 and 1000, and more preferably between 350 and 800. Particularly suitable are amine-based polyols generally have an equivalent weight of from 30 to 6000 and a viscosity of from 1.0 to 20,000 centipoises at 25 to 60° C. Preferred are those having a molecular weight of between 50 and 400, more preferably, between 200 and 350. A wide variety of aromatic and aliphatic polyamines may form part of the amine-based polyols, such as di- and polyamines including ethylenediamine, triethanolamine and toluenediamine, to be reacted with, for example, the alkylene oxides, noted above. Amine-based triols are preferred. Typical amine-based polyols are available from Texaco Corp., under the designation THANOL SF 265 and from BASF Corp. under the designation PLURACOL 355.
[0020] The chemical thixotropic agent (3) imparts chemical thixotropy to the mixture of components (1) and (2) such that sufficient sag resistance is achieved during application of the final paste to the support structure, which is believed to be caused by the formation of adducts from the fast chemical reaction between the isocyanate and amine groups. It is important that chemical thixotropy is induced after mixing, foaming and dispensing onto the substructure as premature chemical thixotropy could lead to gelation in the mixing head. Typical examples of such chemical thixotropic agents are aliphatic, cycloaliphatic, aromatic, araliphatic and heterocyclic amines, including, but not limited to, 4,4′-methylenedianiline, m-phenylenediamine, 4,4′-methylenebis(2-ethylbenzeneamine), isophoronediamine and most particularly diethyltoluenediamine. The amount of thixotropic agent required to induce thixotropic properties may depend on the nature of the specific polyurethane and the specific thixotropic agent used. The amount is generally from 1 to 10%, preferably from 2 to 6%, by weight based on the weight of the polyisocyanate (1).
[0021] The polyurethane systems are prepared by admixing the polyisocyanate with the polyols. The microballoons and any other optional additives are generally included with the polyols. Generally stoichiometric amounts of polyisocyanate and polyol are utilized, with the possibility of deviating from the stoichiometric amount by utilizing up to about 2% excess polyol.
[0022] In order to meet the overall requirements for an acceptable cured polyurethane foamed modeling stock, the cured composition should have a heat deflection temperature (HDT) over 40° C., and preferably over 50° C., and a coefficient of thermal expansion (CTE) of less than 80×10 −6 in/in/° C. in the −30 to 30° C. range and preferably less than 60×10 −6 in/in/° C. Cured epoxy foamed modeling stock should also meet these criteria.
[0023] Also particularly suitable for use in the mechanically frothed syntactic foams are curable epoxy resin/hardener mixtures, as described, for example, in U.S. Pat. No. 6,077,886, issue date of Jun. 20, 2000, incorporated herein by reference, which comprise (1) an epoxy resin, (2) a thixotropic agent in an amount sufficient to induce thixotropic properties, and (3) a hardener comprising (a) at least one polyethyleneimine and (b) at least one other amine having at least two amino hydrogen groups, the combined amounts of (3)(a) and (3)(b) being sufficient to effect cure of the epoxy resin.
[0024] The epoxy resin (1) may consist of one or more epoxy resins which are themselves liquid or may be a liquid mixture of one or more solid epoxy resins with one or more liquid epoxy resins or may be one or more solid epoxy resins dissolved in a diluent such as a diluent conventionally used in epoxy resin compositions. The epoxy resin may be a polyglycidyl ether of a polyhydric alcohol such as 1,4-butanediol or 1,3-propanediol or, preferably, a polyglycidyl ether of a polyhydric phenol, for example a bisphenol such as bis(4-hydroxyphenyl)methane (bisphenol F) or 2,2-bis-(4-hydroxyphenyl)propane (bisphenol A) or a novolak formed from formaldehyde and a phenol such as phenol itself or a cresol, or a mixture of two or more such polyglycidyl ethers. Polyglycidyl ethers of bisphenol A are especially preferred. The epoxy resin, particularly where it comprises a solid epoxy resin, may contain one or more epoxy-functional diluents, usually monoepoxides, or non-epoxide diluents, such as the monoepoxide and non-epoxide diluents conventionally used in curable epoxy resin compositions.
[0025] The thixotropic agent (2) is preferably a thixotropic agent which, it is believed, relies largely on interparticle hydrogen bonding to achieve its thixotropic effect, especially a hydrophilic fumed silica. The amount of thixotropic agent required to induce thixotropic properties may depend on the nature of the specific epoxy resin and specific thixotropic agent used. This amount is generally from 1 to 20%, preferably from 3 to 15%, by weight based on the weight of the epoxy resin (1).
[0026] The polyethyleneimine (3)(a) may have a molecular weight (Mw) from 700 to 1,000,000 or more, preferably from 5000 to 750,000, especially from 25,000 to 750,000, particularly about 750,000. Such polyethyleneimines are commercially available or may be prepared from ethyleneimine by known procedures.
[0027] The amount of polyethyleneimine is generally chosen so that the epoxy resin composition of the invention does not flow during a desired time after the formation of the composition. Preferably, the amount of polyethyleneimine is such that the epoxy resin composition does not flow for at least 60 minutes after formation thereof. In certain specific embodiments of the invention, the amount of polyethyleneimine is such that the epoxy resin composition does not flow prior to gelation thereof, which in some instances requires several hours. The amount of polyethyleneimine needed to impart non-flow properties for a given time can be readily determined by simple experiment. For compositions of the invention containing the especially preferred components (1), (2) and (3)(b) described herein, an amount of polyethyleneimine from 0.2 to 2 parts by weight per 100 parts by weight of the epoxy resin is preferred.
[0028] As examples of amines suitable for use as the amine hardener (3)(b) there may be mentioned those aliphatic, cycloaliphatic, aromatic, araliphatic and heterocyclic amines known as hardeners for epoxy resins, including: alkylenediamines such as ethylenediamine or butane-1,4-diamine; polyalkylenepolyamines such as diethylenetriamine, triethylenetetramine, tetraethylenepentamine, dipropylenetriamine or tripropylenetetramine; N-hydroxyalkyl derivatives of polyalkylene polyamines such as N-(hydroxyethyl) diethylenetriamine or mono-N-2-hydroxypropyl derivative of triethylenetetramine; polyoxyalkylenepolyamines such as polyoxyethylene—and polyoxypropylene-diamines and triamines; N,N-dialkylalkylenediamines such as N,N-dimethylpropane-1,3-diamine or N,N-diethylpropane-1,3-diamine; cycloaliphatic amines having an amino or aminoalkyl group attached to the ring, such as 3-aminomethyl-3,5,5-trimethylcyclohexylamine (isophoronediamine); aromatic amines such as bis(4-aminophenyl)methane or bis(4-aminophenyl)sulphone; amine-terminated adducts of epoxy resins with aliphatic, cycloaliphatic or araliphatic amines as hereinbefore described; N-aminoalkyl-piperazines such as N-(2-aminoethyl)piperazine or N-(3-aminopropyl)piperazine; and polyaminoamides, for example reaction products of polyalkylenepolyamines such as those hereinbefore mentioned with polymerised unsaturated fatty acids, e.g. polymerised vegetable oil acids such as dimerised or trimerised linoleic or ricinoleic acids; or a mixture of two or more of such amines.
[0029] Aliphatic and cycloaliphatic amine hardeners are usually preferred for use as component (3)(b) of the composition, including N-hydroxyalkyl derivatives of polyalkylene polyamines, particularly a mono-N-2-hydroxypropyl derivative of triethylenetetramine, and mixtures thereof with polyaminoamide reaction products of polyalkylenepolyamines and polymerised vegetable oil acids and the amine functional reaction products of amines and epoxy group containing compounds. The amount of (3)(b) is preferably such that (3)(a) and (3)(b) together provide from about 0.75 to 1.25 amino hydrogen equivalents per 1,2-epoxide equivalent of the epoxy resin (1).
[0030] The epoxy resin composition may be formed conveniently by stirring a preformed mixture of (1) and (2) together with a preformed mixture of (3)(a) and (3)(b). The thixotropic agent may also be conveniently present in the hardener mixture.
[0031] The mechanically frothed syntactic foam used in accordance with the present invention may also be made from a polyester froth-forming mixture. Polyesters and formation thereof are well known in the art. The same general procedure followed for forming the polyurethane and epoxy froth forming mixture applies for polyesters as well, incorporating an agent to induce chemical thixotropic properties for achieving sufficient sag resistance.
[0032] The seamless master modeling paste prepared in accordance with the present invention contains a relatively uniform distribution of microballoons or hollow microspheres. Hollow microspheres are usually hollow thermoplastic spheres composed of acrylic type resins such as polyacrylonitrile and polymethylmethacrylate, acrylic modified styrene, polyvinylidene chloride, copolymers of styrene and methyl methacylate, and the like; thermosetting resins such as phenolic resins, epoxy resins, urea resins and the like; or hollow glass, silica, ceramic or carbon spheres that are very light in weight and act as a lightweight filler in the syntactic foam. Thermoplastic microballoons are preferred. Illustrative examples of suitable microballoons include, but are not limited to, Exapancel, available from Akzo Nobel Corporation; Phenolic microballoons, available from CQ Technology Corporation; and Matsumoto microspheres available from Yusht-Seiyaku Company. These microballoons preferably have a diameter of about 5 to about 250 micrometers. The microballoons, or hollow microspheres, suitable for use in the invention are conventional in the art and methods for production of these microballoons are well known. Such microballoons are readily available commercially. These microballoons can be compressed somewhat when subjected to external pressure. However, they are relatively fragile and will collapse or fracture at high pressures. Therefore, there is a pressure range under which the microballoons can effectively operate. The microballoons facilitate machining, lead to reduced density and reduce the coefficient of thermal expansion. The surface of the microballoons may be treated suitably for better compatibility with the resin composition.
[0033] The microballoons are used in an amount sufficient to produce products of uniform density, but not too much as to produce difficulty in mixing such that nonhomogeneous products are produced. Suitable amounts are about 0.5 part to about 5 parts, based on 100 parts of the resin, preferably about 1 part to about 3 parts, per 100 parts of resin. The microballoons may be conveniently added with the hardener component, or they may be added with the resin component.
[0034] The formed froth-forming composition of the invention may also contain minor amounts of accelerators and additives conventionally used in the particular application, such as diluents, fillers (such calcium carbonate), fibers, pigments, dyes, fire retardants, antifoaming agents, wetting agents and polymeric toughening agents. Of particular interest is the addition of molecular sieves, which function as moisture scavengers, and are well known to those skilled in the art, being zeolites with open-network structures. Also of particular interest is the addition of surfactants or antifoaming agents such as a silicone surfactant like Dabco DC 197 Surfactant, available from Air Products, with others being well commercially available and well known to those skilled in the art. It has also been found that the addition of calcium stearate improves the machinability of the cured material and thus addition thereof is advantageous. These auxiliary materials may be conveniently added with the hardener component, or they may be added with the resin component.
[0035] Techniques for producing mechanically frothed syntactic foams are known in the art. For example, the article “Mechanically Frothed Urethane: A New Process for Controlled Gauge, High Density Foam”, by Marlin et al., Journal of Cellular Plastics, November/December, 1975, describes such techniques. For example, mechanically frothed polyurethane foams are prepared by mechanical incorporation of an inert gas such as air into the isocyanate and polyol mixture, followed by polymerization to form the polyurethane foam. This is unlike the conventional polyurethane foam where foaming and polymerization occur simultaneously. A surfactant is employed in the formulation in order to permit the generation of froth, and the urethane polymerization is delayed through the expansion step and takes place after the froth has been applied to the substrate. The amount of air in the froth determines the density and consistency. The basic equipment is simple wherein the froth is generated continuously in a mixer equipped with blades to generate shear for dispersing the inert gas in the liquid mixture of isocyanate and polyols. The polyol component, which contains surfactant, additive(s) and filler(s) is metered as one stream. The isocyanate is metered as a separate stream, and inert gas is metered through a third inlet to achieve a given density. Machines for processing the foams are commercially available and are known in the field. Mechanically frothed epoxy and polyesters foams are prepared in a similar manner.
[0036] Inert gases which are suitable for use in accordance with the invention include those that are gaseous at room temperature and preferably not liquefied at −30° C., and further that are not reactive with the resin and hardener components. They include, for example, air, nitrogen gas, carbon dioxide gas and the like.
[0037] Dispersing of inert gas is carried out by mechanical frothing where the inert gas is introduced, under mechanical stirring, into the liquid phase comprising the resin, hardener, microballoons and optional additives to obtain a foamed froth-forming composition containing therein the inert gas substantially homogeneously distributed.
[0038] The amount of the inert gas introduced into the foamed resin-forming composition may be varied, particularly by use of a flow meter, according to the desired properties of the final product. In general, suitable amounts include about 10% to about 70% by volume, preferably about 20% to about 60% by volume. The bulk density of the resulting cured articles is usually 0.3 to 0.9 g/cm 3 , preferably 0.4 to 0.8 g/cm 3 .
[0039] Conveniently, separate tanks are filled with the resin and hardener. The application of low pressure to the tanks facilitates pumping of the materials. Gear tanks deliver the resin and hardener from the tanks to the mix block where the resin, hardener and inert gas are mixed under high shear. The compressed air is injected directly into the mix block. A dynamic mixer, with a hose attached thereto, and chamber are attached to the mix block. The amount of compressed air injected into the mix chamber is controlled with a flow meter, which allows for controlled variances in density of the dispensed material. The residence time in the mix block, the high speed of mechanical stirring to dispense the inert gas finely into the mixture and the length of the hose attached to the chamber influence how well the injected air is homogeneously dispersed into the resin and hardener mixture.
[0040] The resulting frothed syntactic resin composition containing therein the inert gas is useful as a seamless master modeling paste, which is dispensed onto the substructure. Curing thereof can be carried out as described hereinabove.
[0041] Machining or cutting can be carried out using conventional tools or cutting machines, such as milling machines, machining centers and the like, into the desired shape. Of particular interest is the use of a computer numerical control (CNC) machine. The shaped article can be used modeling material, and is useful for the production of master models, design models, tracing models and prototype tools.
[0042] From the foregoing description, it is apparent to those skilled in the art that the total fabrication cost of a model using the method of the present invention is more economical than the conventional method of using wood or epoxy synthetic foam model blocks. An additional and important advantage is a resulting model surface that is seamless and free of bondlines.
[0043] This method is further advantageous in that the amount of syntactic material used is greatly reduced over the conventional method since only a thin layer is dispensed onto the substructure surface. Since syntactic materials are inherently hygroscopic, their moisture absorption causes some dimensional change over time. By minimizing the amount of syntactic material used, the dimensional change as the result of moisture absorption is thereby reduced.
[0044] In addition to the advantages mentioned above (namely lower and more uniform density, better machinability, smoother surface characteristics, and much greater overall efficiency), the seamless master paste produced in accordance with the present invention exhibits low linear shrinkage and produces even large models that hold high tolerances. The finished article has excellent edge strength, cured shore hardness, flexural strength, heat deflection temperature, compressive strength as well as coefficient of thermal expansion.
[0045] The present invention is illustrated by reference to the following Examples, which are not intended to limit the scope of the present invention in any manner whatsoever. All parts and percentages are provided on a weight basis unless indicated otherwise.
EXAMPLE 1
[0046] This example illustrates the preparation of a typical polyurethane seamless master modeling paste of the invention.
[0047] The formulation noted in the Table 1 below is prepared by charging the hardener system containing the polyols, microspheres and optional components to a mixing tank and mixing at low speed for 15-30 minutes. A second tank is filled with the isocyanate resin component, and a third tank filled with compressed air is provided. The hardener system and resin component are delivered to a mix block by use of a gear pump, with low pressure (5-10 psi) being applied to the tanks to facilitate pumping of the materials. The compressed air is injected directly into the mix block. In the mix block, the materials and compressed air are homogeneously distributed by using a dynamic mixer under high shear (about 6900 rpm) with a residence time of 2-5 seconds. Residence time is the time in the mixer, which varies inversely with flow rate. For easy control of the density of the dispensed paste, the amount of compressed air injected into the mix chamber is regulated with a flow meter. In this formulation, air reading is 26 ml/min.
[0048] The paste is dispensed onto the substructure at a thickness of about one inch and cured at ambient temperature for at least 10 hours. The crude article is shaped to its final contour by use of a Computer Numerical Control (CNC) machine.
[0049] The paste is evaluated as follows. The sag resistance of the paste is measured prior to curing by dispensing the paste at a thickness of 0.75 to 1.5 inches horizontally on a vertical surface. A measurement of 0.75-1.5 inch is desirable, and indicates that the material sags or slumps only this much. The density, heat deflection temperature (HDT), 66 psi load and coefficient of thermal expansion (CTE), over −30° C. to +30° C., of the paste are measured at 25° C. after curing at ambient temperature for a minimum of 24 hours. Density is measured in accordance with ASTM D792; HDT, with ASTM D648; and CTE, with ASTM DE831.
[0000]
TABLE 1
Formulation 1
(pts by weight)
Hardener System
Low molecular weight polyol 1
21.29
High molecular weight polyol 2
34.73
Thermoplastic microspheres 3
1.43
Molecular sieve powder 4
4.86
Calcium carbonate
29.53
Calcium stearate
2.86
Diethyl toluene diamine
4.00
Reactive colorants
0.55
Silicone surfactant 5
0.75
Resin
Polymeric MDI 6
100.00
Reaction Ratio
58/100
Properties
Sag Resistance (uncured paste)
0.75-1.5
inch
Density (cured)
0.56
g/cm 3
HDT (cured)
72°
C.
CTE (cured)
54.4 × 10 −6
in/in/° C.
1 Poly-G 37-500, from Arch Chemicals
2 Poly-G 30-280, from Arch Chemicals
3 Expancel 551 DE, from Akzo Nobel
4 Molecular Sieve Type 3A, from UOP
5 Dabco DC 197 Surfactant, from Air Products
6 Polymethylene polyphenyl isocyanate, functionality of 2.7 (CAS No. 9016-87-9
[0050] The data illustrate the excellent performance characteristics of the pastes prepared in accordance with the present invention. Notably, the paste of the invention gives excellent sag resistance properties.
COMPARATIVE EXAMPLE 1
[0051] This example illustrates the preparation of a comparative polyurethane formulation.
[0052] The same general procedure of Example 1 is followed, except that the formulation noted in Table 2 below is used. The comparative polyurethane formulation is the same as for Example with the exception that the diethyl toluene diamine is omitted. The properties of the paste so prepared show that this formulation is not suitable for the preparation of a seamless master modeling paste due to the poor dispensing characteristics as indicated by the low resistance to sag of the dispensed paste. Sag resistance is measured as in Example 1.
[0000]
TABLE 2
Comparative Formulation 1
(pts by weight)
Hardener System
Low molecular weight polyol 1
22.18
High molecular weight polyol 2
36.20
Thermoplastic microspheres 3
1.49
Molecular sieve powder 4
5.06
Calcium carbonate
30.77
Calcium stearate
2.98
Diethyl toluene diamine
—
Reactive colorants 5
0.57
Silicone surfactant 6
0.75
Resin
Polymeric MDI 7
100.00
Reaction Ratio
54/100
Properties
Sag Resistance
>1.5 inch*
*This material exhibits virtually no sag resistance.
EXAMPLE 2
[0053] This example illustrates the preparation of further typical polyurethane seamless master modeling pastes of the invention. The formulations noted in Table 3 below are prepared in the same general manner as in Example 1, with the exception that the amounts of various components are varied. The properties of the paste so prepared show that these formulations are suitable for the preparation of a seamless master modeling paste due to the excellent dispensing characteristics as indicated by the high resistance to sag of the dispensed paste. Sag resistance is measured as in Example 1.
[0000]
TABLE 3
Formulation 2
Formulation 3
(pts by weight)
Hardener System
Low molecular weight polyol 1
9.21
2.78
High molecular weight polyol 2
46.61
53.04
Thermoplastic microspheres 3
1.44
1.44
Molecular sieve powder 4
4.90
4.90
Calcium carbonate
29.76
29.76
Calcium stearate
2.88
2.88
Diethyl toluene diamine
4.00
4.00
Reactive colorants 5
0.48
0.48
Silicone surfactant 6
0.72
0.72
Resin
Polymeric MDI 7
100.00
100.00
Reaction Ratio
52/100
48/100
Properties
Sag Resistance
0.75-1.5 inch
0.75-1.5 inch
EXAMPLE 3
[0054] Table 4 below shows the results of a machining test performed on Formulation 1. The machining test is carried out as follows. The percent by weight of dust (i.e., particles of lass than 0.5 mm in size) is measured during the normal CNC machining operation. Several spindles speeds and feed rates are used and the percentage of dust is compared to a commercially available higher density modeling material XD 4503, density of 0.8 g/cc, (epoxy/amine system) available from Vantico Inc.
[0000]
TABLE 4
Spindle Speed
(rpm)/Feed Rate
Total Shavings
Particles
Dust (%)
Dust (%)
(m/min)
(g)
<0.5 mm
<0.5 mm
<0.5 mm 1
20 k/2.7
2.81
0.19
6.76
9.71
20 k/1.0
2.70
0.32
11.85
9.27
12.5 k/2.7
2.74
0.14
5.11
5.39
12.5 k/1.0
2.59
0.19
7.34
4.55
7.5 k/2.7
2.94
0.10
3.40
1.90
7.5 k/1.0
2.90
0.16
5.52
2.93
1 Comparative percent dust generated by XD 4503
[0055] The results of the test show very good machining performance, which is similar to that of XD 4503. Other characteristics observed during machining, such as surface smoothness, edge definition and odor, indicate that the polyurethane formulation prepared in accordance with the present invention has excellent overall machinability.
EXAMPLE 4
[0056] This example shows the ease with which variable density pastes can be produced in accordance with the invention. The same general procedure of Example 1 is followed, using the components of Formulation 1, except that the amount of air injected into the mix chamber is varied through the use of the flow meter. Table 5 below sets forth the flow of air and the resultant density of the paste so produced. The density is measured as in Example 1.
[0000]
TABLE 5
Air reading on the Flow Meter (ml/min.)
Density (g/cm3)
0
0.70
12
0.61
20-21
0.57
26
0.55
27
0.53
28
0.50
29
0.46
EXAMPLE 5
[0057] The example shows that the exotherm of the system can be controlled by varying the ratio of high molecular weight polyol to low molecular weight polyol while maintaining acceptable chemical thixotropy properties. Table 6 below sets forth the peak exotherm of formulations 1-3. The peak exotherm is measured during reaction of the resin and hardener components.
[0000]
TABLE 6
Peak Exotherm
Formulation No. 1
(° C.)
Is Chemical Thixotropy Apparent?
1
123.7
YES
2
114.5
YES
3
106.1
YES
1 Formulations Nos. 1, 2 and 3 have a ratio of high to low molecular weight polyol of 62:38; 83.5:16.6; and 95:5, respectively.
EXAMPLE 6
[0058] Table 7 below shows the use of various isocyanates in combination with the hardener system of Examples 1 and 3. The same general procedure of Example 1 is followed to produce the pastes. The data show that the use of different isocyanates allows for control of the peak exotherm of the resin/hardener reaction while maintaining good chemical thixotropy.
[0000]
TABLE 7
Reaction
Hard-
Ratio
NCO
ener
(R/H
Peak
Chemical
Resin
Content
System
by wt)
Exotherm
Thixotropy
Polymeric
31.5%
1
58/100
123.7° C.
YES
MDI
Prepolymer
17.8%
1
102/100
104.8° C.
YES
1 1
Prepolymer
18.3%
1
100/100
88.4° C.
YES
2 1
Prepolymer
14.4%
1
128/100
78.5° C.
YES
3 1
Prepolymer
11.4%
1
161/100
68.7° C.
YES
4 1
Polymeric
31.5%
3
48/100
106.1° C.
YES
MDI
Prepolymer
17.8%
3
84/100
78.3° C.
YES
1
Prepolymer
14.4%
3
106/100
72.2° C.
YES
3
1 The prepolymers are made using Isonate 143L (modified MDI), available from Dow, and Arcol 24-32 Polyol, available from Bayer. The NCO content is varied by blending the prepolymer at various ratios with other isocyanates.
EXAMPLE 7
[0059] The following materials are formulated for their non-slumping properties following mixing and prior to the cure, and their ability to retain air once dispersed into it.
[0000]
pts by weight
Resin System
Epoxy resin blend
40-60
Non-reactive diluents
5-10
Silicone surfactant
0.01-0.5
Calcium stearate
0-10
Non-reactive colorants
0-5
Alumina trihydrate
20-40
Thixotropic agent
0-10
Hardener System
Aliphatic polyamine
0-15
Amine/epoxy resin adduct
10-20
Low molecular weight polyol
10-30
Non-reactive diluents
0-10
Polyethyleneimine
0-5
Alumina trihydrate
20-40
Silicone surfactant
0.01-0.5
Thixotropic agent
0-10
Reaction ratio Resin:Hardener is 100:90 parts by weight
Density of resin: 1.4 g/cm 3
Density of hardener: 1.3 g/cm 3
[0063] The pre-prepared and packed materials are loaded into a 2KM 1900 meter-mix dispensing machine in 50 liter steel drums. The resin and hardener components are delivered to a mixing block by use of pumps at low pressures (5-20 bar) giving a material flow rate of about 100 g/min. Air from a compressed air line is fed directly into the mixing block. The rotary mixer in the block is variable in speed to give the desired frothing effect on resin, hardener and air components together. The compressed air is regulated using a flow meter and the speed of the rotary mixer controlled via the meter-mix machine.
[0064] In this example the following parameters are used:
Air flow: 4 bar Material pressure A: 16 bar Material pressure B: 5 bar Flow rate: 100 g/min Mixer speed: 1400 rpm
[0070] The paste is extruded onto a solid substrate covered with a release paper and cured at ambient temperature for at least 10 hours.
[0071] The material is evaluated as follows. The density is measured using a specific gravity cup (pyknometer). The uncured material from the machine is measured at a density of 0.67 g/cm 3 showing the successful incorporation of air into the mixed material. On visual inspection of a cut through the material it can be seen that there was good uniform dispersion of the air within the sample. The cell size is uniform. | The present disclosure relates to a seamless model free of bond lines made by a method which includes the steps of providing a substructure having an exposed outer surface, applying a modeling paste to the outer surface of the substructure in the form of a continuous layer, curing the continuous layer of applied modeling paste, and machining said cured layer of modeling paste to the desired contour to form the seamless model. The modeling paste may be a mechanically frothed syntactic foam prepared by injecting inert gas with mechanical stirring into either a formed froth-forming polyurethane or epoxy composition containing mieroballoons. | 2 |
FIELD OF THE INVENTION
The present invention relates to an improved device for the collection of mammalian, including human, blood and the separation therefrom of defined volumes of plasma or serum, which device is capable of maintaining said plasma or serum in stable condition without refrigeration during transportation, e.g., by mail, to a remote location for quantitative or qualitative assay in a laboratory. More particularly, with the present invention, collection of the blood samples can be performed without the services of a professional phlebotomist (or other medical professional) and separation of the plasma or serum therefrom is effected without the need for centrifuges or other mechanical devices. In addition, the device of the present invention receives an unmetered volume of whole blood, separates the plasma or serum from the red cells and then meters a defined volume of the plasma or serum into the sample pad. This plasma or serum sample is stabilized on the pad and is protected from contamination until it can be suitably assayed in a laboratory that may be remote from the collection site.
BACKGROUND OF THE INVENTION
There are many contexts in which the ability to assay mammalian blood plasma or serum is extremely important. Firstly, the diagnosis and/or monitoring of many pathological conditions requires such an ability, as does the monitoring of certain pharmaceutical regimens. Secondly, in human beings, such an ability may be important to permit a well-founded assessment of a person's fitness to undertake certain forms of intensive physical activity, such as certain forms of athletic activity. In some of these instances, assay of a single sample of plasma or serum for a given constituent, e.g., a ligand, may provide the desired information; in others, it is important that a series of plasma or serum samples collected at stated intervals or after defined events, such as levels of heart-rate raising exercise or intake of food or medicine, may need to be assayed to provide the desired information.
At present, there are well established means for the collection of whole blood samples and for transport of these samples to a laboratory, followed by processing to separate the red cells from the plasma and analysis of the blood plasma portion thereof to make a qualitative or quantitative assessment as to one or more actual or suspected components thereof. For example, the collection of venous blood in sterile vacuum tubes such as Vacutainer® brand tubes is well known. But such blood collection requires the services of a trained health professional, such as a nurse, doctor or professional phlebotomist. It is often extremely inconvenient for a mammalian patient to attend at a blood collection site, as well as costly. When it is necessary to collect a series of blood samples from the same subject over intervals of time, moreover, inconvenience and cost are greatly multiplied.
In addition, samples of liquid blood, plasma or serum usually require refrigeration and expeditious transport to the analytical laboratory if their integrity is to be maintained. Despite a variety of chemical stabilizers available in collection tubes such as Vacutainer® tubes, sample stabilities often are only about 48 hours and commonly this storage time is achieved only when the tubes are kept under refrigeration.
Numerous simple devices are also in use for separation of red blood cells from plasma or serum immediately after the collection of a whole blood sample from a mammalian subject. These devices generally operate on a lateral flow chromatographic principle and are so designed that the separated plasma or serum is immediately subjected to a qualitative or quantitative assay for at least one ligand, often by use of a "throwaway", one-use-only, device pre-impregnated with a binding partner for each ligand to be assayed. Such devices typically provide for lateral flow of the sample along a pre-impregnated pathway and for development of a color reaction when the ligand assayed for is present. In some of these cases the blood separation device and subsequent plasma or serum assay device are constructed as a single disposable unit--but in all such cases the object is to obtain a plasma or serum sample and assay that sample while the mammalian patient is present in the medical practitioner's office. Descriptions of blood separation devices of the lateral flow, chromatographic genre appear, inter alia, in U.S. Pat. Nos. 5,135,719; 4,816,224; 4,477,575; 5,186,843; 5,262,067; 4,933,092 and European patent 0295526. In these and similar known blood separation devices, media used in the separation step include various fiberglasses, composite products of the types, e.g., sold under the registered U.S. trademarks Hemasep and Cytosep, and other hydrophilic fibrous materials having effective pore sizes slightly larger than the hydrodynamic volume of a red cell. In general, the physical dimensions and arrangement of the fibers in these media are such that they impede the flow of red blood cells at the surface to which the blood sample is applied while allowing relatively unimpeded flow of the plasma or serum by capillarity. While the red cells are able to move through the fibrous matrix, their flow rate is much slower than that of the plasma or serum, resulting in the formation of a red-cell-free zone at the leading edge of the flow. Because the plasma or serum volumes supplied by separations effected with these devices are somewhat variable, quantitative assays for ligands using such plasma volumes require the development and use of a calibration curve for each specific ligand being determined. Because such calibration curve development is time-consuming and tedious, and somewhat impractical of performance in many point-of-care milieus, such as medical practitioners' offices, the serum or plasma volume separated by these devices is, as a practical matter, most often subjected to a qualitative assay for the presence of the target ligand.
Simple devices are also known that permit blood sample collection, stabilization and transport, such as depositing a drop of peripheral blood onto a sheet of filter paper and allowing it to dry. Such a device is currently used for qualitative detection of inherited diseases in newborns, such as phenylketonuria. More recently, a similar "test card" comprising filter paper has been suggested for a commercial, mail-in system for the qualitative detection of HIV antibodies in whole blood. Thus, U.S. Pat. No. 5,641,682 refers to a test card of this type supplied in a commercial over-the-counter kit. The person desiring an HIV test is directed to place multiple whole blood spots on the card, allow them to dry, and then to convey the card containing dried blood spots to a laboratory where an assay for HIV antibody is performed. This simpler means of whole blood collection does not require the services of a trained phlebotomist. It suffers from two main disadvantages, however: first, it does not allow for the collection of a defined volume of blood, blood plasma or serum; and second, mere drying of whole blood may not adequately stabilize the blood constituents from the time of collection to the time of assay. Quantitative assays for various substances in plasma or serum, such as antibodies, enzymes, hormones, drugs and small molecular weight constituents such as glucose, cholesterol, or lactic acid, require a knowledge of the plasma or serum sample volume. Dried whole blood samples contain an unknown volume of blood plasma or serum. The plasma or serum volume contained per unit area of a dried blood spot varies according to the hematocrit of the sample and as a result of the duration and other conditions of the drying process; the plasma or serum volumes resulting from lateral chromatographic separation of red cells and plasma have been found to be highly variable. Other sources of variation can be related to the uniformity or lack thereof, and other characteristics of the collection matrix, among other factors.
SUMMARY OF THE INVENTION
The present invention embodies a collection device that can reliably be used by anyone without special training of any nature for the collection of one or more samples of mammalian whole blood. This device in its simplest form comprises a single blood-receiving port that has been formed in an upper layer which comprises hydrophobic material, which layer is firmly bonded to an underlying suitable hydrophilic layer impregnated with a blood agglutinating or clotting agent. This hydrophilic layer is in contact with an underlying second hydrophilic layer into which it reliably meters a defined volume of plasma or serum, whereupon the two upper layers are mechanically stripped away and the plasma or serum in the second hydrophilic layer is allowed to dry. The second hydrophilic layer is underlaid with a second hydrophobic layer which, inter alia, aids in the retention of the plasma sample within the second hydrophilic layer during the drying period. In the separation step conducted in the first hydrophilic layer and during transfer of a metered volume of the serum or plasma into the second hydrophilic (plasma retention) layer, the capillary flow of serum or plasma is vertical rather than lateral and hence the flow path is short in relation to the known lateral flow separation devices.
This use of a vertical flow principle to separate the serum or plasma from the red cells and meter a defined volume into the second hydrophilic, or plasma retention, layer is an important aspect of the device of this invention.
For mailing or other transport to a laboratory, the device of this invention, the plasma or serum retention layer is covered with a protective cover so arranged as to permit air to circulate over and contact the sample retention layer even when the cover is closed.
Simple tests and, in some instances, other criteria for the individual layer components are more particularly described hereinafter.
The device may be constructed with multiple whole blood sample-receiving stations, each comprising two layers of hydrophilic material sandwiched between two layers of hydrophobic material as described.
After the blood collection, separation and metering for all sample-receiving stations is complete, so that the two upper layers have been stripped away and the plasma (or serum) retention layer has been air dried at each station, preferably while covered as hereinafter more fully described, the device is closed with the individual station covers in place and the entire device is preferably sealed into a resealable, zip-lock or similar pouch containing a desiccant. This pouch and desiccant aid in maintaining sample stability during mailing or other transport to a laboratory in that they maintain dryness of the plasma retention pads as well as providing barriers to contamination, sunlight, artificial light, humidity and other adverse, frequently variable, environmental factors.
When the device of the invention is received at a laboratory the hydrophilic sample retention pad (second hydrophilic layer) is stripped away from the underlying second hydrophobic layer. The dried plasma or serum may then be extracted into any of various suitable media and analyzed for known or suspected target constituents. Alternatively, the sample retention pad can be placed in contact with the reaction pathway of a device adapted to conduct a preselected immunospecific assay, wetted with a suitable buffer or other appropriate liquid and subjected to the assay.
Specific analytical modalities and immunoassays are well known and are not within the scope of this invention. The plasma retention pad of the present invention, in general, can be treated by known extraction and/or contact methods so as to enable analysis or assay of the plasma sample by any of the well known modalities for effecting it.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1A is a side view of one blood receiving station according to the present invention as it exists prior to the application of a whole blood sample.
FIGS. 1B and 1C are top views, respectively, of (1) the upper hydrophobic layer and attached first hydrophilic or blood sample receiving layer and (2) the lower hydrophilic layer with appended lower hydrophobic or plasma retention layer after mechanical separation of these units from each other.
FIG. 2 illustrates the contact angle test with a water drop used to test hydrophobicity of proposed materials to determine their acceptability to be used in the devices of this invention as hereinafter described.
FIG. 3A depicts a typical device of this invention which is equipped with five blood sample receiving stations, as it appears during fabrication of the device with only the bottom hydrophobic layer and the second (plasma retention) hydrophilic layer, the latter in the form of five discs of material in place. The device also has this appearance when ready to send to a laboratory after separation of the upper hydrophobic and underlying first hydrophilic layers.
FIG. 3B depicts a single section of the preferred arrangement of the unit, fabrication detail of which appears in FIG. 3C.
FIG. 3C is an inverted side view of the fabrication of a unit comprising a particularly preferred blood separation (first hydrophilic) layer attached to a hydrophobic material mounted on a solid surface.
FIG. 3D illustrates the preferred fully assembled device as it appears before application of any whole blood sample.
FIG. 3E is a side view of an uncovered receiving station.
FIG. 3F shows an exaggerated detail of a single blood receiving station, in side view, prior to application of a blood sample and FIG. 3G shows a side view of the same blood receiving station again in exaggerated detail, after stripping away of the two upper layers from the plasma retention pad and lowering of the cover over the station.
DETAILED DESCRIPTION OF THE INVENTION
Early in the work which led to the present invention, it was discovered that the separation media employed in the various devices which separate the red cells from plasma or serum using a lateral flow chromatographic principle as mentioned hereinabove are unsuitable for obtaining a defined volume of red-cell-free serum or plasma from a whole blood sample. "Defined volume" as used herein, means the volume of plasma, as determined from a standard curve for L-lactate in fresh, red-cell-free plasma obtained as shown in Example 2 hereof, that when analyzed by the same method gives, within the limits of experimental error (taken as a coefficient of variation not exceeding 6.0) the same L-lactate content in millimoles as was obtained by analyzing 6 μL. of fresh red-cell-free plasma. Thus, while defined volume as so used is not reproducible to a mathematical preciseness of two decimal places, it is a volume that is sufficiently consistent and reproducible that comparable analytical and/or assay results, well within the experimental error of the available analytical and assay methods, are regularly obtained.
The early work on blood separation media employed in the blood separation devices that utilize the lateral flow chromatographic principle showed three problems: to wit, (1) separation of a plasma zone that yields enough red-cell-free plasma for routine wet chemistry analysis of, e.g., glucose or L-lactate content was slow, taking 10-30 minutes or more to yield an acceptable-sized red-cell-free zone; (2) the size of the red-cell-free zone varied considerably from sample to sample, whereby configuring a single geometry that would yield a minimum plasma volume, in the order of 2-10 μL. of plasma that was both isolatable and separable from the red-cell-containing zone was difficult to impossible; and (3) zones visually free of red cells that did form in these media did not contain an essentially constant volume of plasma per unit area.
When agglutinating agents as described in U.S. Pat. Nos. 4,933,052 and 5,135,719 and European patent 0295526 were added to these separation media, the only problem to some extent alleviated was the first one above--i.e., the speed of separation of red cells from plasma increased.
By measuring blood hematocrit in various samples, it was found that the second problem mentioned above is roughly related to hematocrit level (hematocrit being defined as the volume fraction of the packed red cell component of blood) in that the higher the hematocrit, the longer it takes for an essentially standard-sized red-cell-free zone to form in these lateral flow separation media.
Adding a plasma acceptor zone comprising a porous hydrophilic medium such as filter paper to various lateral flow separation media was also tried with the disappointing result that a highly variable volume of plasma per unit area was formed on the plasma acceptor medium. This was true even when an agglutinant was employed in the separation medium.
When, however, a vertical format device was made using a separation medium adopted from a lateral flow device and having an agglutinant therein and the separation zone was followed by a plasma capture medium, it was observed that a defined volume of plasma was sometimes captured in the capture zone.
Further efforts to arrive at a blood separation device capable of capturing a defined volume of plasma regularly and reproducibly led to the development of the four-layer "sandwich" consisting of a first hydrophobic layer, a first hydrophilic blood separation layer containing agglutinant or clotting agent, a second hydrophilic plasma capture layer and a second hydrophobic layer, which "sandwich" is the essence of the present invention. These efforts also led to the development along the way of criteria for the materials used in the various layers.
Blood separation media useful in this invention must be agglutinin or coagulating agent impregnated. Preferably the agglutinin is a mixture of a lectin with no blood group specificity, of which phytohemagglutinin P is most preferred and a polycationic chemical such as hexadimethrine bromide or poly-(1,1-dimethyl-3,5-dimethylene piperidinium chloride), with hexadimethrine bromide being preferred. Other lectins which may be substituted are lectins from wheat germ (Triticum vulgaris), potato (solanum tuberosum), soybean (glycine max) and that from the bacterium Mycoplasma gallisepticum. A suitable substitute for lectinpolycationic agent mixture is a mixture of a natural coagulating agent, such as thrombin or snake venom, with a polycationic agent or a cocktail of the type disclosed in U.S. Pat. No. 5,089,415. Other acceptable agglutinating and clotting agents will readily occur to those skilled in blood separation techniques.
The media that are suitable for the blood separation layer can be identified by a simple test as follows: A 2.5×0.5 cm. test strip of the candidate material is cut and placed on a cellophane tape-covered solid support, where it is held in place by a 1 cm. wide, 2 cm. long cellophane tape strip placed across the test strip at right angles in a location 0.5 cm. from the end of the test strip. A drop of whole blood of 50 μL. or greater volume, to which has been added a known anticoagulant, is placed on the cellophane in contact with the end of the test strip nearest the anchoring cellophane tape. This blood is allowed to chromatograph laterally through the test strip and is prevented from migrating over or under the test strip by the anchoring cellophane tape. If this chromatography produces a visual red-cell-free zone at its leading edge that is at least 2 mm. long, the medium of the test strip is suitable for use as the first hydrophilic blood separation layer of the device of this invention, once it has been impregnated with agglutinating or clotting agent.
Suitable media for the plasma capture and retention, or second hydrophilic layer are cellulosic filter papers, ion exchange papers, fiberglasses, nylons, certain grades of composite media such as Cytosep® and the like.
The hydrophobic layers which abut the top of the blood separation layer and the bottom of the plasma capture and retention layer may be of the same or different material. Suitable materials are those which meet the following test:
A drop of water is carefully placed on a horizontal, flat surface of the candidate material. This drop of water will form a bead on all suitable materials and will rapidly assume a shape as depicted in FIG. 2 hereof in which the edge of the drop forms an angle ⊖ with the flat surface of the candidate material at the point of their contact. Materials sufficiently hydrophobic to be used in the hydrophobic layers of the device of this invention exhibit a minimum contact angle of 60 degrees, preferably 80 degrees and most preferably 85 degrees. See, e.g., Myers, D, in Surfactant Science and Technology, pp. 305-306 (VCH Publishers, New York, 1988).
If a candidate material has an adhesive or other coating, the test must be performed on the coated surface. It has been found that a coated material that passes the test on its uncoated surface but is hydrophilic on the coated surface will, if used as the second hydrophobic layer, prevent capture/retention of a defined volume of plasma in the plasma capture and retention layer.
Among suitable hydrophobic materials are cellophane tape, polyethylene, any solid plastic material that meets the hydrophobicity test and is heavy enough to act as a solid base support and any hydrophobic plastic tape that is affixed to a solid base such as cardboard.
In fabricating the device, certain precautions must be taken. The first hydrophobic layer and the whole blood separation layer must be firmly bonded together at the edges so as (1) to prevent red blood cells from migrating around the edges of the blood separation layer and contaminating the plasma collection and retention layer, and (2) to provide a means for ready mechanical separation of the blood cell separation layer from the plasma collection and retention layer.
One means of effecting this bonding is to heat seal the edges of the first hydrophilic, blood separation layer to a polyethylene coated solid support. The two hydrophobic layers attached to base supports each extend well beyond the edges of the two hydrophilic layers at every blood receiving station. Means must be provided at each station to hold those portions of these hydrophobic layers that extend beyond the bounds of the hydrophilic layers firmly in contact with one another so that they will (1) keep the two hydrophilic layers in firm, uniform, surface-to-surface contact during blood sample application, separation and the wicking of the plasma into the lower hydrophilic layer and also (2) allow subsequent, facile mechanical separation of the two solidly supported hydrophobic layers so that there is isolation of the plasma in the plasma retention layer. A wide variety of such means are known for this purpose and any of them that will perform the necessary functions is acceptable.
Means that have been tested successfully include creating the base supports out of strips of cardboard, and spot gluing the supports together, cardboard to cardboard, on opposite sides of the blood sample application hole, about 1 cm from its edge. To separate the supports after the plasma sample has been captured, the strips are simply pulled apart, tearing the paper surface of the cardboard at the glue spots. Another preferred means is to utilize a double sided tape for the second or lower hydrophobic layer, mounting it on a cardboard base. If this hydrophobic layer is extended about 1 cm beyond the edges of the adjacent hydrophilic layer, it can be pressed to the inner surface of the first or top hydrophobic layer, holding the two support bases together. After the plasma has saturated the second hydrophilic (retention) layer, the plasma sample may be isolated by pulling the supports apart.
In general, the device requires the creation of a sandwich of two hydrophilic, porous media designated (3) and (4) in FIG. 1A, surrounded by layers marked (2) and (5) that are hydrophobic, relative to the porous media, and where one side of the upper hydrophilic layer, the sample-application side, is initially in contact with air, through hole (1). Thus, the blood sample applied at (1) begins to move through (3) by capillary action, but red cells are agglutinated there and become trapped. Plasma, in contrast, continues to flow through and makes contact with hydrophilic layer (4) and is drawn into it by capillary action. The plasma sample eventually saturates the voids of (4), thereby metering a defined plasma sample volume. The hydrophobic environment of the layers (2) and (5) that surround the edges of (3) and (4) does not itself absorb plasma. Moreover, the hydrophobicity of these layers appears to prevent the creation of a capillary force in the space between them. Without a capillary force, plasma is retained only in the hydrophilic plasma capture layer and a defined volume of plasma is obtained.
Separation of the hydrophobic layers which are either attached to neutral supports like cardboard (not shown in FIG. 1) or are thick enough to act as supports, isolates the plasma sample in (4). The surface-to-surface vertical flow separation format, moreover, allows no free liquid plasma to contact (4). Thus, when the hydrophobic layers are separated, there is no variable partition of liquid plasma into (4) as there would be, for example, if a strip of (4) were dipped into a drop of excess liquid plasma and then removed. Experience has shown that dipping of hydrophilic material suitable for (4) into a drop of liquid plasma, and withdrawing it, does not capture a defined reproducible volume of the plasma. The essentially uniform, reproducible partition of plasma between (3) and (4) followed by timely separation of these layers from one another, is a particularly valuable feature of this invention.
To foster the intention of making the device of this invention reliably useable by almost any person, several other optional features may be added to the device. For example, an athlete wishing to determine his or her exercise-induced lactate levels will want to collect several blood plasma samples, one immediately following each bout of a set of increasingly rigorous exercise bouts. Thus, multiple blood receiving stations including means for isolating multiple blood plasma samples may be included in a single device and kit, instead of only one such station.
FIGS. 3A to 3G illustrate various aspects of a device of this invention having five sample receiving stations. This device may be used, e.g., by athletes training for endurance in competitive athletics. The quantitative relationship between exercise intensity and the level of lactic acid in the blood has been used for decades to optimize the training of elite, Olympic-level athletes, see Weltman, Arthur, The Blood Lactate Response to Exercise (Human Kinetics Press, Champaign, Ill. 1994). Such assessment requires that the blood sample be collected within less than two minutes of completing the exercise, i.e., sample collection on-site at the track, court-side, or the like, and that the red cells, which produce lactic acid in a non-exercise related way, be separated from the plasma within a few minutes. Other possible uses for a device as illustrated in FIGS. 3A to 3G are in periodic monitoring of the level of a therapeutic drug where blood samples on an hourly or other periodic basis must be tested, periodic monitoring of blood constituents such as cholesterol or for mass screening for constituents such as blood glucose or blood urea nitrogen (BUN). Other uses for a device of this invention with multiple blood-receiving stations will readily occur to those skilled in the art.
As illustrated in the FIGS. 3A to 3G inclusive, each sample receiving station is provided with a cover. This is to prevent contamination of unused or completed sampling means by spillage of blood or other contaminants. These figures also illustrate the use of a protective flap that covers the completed set of samples, and their individual covers, as a further aid that prevents inadvertent mechanical damage during shipment to the laboratory.
One other key feature of the design shown in FIGS. 3A to 3G is that the individual sample covers are arranged to allow air to circulate over the sample even when the cover is closed. This is intended to foster drying of the sample. After the sample receiving stations have all had samples applied to them in the manner herein described, the device is sealed in a re-sealable, zip-lock foil pouch that also contains a desiccant which is provided in the kit with the device. The pouch and desiccant foster the maintenance of sample stability by maintaining dryness during transport, as well as providing a barrier to adverse environmental factors like sunlight.
The additional optional features illustrated here promote the intended use of the devices of this invention by providing barriers to contaminations and adverse environmental factors such as humidity and light. There are a plethora of ways of providing such features which are well-known or obvious to those skilled in the art. Any or all of them can be added to an embodiment of the instant invention.
Referring to FIGS. 3A to 3G, to further illustrate details of a device of this invention having five receiving stations, 24 point chipboard is cut to form all items bearing the "11" numeral in FIG. 3A. These include a device base section 11A, a "matchbook"-like flap labelled 11B and 5 individual sample covers in a device top portion divided into 5 segments each labelled 11C.
The segmented top 11C is double folded at edge 11E in such a way that each of the five segments may be individually folded over bottom portion 11A to cover one of the exposed plasma retention pads upon completion of the blood sample delivery and separation and the plasma isolation process at that station. In each segment a dome 14 of a diameter larger than the corresponding plasma sample retention pad (second hydrophilic layer) 11A has been embossed.
In assembling the device the bottom ("second") hydrophobic layer comprising wide, double sided hydrophobic adhesive plastic tape 12 from Minnesota Mining and Mfg. Co. is applied along the length of 11A, spaced apart from fold line 11E and parallel to it. Filter paper, Ahlstrom 601 is punched into appropriately sized discs to form the lower ("second") hydrophilic layer (i.e., the plasma retention layer) of each sample receiving station. The discs 1B are each located at even intervals along the hydrophobic tape 12, such that their centers and those of the domes 14 will align when the 11C sections are folded over to cover the isolated plasma samples.
Cytosep 1660 from Ahlstrom, Inc. of Mt. Holly Springs, Pa. is impregnated by coating with a mixture of 50 mg. of phytohemagglutinin P (obtained from Phaesolus vulgaris and supplied by Difco) and 450 mg. of Hexadimethrine bromide (obtained from Aldrich Chemical Co.) per square foot of the Cytosep. After coating, the Cytosep, which comprises the upper (first) hydrophilic layer that acts to separate red blood cells from plasma or serum, is dried and punched into discs 18 of slightly larger diameter than discs 13. These discs 18 are centered over discs 13 in the following manner: 24 point chipboard is coated on one side (labelled 15A in FIGS. 3A to 3G) with a polyethylene layer 17 and cut into five suitably sized strips. A hole of slightly smaller diameter than discs 18 is punched into each of the strips 15 at locations which are centered so that they would fall beneath each of the domes 14 if the device were closed. Each agglutinant coated Cytosep disc 18 is heated around its edge 19 while being pressed against polyethylene layer 17 to seal it to one of the coated chipboard sections 15 at a position that is centered over hole 16. Each chipboard section 15 is then positioned so that hole 16 and Cytosep disc 18 are centered over one of the filter paper discs 13 with the Cytosep surface in abutting contact with the filter paper, while the polyethylene coated side 15A of each chipboard section 15 is pressed against adhesive tape 12 to anchor it in place. Thus the "sandwich" of blood separation layer 18 in contact with plasma isolation/retention layer 13 surrounded by upper and lower hydrophobic layers 17 and 12 is fabricated at each sample receiving station. For shipping and/or storage, the protective covers 11C are folded over the respective stations and the flap 11B is folded over the closed covers.
To use the device, one folds flap 11B and a protective cover 11C containing a domed cover 14 back and applies a drop of blood to hole 16. After a minimum of 2 minutes and a maximum of ten minutes, the portion of section 15 that overhangs base 11A is grasped and peeled off, thereby isolating plasma sample retention pad 13. Protective cover 11C containing domed cover 14 is then closed over pad 13. By virtue of double fold 11E and dome 14, sample retention pad 13 is not sealed shut but remains in contact with air so that the plasma on pad 13 dries.
When plasma has been transferred to all of the pads 13 and they have all been isolated as described and covered, the flap 11B is again closed over protective covers 11C and the device is sealed in a foil pouch with desiccant for transport to a laboratory. Upon arrival there, the sample retention pads 13 are removed from adhesive strip 12 and the plasma is extracted into a suitable medium for analysis or assay.
Obviously, there are many possible ways of constructing the device of this invention. The foregoing specific description keyed to illustrative FIGS. 3A to 3G is not meant to limit in any way the possible embodiments of the invention that meet the criteria described hereinabove for specific materials, nor is it intended to limit the choice of obvious alternative geometries, support materials, agglutinating or clotting agents, sizes, shapes or the like.
One of the surprising benefits of using the devices of this invention was the realization that plasma or serum dried on a material that meets the criteria disclosed herein for the second (bottom) hydrophilic layer that receives and retains a defined volume of plasma or serum is that the constituents of the plasma thus air dried are highly stable.
The following examples serve to illustrate this stability, other benefits that follow from using this invention, and certain critical limitations of the invention or its use:
EXAMPLE 1
The surprising stability of blood plasma constituents air dried on filter paper is illustrated in this example.
In this experiment, a sample of EDTA-anticoagulant-treated blood was used to compare the stability of some constituents of blood plasma. One portion of this blood was centrifuged at 1,500×g for 10 minutes and the clear plasma was separated from the red cells. Replicate 6.00-μL. aliquots of this plasma were pipetted onto filter paper discs (13 as described above by reference to FIGS. 3A to 3G), mounted on a hydrophobic tape attached to a cardboard support, and the plasma was allowed to air dry. These discs were sealed into a foil pouch with a silica desiccant pack and left to incubate. At the same time, aliquots of the same whole blood and of the isolated plasma were sealed into microfuge tubes and also left to incubate at room temperature. A portion of the clear plasma as freshly separated was assayed on the day of its separation by centrifugation for its content of lactic acid, glucose and lactate dehydrogenase. After 7 days storage at room temperature, the whole blood was centrifuged to obtain plasma, and this plasma, the air dried plasma, and the stored liquid plasma samples were assayed for the same constituents. The results are shown in Table 1. The whole blood sample was difficult to analyze for lactate and glucose due to the coloration of the sample by hemoglobin.
When the experiment is repeated, but the incubation is performed at 50° C., the results are obtained as shown in Table 2. Clearly, air drying of plasma on a suitable hydrophilic support is the best mode of preserving its constituents.
TABLE 1______________________________________Recovery of plasma constituents after 7 days at room temperature Lactate Glucose LDHMedium (mM) % (mM) % μ/L %______________________________________Day 0, 0.81 100 4.1 100 102 100PlasmaDay 7, 0.86 106 4.0 98 80 78PlasmaDay 7, 3.8 469 1.3 32 256 251BloodPlasmaDay 7, 0.78 96 4.0 98 107 105DriedPlasma______________________________________
TABLE 2______________________________________Recovery of plasma constituents after 7 days at 50° C. Lactate Glucose LDHMedium (mM) % (mM) % μ/L %______________________________________Day 0, 0.81 100 4.1 100 102 100PlasmaDay 7, 0.74 91 3.5 85 <15 NotPlasma DetectedDay 7, 4.9 605 <0.1 Not <15 NotBlood Detected DetectedPlasmaDay 7, 0.83 102 3.9 95 97 95DriedPlasma______________________________________
EXAMPLE 2
A set of 20 replicated plasma samples, prepared as described in relation to FIGS. 3A-3G, were obtained from 30 μL. drops of citrate-anticoagulated blood. Simultaneously, an aliquot of the whole blood was centrifuged to prepare plasma, and this plasma was immediately analyzed for its content of L-lactate. From this analysis, a standard curve was prepared in a known manner, relating content of L-lactate to plasma volume. After air drying the plasma retention discs of this invention, the discs were eluted with a buffer containing 50 mM MOPS of pH 7.4, 0.1% Bovine Serum Albumin (BSA), and 0.1% Triton X-100. The eluate was assayed for lactate and the average volume of plasma contained on the discs was calculated from a comparison of the lactate response results to those of the plasma-volume standard curve.
The experiment was repeated with EDTA-anticoagulant-treated blood spiked with 1 mM 4-aminoantipyrine as reporter molecule. These results are all shown in Table 3.
TABLE 3______________________________________Volume of Plasma Recovered from the instant invention (n = 20)Volume Deter- Mean Volume Standard Deviation Coefficient ofmination by: (μL) (μL) Variation (CV)______________________________________Lactate 5.68 0.31 5.44-Amino- 5.83 0.21 3.6antipyrine______________________________________
EXAMPLE 3
Experiment 2 was repeated with ten replicated plasma samples each, but the following changes in the devices were made.
A. Instead of covering the support base 11A of FIGS. 3A to 3G with double sided plastic tape 12, such tape was used only directly under the plasma absorption disc 13 thus exposing the paper covered surface of 11A adjacent to the disc 13. A section 15 with attached disc 18 was spot glued to the support 11A at points above and below hole 16, and about 1 cm. away from the hole.
B. Instead of using double sided plastic tape 12 of FIGS. 3A to 3G, disc 13 was attached to support 11A with Elmer's glue gel, a water soluble glue that leaves a hydrophilic surface when dried, or with Borden's neoprene-based contact cement, an adhesive that also leaves a hydrophilic surface. A section 15 with attached disc 18 was spot glued to 11A as in A part hereof, above.
C. Instead of heat sealing treated Cytosep 8 to a polyethylene coating on support surface 5A, the circumference of the Cytosep was glued to the uncoated paper surface of 5A using Duco cement.
D. Cytosep disc 8 was only sealed to surface 5A at 4 spots, so that its circumference was not completely sealed to polyethylene coating 7, and hence gaps were present.
When devices constructed as in A, B or C were tested for the reproducibility of the plasma volume captured, the coefficients of variation of the captured volume varied from 7 to 11%, and this was considered unacceptable for a quantitative analysis. Devices constructed according to section D above were badly contaminated with red blood cells from leakage of blood around the edge of disc 8. These devices failed to perform the required red cell-plasma separation.
These results illustrate the benefit of surrounding the plasma capture disc-red cell separation matrix with a hydrophobic surface, to foster the reproducibility of plasma uptake into the plasma capture medium. It also illustrates the critical requirement to completely seal the blood cell separation medium to its support tab, so that red blood cells must pass into the separation medium and not pass around it.
EXAMPLE 4
Devices constructed as in Example 2 are developed with whole blood, except for three variations:
A. devices were supplied with blood drops varying from 17 to 70 μL in volume;
B. The time that blood was in contact with the device before isolation of the plasma sample was varied from 1.5 to 5 minutes;
C. Prior to applying the blood to the device, the hematocrit of the blood was adjusted to varying levels between 35 and 57%.
TABLE 4______________________________________Changes in Average Percent Recovery and CV of the nominal(5.7 μL) plasma sample volume in response to changes in:A. Blood Volume (μL) Percent Recovery Coefficient of Variation______________________________________17 87 6.720 92 5.325 100 4.730 100 3.070 102 5.9______________________________________B. Time on Device (min) Percent Recovery Coefficient of Variation______________________________________1.0 92 4.21.5 92 3.62.0 100 4.33.0 100 3.35.0 104 3.9______________________________________C. Hematocrit Percent Recovery Coefficient of Variation______________________________________57 87 1153 96 4.648 102 3.541 100 2.936 108 4.8______________________________________ A. Whole blood sample volume, B. Duration of blood incubation on the device before isolation of plasma; and C. Hematocrit of the blood. The average volume of plasma captured in tests A and B was essentially constant as shown in Table 4. In test C, the plasma volume captured was constant up to a hematocrit level of 53 but the captured volume was reduced significantly when blood of hemacrit 57 was used.
This example illustrates that the devices will operate reliably in the hands of untrained users, without a need for precisely measuring the whole blood sample volume, or precisely timing the period between blood sample application to the device and the isolation of the plasma retention disc from the blood separation disc. In the latter instance, other work has shown intervals of from two to ten minutes between blood sample application and plasma retention disc isolation give satisfactory results within the limits of experimental error. Intervals of two to five minutes are, however, preferred.
The example also shows the device will work satisfactorily with blood samples of hematocrit from 35 to 53. The blood of at least 99% of the human population has a hematocrit less than 57, according to C. Lentner, Ed., Geigy Scientific Tables, Vol. 3, p. 207 (CIBA-GEIGY: Basle).
EXAMPLE 5
To devices prepared as in Example 2 whole blood spiked with 1 mM lithium chloride and 1 mM sodium salicylate is applied. Plasma samples prepared by immediate centrifugation of this blood are compared to plasma isolated in the devices of the invention, allowed to dry and stored for 7 days in sealed, desiccated foil pouches. The following plasma components are recovered essentially quantitatively from the device plasma samples: Lactate dehydrogenase, lactic acid, glucose, cholesterol, anti-hepatitis B antibodies, insulin, lithium, salicylate and TSH.
It is anticipated that the following possible plasma components of plasma isolated and air dried in devices of this invention will similarly be essentially quantitatively recoverable: Alanine aminotransferase, Creatine kinase, Glutamate oxalacetate transaminase. Alkaline phosphatase, Plasma renin, Glucose-6-phosphate uridyl transferase, Plasma ACTH, Luteinizing hormone, Calcitonin, Cortisol, Catecholamines, Androstenedione, Atrial natiuretic factor, Glucagon, Progesterone, Testosterone, Estrogen and its metabolites, Estriol, Triglycerides, Ammonia, Vitamin C, Zinc, Antinuclear antibodies, Anti-DNA antibodies, Extractable nuclear antigen antibodies, Antimitochondrial antibodies, Anti-smooth muscle antibodies, Antithyroid antibodies, Thyroid-stimulating immunoglobulins, Cardiolipin antibodies, Rheumatoid factor, Acetylcholine receptor antibodies, Rubella antibodies, Anti-HIV antibodies, Anti-CMV antibodies, Hepatitis B surface antigen, EBV antibodies, RSV antibodies, Herpes simplex antibodies, Antifungal antibodies, Anticandida antibodies, Bacterial meningitis antigen, Lyme disease antibodies, Syphilis antibodies, CEA, AFP, hCG, ACTH, Prostatic acid phosphatase, Prostate specific antigen, Tissue polypeptide antigen, Tenagen (Tennessee Antigen), Pregnancy-specific glycoprotein, Serotonin, Amikacin, Caffeine, Carbamazepine, Chloramphenicol, Desipramine, Digoxin, Diisopyramide, Ethosuccinimide, Gentamicin, Imipramine, Lidocaine, Methotrexate, Phenobarbital, Phenytoin, Primidone, Procainamide, NAPA, Quinidine, Theophylline, Tobramycin, Valproic acid, Pseudo-cholinesterase, Mercury, Arsenic, Antimony, Selenium, and Bismuth.
It is emphasized that many variations in the devices of this invention, which will be readily apparent to those skilled in the art, can be made without departing from the scope of the invention. It is accordingly intended that the scope of this invention be limited only by the appended claims. | A process for separating plasma or serum from mammalian whole blood includes the steps of applying a sample of blood through a hydrophobically faced sample receiving hole positioned in a first upper layer of hydrophobic material to a first layer of fibrous hydrophilic material which has been impregnated with a blood agglutinating agent so that it acts to retain red blood cells but not plasma or serum and layer is sealed at its upper edges to the first layer of hydrophobic material and allowing the liquid portion of the sample to flow downwardly through the first layer of fibrous hydrophilic material into a second layer comprised of a different fibrous hydrophilic material which second layer is sealed at its lower edges to a second layer of hydrophobic material whereby it acts to retain the plasma or serum. | 6 |
BACKGROUND
[0001] In foam assembly processes, such as foam mattress assembly, water based adhesives provide a safe, effective, and non-hazardous solution for bonding foam pieces together. However, the adhesive contains a large percentage of water. Therefore if a foam assembly bonded with water-based adhesives is packaged before fully dried, mold, unpleasant odors, substrate material breakdown, and the like may develop.
[0002] Further, even aside from the water of the water-based adhesives, foam can contain appreciable amounts of water, such as 1% to 2% water by weight, based solely on how it is stored. If stored in humid environments, the foam will retain a higher percentage of water weight compared to being stored in low humidity conditions. This water can also be a problem for mold and mildew growth when the mattress is packaged. This water, even on its own, can cause issues, and these issues may be compounded when water-based adhesives are present.
[0003] In particular, in foam mattress assembly and other assembled foam products, a fast growing trend in industry is to compress said assemblies into a box that may be shipped directly to customers. The boxes are sized such that traditional package shipping companies can handle them. These foam mattresses are laminated, and then enclosed in an impermeable plastic bag which is vacuumed and compressed so that it fits into the mattress boxes. Vacuuming alone to compress the package does not adequately extract water from the package, so trapped moisture is a common occurrence. Currently, the primary solution for this problem is to simply let the foam assemblies rest for a certain time period. However, this slows down the manufacturing and shipping process, and requires extra storage space at the manufacturing site.
[0004] Therefore, what is needed is a system that may allow for rapid drying of the assembled adhered foam elements to allow for a shorter processing time between assembly and packaging.
SUMMARY
[0005] The subject matter of this application may involve, in some cases, interrelated products, alternative solutions to a particular problem, and/or a plurality of different uses of a single system or article.
[0006] In one aspect, the present invention involves an apparatus configured to remove moisture from laminated foam assemblies. The present invention operates generally by drawing air through a foam product. In a particular aspect, a vacuum box is provided that provides walls and a base to support a foam assembly that can be quickly and easily moved into and out of the box for drying of the adhesive by drawing air through the foam assembly. As this air passes through the foam assembly, moisture within the foam, either from the atmosphere and/or water based adhesive is evaporated, allowing for more effective, safe, and sanitary long term packaging.
BRIEF DESCRIPTION OF THE FIGURES
[0007] FIG. 1 provides an elevation view of one embodiment of the foam drying apparatus of the present invention.
[0008] FIG. 2 provides a side view of an embodiment of the present invention.
[0009] FIG. 3 provides a side view of another embodiment of the present invention.
[0010] FIG. 4 provides an elevation view of yet another embodiment of the present invention.
[0011] FIG. 5 provides a side view of still another embodiment of the present invention.
[0012] FIG. 6 provides a side view of yet still another embodiment of the present invention.
[0013] FIG. 7 provides an elevation view of another embodiment of the present invention.
[0014] FIG. 8 provides an elevation view of another embodiment of the present invention.
[0015] FIG. 9 provides a side view of an embodiment of an adjustable side wall of the present invention.
DETAILED DESCRIPTION
[0016] The present invention concerns an apparatus to reduce or eliminate water from a foam assembly. The present invention involves an apparatus that is configured to draw air through laminated foam assemblies such as foam mattresses and the like. Generally, the apparatus provides a base area and sidewalls on which the foam assembly may be placed and supported. For example, the foam assembly may be placed on a rack, rollers, and the like. Below, or otherwise adjacent to the base, a vacuum attachment allows a vacuum to be drawn on, and applied to, all or nearly all of a surface area of one face of the foam assembly. The vacuum attachment applies the reduced pressure to the surface area of the foam assembly. The apparatus is configured to be operated for a period of time on a foam assembly sufficient to adequately dry the foam assembly. This time frame may vary depending on the variables particular foam assembly such as its size and the amount of adhesive used. Air on the opposite side of the foam assembly is drawn through it towards the vacuum attachment. As the air passes through the foam assembly, moisture is evaporated and carried out of the foam.
[0017] As used herein, a foam assembly may be any assembly that comprises two or more foam pieces laminated together using an adhesive. It is even possible that a foam assembly may be a single foam element. Foam assemblies may be any size, shape, foam type(s), and configuration, without straying from the scope of the present invention.
[0018] In one embodiment, the present invention provides a vacuum box for drying rectangular foam assemblies, for example mattresses. The box is formed of an air permeable base on which a foam assembly may rest, as well as side walls to cover the sides or part of the sides of the foam assembly held therein. A vacuum attachment, such as a pipe and a spacing underneath the base allows a low pressure zone to be applied to a foam assembly resting on the base. In some embodiments, the base may have a plurality of rollers so as to allow the foam assembly to be rolled into position for drying.
[0019] In a particular embodiment, around a perimeter of the vacuum box are four side walls configured to abut the sides of the foam assembly. In some embodiments, one or more walls may have vents allowing air to pass through. For example, these vents may be located at typical core heights where two foam layers are adhered together. In one embodiment shown, vents are positioned at 4, 5, 6, 7, 8, and 9 inches from a base of the foam assembly. By allowing air flow over the sides of the foam assembly, particularly at adhesion points, the adhesive may be dried more quickly particularly at the seams.
[0020] Some embodiments of the drying system may be particularly configured and sized for mattress drying (though it may be used for the drying of any foam assembly). As such, one of the side walls may be adjustable to adapt to varying widths of mattresses as shown in the various broken vertical lines of FIG. 4 (discussed in detail below). Further, an end wall may be adjustable to adapt to varying lengths of mattresses as shown by the various broken horizontal lines of FIG. 4 . Once the box is sized, the foam assembly may be moved or slid into position, vacuum drawn, and then moved or rolled out of the box. Sizing of the vacuum area may vary greatly and is not a limiting aspect of the present invention.
[0021] A stationary side or end wall may be equipped with inflatable bag portions along all or part of the side wall. These inflatable bag portions allow a seal to be formed against both side walls by urging against the foam assembly once inflated, and in turn pushing it against the opposing side wall. By forming this seal, air is more directly forced through the foam assembly, increasing air flow through the assembly which in turn increases drying rate of the adhesive. A similar inflatable bag structure may be applied to at least one end wall as well. The bags may then either be deflated to release the foam assembly, or may remain inflated until a differently sized foam assembly is to be dried in the vacuum drying assembly.
[0022] Common mattress sizes include:
[0023] Twin: 38″×74.5″
[0024] Twin XL: 38″×79.5″
[0025] Full: 53″×74.5″
[0026] Full XL: 53″×79.5″
[0027] Queen: 60″×79.5″
[0028] King: 76″×79.5″
[0029] California King: 71″×83.5″
[0030] Accordingly, the adjustable side and end walls of the vacuum box may be adjustable to these sizes to be used for all common mattress sizes. In one embodiment, the adjustable walls may be adjusted to fit within close tolerances (+/−one inch) to these sizes. In another embodiment, the adjustable walls may be configurable to leave a minor spacing between the expected size and the walls, and then the inflatable bags, pads, or the like, may be used to ensure proper sizing. This embodiment may allow for movement into and out of the vacuum box without wall interference or friction. In one non-limiting example, the adjustable walls may be configured to be spaced as follows for the different mattress size operation:
[0031] Twin: 39″×75″
[0032] Twin XL: 39″×81″
[0033] Full: 54″×75″
[0034] Full XL: 54″×81″
[0035] Queen: 61″×81″
[0036] King: 77″×81″
[0037] California King: 72″×85″
[0038] In some embodiments, a heat source may be present on an opposite side of the foam from the vacuum draw side. The heat source serves to heat air that is drawn towards and through the foam assembly. The heat source may be any structure capable of increasing the temperature of ambient air. For example, a convection heat source, infra-red heat source, and the like. In a particular further embodiment, a fan or other air moving structure may force air, such as heated air, towards the foam assembly to further enhance the transport of the air through the foam assembly. Heated air has a greater moisture transport capacity compared to ambient temperature air. Therefore, as heated air is urged through the foam assembly, it picks up more moisture from the foam, allowing the foam to dry faster. In varying embodiments, heated air may range from 80-275 degrees Fahrenheit, but lower and higher temperatures may also be used without straying from the scope of this invention. Typically, embodiments of foam being dried may be able to handle temperatures of up to 250 to 275 F for short periods of time without damage.
[0039] In another embodiment, desiccated, dehumidified, or otherwise dry air may be used for passage through the foam. By passing dry air, as opposed to moist ambient air, through the foam assembly, moisture absorption may be more rapid and efficient. The term “dry air” is used herein to refer not only to fully dry air, but also air that has a lower moisture content than surrounding ambient air. The dry air may be used in addition to the heat source (providing hot, dry air), or as an alternative to it. This dry air embodiment may be particularly useful in non-air conditioned assembly facilities that may have higher than normal humidity levels.
[0040] The present invention has, in initial tests, provided drastically enhanced performance compared to the prior art method of simply letting the foam assemblies rest at ambient conditions. For example, substantial and sufficient drying and adhesion (foam tear) has been achieved in only five minutes of drying using this drying apparatus. Equivalent drying and adhesion of the foam assembly at ambient conditions may take up to six hours or more. Depending on permeability and moisture content of the foam assembly, more or less time on the drying apparatus may be required, however this applies even more so when drying at ambient temperatures. For example, if ten to fifteen minutes on the drying apparatus of the present invention is required, the drying time at ambient temperature may be ten to twelve hours. As such, even if additional time is required on the drying machine, it is on the order of minutes, as opposed to hours using prior art techniques.
[0041] In one embodiment of drying a foam mattress, a top foam layer may be coated with adhesive, and then placed on a core foam layer. In such an embodiment, either the top layer or core may be closest to the vacuum source that draws the vacuum, however typically the core layer will be facing the vacuum attachment. Further, by drawing air through the foam, there is a compression of the layers together, which may aid in final adhesion.
[0042] Any type of foam assembly may be dried using the present invention. As such, the apparatus, rack, funnel, body providing structure for the apparatus, and the like may be any shape and size to receive a particularly sized foam assembly for drying. Further, in some embodiments, an adapter may be installable to allow for varied sizing, while maintaining a snug fitting around the foam assembly so that air does not simply go around the foam assembly instead of through it. Similarly, the present invention may be operated in any orientation, whether that be drawing air downward, to a side, or upwards, without straying from the scope of the present invention.
[0043] In one exemplary embodiment of operation, a laminated foam assembly product may be either transferred from its assembly position onto a support rack of the drying assembly, or may be assembled in place on the drying assembly. Once the foam elements are assembled and laminated together by water-based adhesive, the system may be activated. Activation involves drawing a low pressure area so that the foam assembly is between the low pressure area and the atmosphere, which in turn draws air through the foam assembly. In some embodiments, as noted, this air may be heated by a heating device adjacent to the foam assembly on the opposite side of the assembled foam from the vacuum attachment. In a particular embodiment, air being drawn through the foam assembly by the drying apparatus may be initially heated for part of processing time, and then may be ambient temperature or otherwise cooler than the heated air for part of the processing time. In this embodiment, the foam assembly may be cooled so as not to be excessively hot during packaging. For example, in a five minute drying process, an initial three minutes may be using heated air, while a last two minutes may be using cooler air than the heated air.
[0044] Turning specifically to the figures, multiple embodiments of the present invention are provided. A simple embodiment of the drying system of the present invention is shown in FIGS. 1 and 2 . In these figures, the invention is formed as a body having side walls 10 and end walls 11 . A rack 21 serves as an air permeable base on which a foam assembly may rest. An air outlet 13 below the rack 21 is configured to have a vacuum pump (not shown) attached thereto in order to draw a low pressure below the rack 21 , causing exterior air to pass through the rack 21 (and any foam assembly thereon). A funnel 22 may provide an effective structure of the vacuum attachment to draw the low pressure zone over an entire area of the rack 21 , though it should be understood that any structure may be used.
[0045] FIG. 3 provides a side view of an embodiment of the drying system having a foam assembly 12 resting on rack 21 . The foam assembly 12 , in this embodiment, is formed of a top foam layer 12 A, and a bottom foam layer 12 B, bonded together by an adhesive 12 C. A heat source 31 heats air 32 as it passes towards the foam assembly 12 because of the low pressure zone applied by the vacuum source (not shown) through the air outlet 13 and funnel 22 . Such an embodiment utilizes the ability of heated air to carry more moisture than cool air, which allows more effective removal of water from the foam assembly by the heated air 32 passing through. This air collects moisture and becomes moist air 33 after passing through foam assembly 12 . Moist air 33 moves through the funnel 22 and outlet 13 in direction A as directed by the outlet 13 .
[0046] FIGS. 4-6 provide various views of embodiments of a drying system with an adjustable base to allow for drying of various sized foam assemblies. The device has a stationary side wall 40 , an adjustable side wall 42 , an adjustable end wall 43 , and an end wall 41 . In some embodiments, sidewall 40 and end wall 41 may have a padding or inflatable bag portion 55 to provide pressure against a foam assembly to control air entry at the foam-wall interface. A similar padding or inflatable bag portion 52 may be provided on side wall 40 . As seen in FIG. 4 , the adjustable end wall 43 and side wall 42 may be adjusted to a number of lengths L 1 , L 2 , and L 3 , and a number of widths W 1 , W 2 , W 3 , W 4 , and W 5 , for example. In a particular embodiment, the foam drying system may be integrated into a conveyor system. As such, a foam assembly may enter into the drying system area, be dried for a time period, and then conveyed out of the area using the conveyor rollers 54 . In such an embodiment, the foam may travel in direction D, for example. In a particular embodiment, end walls 41 and 43 may be able to be swung open to allow the foam assembly into and out of the drying base area. In the embodiment shown, hinges 51 allow this motion. Vents 53 are positioned on side wall 40 . These vents 53 allow air to enter the sides of the foam assembly.
[0047] FIGS. 7 through 9 show various embodiments of another embodiment of the adjustable-area system. In this view, adjustment of the area of the drying device is achieved by adjustable walls 72 and 73 , which are connected to air impermeable sheets 74 and 75 respectively. Typically air impermeable sheets 74 , 75 are a rubberized or plastic material, but may also be a heavy fabric, or other membrane. The sheets can be connected to a rolling structure, for example as shown in FIG. 9 , rolled area 91 and spool 92 , to allow the sheet to be retracted by rolling and extended by unrolling. In varying embodiments, only an adjustable end wall or an adjustable side wall may be used, or both may be employed. The adjustable walls 72 , 73 , may be slideable or otherwise movable to the desired position, and fixable in this position during drying operation. This allows for rapid adjustment of the device for variously sized foam assemblies with minimal downtime. The sheets 74 , 75 may be guided by tracks on their ends. Further, each sheet 74 , 75 may have an upwardly extending side wall 73 which provides a face to abut a foam assembly edge. The side wall 73 may be supported in any manner, for example at its ends, at its base, on tracks, and the like. In some embodiments, a force-applying device such as a piston or spring may be utilized to urge the side wall against a foam assembly therein. This structure may function to provide a more air-tight seal between the side wall and edge of the foam assembly to prevent air from leaking between the two.
[0048] While several variations of the present invention have been illustrated by way of example in preferred or particular embodiments, it is apparent that further embodiments could be developed within the spirit and scope of the present invention, or the inventive concept thereof. However, it is to be expressly understood that such modifications and adaptations are within the spirit and scope of the present invention. | A foam drying apparatus is provided. The apparatus is configured to pass air, and in some cases heated and/or dried air, through a quantity of foam. This air passing through the foam absorbs or otherwise carries moisture out of the foam, drying it. The apparatus may utilize a pressure differential on opposite sides of the foam, causing air on the higher pressure side to pass through the foam. Typical applications may include the drying of foam assemblies which use water based adhesives to accelerate drying of the adhesive and/or removal of water from the foam assembly, and packaging of the foam assembly. | 5 |
BACKGROUND OF THE INVENTION
(a) Field of the Invention
The present invention relates to high strength PAN fiber composed of a high molecular weight AN polymer and a method of producing the same.
(b) Description of the Prior Art
PAN fiber, one of the "three big fibers" and ranking with nylon and polyester fibers, is widely used in the field of wearing apparel which makes the most of its characteristics such as clearness of dyed color, bulkiness, etc. The strength of PAN fiber for use in such wearing apparel is in the order of 3 to 4 g/d.
Carbon fiber produced by carbonizing PAN fiber is used as a reinforcing fiber for composite materials because of its excellent physical properties (high strength, high modulus of elasticity). Since the surface condition, cross-sectional shape, physical properties, etc. of the carbon fiber are determined for the most part by the characteristics of the starting material PAN fiber (precursor), its improvements are contemplated actively. However, the strength of the precursor produced on an industrial scale is generally limited to about 5 to 8 g/d.
On the other hand, the aromatic polyamide fibers represented by Kevlar® produced by DuPont, have a strength higher than 20 g/d owing to their stiff molecular structure, and therefore they are establishing a firm position as reinforcing fiber for tire cord and composite material.
In such a situation, appearance of a high strength PAN fiber is expected that can be used as precursor of highly reliable carbon fiber serviceable for astronautics and aeronautics, or that can be used as reinforcing fiber singly. As an attempt in this regard, Japanese Pat. No. 52125/1981 describes that a high strength PAN fiber can be produced by a special technique which comprises solution-polymerizing AN in a concentrated solution of a complex salt (NaZnCl 3 ), under the action of ultra violet rays, in the presence of formaldehyde and hydrogen peroxide; spinning the thus-obtained solution directly into a coagulation bath; and stretching the resulting fibers at the time of coagulation, thereby to form an oriented tissue in the skin portion. However, even by this method, a strength of 16 g/d is attained at the highest.
SUMMARY OF THE INVENTION
Under such circumstances we conducted research for providing a novel high strength PAN fiber which by far exceeds the conventional level. As a result, it has been found that it is possible to produce a PAN fiber having a tensile strength higher than 20 g by integrally combining technical means which comprises using an AN polymer having a special molecular weight, preparing a spinning solution under particular conditions, spinning the solution, coagulating the resulting filaments, subjecting the coagulated filaments to multistage stretching and then drying the filaments. The present invention has been achieved by this discovery.
An object of the present invention is to provide a high strength PAN fiber having a strength not less than 20 g/d which greatly exceeds the level of the conventional technique, and to provide an industrially advantageous method of producing the same. Another object of the invention is to provide a high strength PAN fiber which can exhibit a remarkable effect in industrial use such as reinforcing fiber for tire cord, resin, etc. and precursor for use in carbon fiber. Other objects of the invention will become apparent from the following detailed explanation.
The PAN fiber that can attain such objects of the present invention is a fiber having a tensile strength not less than 20 g/d produced from a polymer mainly composed of AN and having a weight average molecular weight not less than 400,000. Such a PAN fiber can be produced in an industrially advantageous manner by dissolvoing a polymer composed mainly of AN and having a weight average molecular weight not less than 400,000 in a solvent for said polymer while defoaming the solution under reduced pressure; spinning the thus-obtained spinning solution; coagulating it into filaments; subjecting the filaments to multistage stretching under temperature conditions such that the later the stretching stage the higher the temperature; and then drying the filaments at a temperature lower than 130° C. under tension.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
In the production of the PAN fiber having a tensile strength not less than 20 g/d, the object of the present invention, the molecular weight of the polymer is important. It is necessary to use a polymer having a weight average molecular weight not less than 400,000, preferably not less than 800,000. As detailed in Journal of Polymer Science (A-1) Vol. 6, pp 147-159 (1968), said molecular weight is obtained by measuring the intrinsic viscosity, [η], of the polymer in dimethylformamide (DMF) and calculated by the following formula:
[η]=3.35×10.sup.-4 M.sub.w.sup.0.72
wherein M w represents weight average molecular weight.
To produce such a high molecular weight polymer, any method can be used without limitation as long as the polymer has a molecular weight of not less than 400,000. However the polymer can be produced advantageously on an industrial scale by suspension polymerization of the monomer in an aqueous medium containing a water-soluble polymer, in the presence of an oil-soluble initiator, while maintaining an unreacted monomer concentration higher than 9 weight % in the reaction system. As the monomer is used AN alone or a monomer, there mixture composed of more than 85 weight % AN, preferably more than 95 weight % AN and a known comonomer copolymerizable with AN.
The production of a high strength fiber depends on to what extent it is possible to bring all the molecular chains forming the fiber near to the state of the chains extended in the fiber direction to their full length. For the attainment of such a state, it is important to produce a polymer solution (spinning solution) in which the polymer chains are sufficiently disentangled so that the molecular chains can be easily arranged in parallel and oriented in the fiber direction in the steps of spinning and stretching. As examples of the solvents for producing such a polymer solution, there may be mentioned organic solvents such as DMF, dimethylacetamide, dimethyl sulfoxide, etc. and inorganic solvents such as thiocyanates, zinc chloride, nitric acid, etc. In the wet spinning process, inorganic solvents are superior because they give coagulated gel fibers of better uniformity. Among others, thiocyanates are preferred. It is necessary that the polymer concentration should be fixed generally low, because the viscosity of the spinning solution tends to be high owing to the high molecular weight of the polymer. In addition, the concentration depends on the kind of the solvent, molecular weight of the polymer, etc. Therefore, it is difficult to fix it definitely. However, it is desirable to fix it within the range of from 5 to 15 weight %. The dissolution temperature of the polymer is desirably 70° to 130° C. and the viscosity of the polymer at 30° C. is desirably within the range of from 500,000 to 10,000,000 c.p. Since the viscosity of the high molecular weight polymer is high, defoaming becomes extremely difficult once it contains air bubbles. Also, the air bubbles contained in the spinning solution not only lower the parralel arrangement and orientation of the molecular chains but also they themselves form a great defect and a cause of an extreme drop of the strength of the fiber finally obtained. Therefore it is necessary to dissolve the polymer while defoaming the solution under reduced pressure.
As for the spinning method, any of dry-spinning, wet-spinning and dry/wet spinning may be employed. However, because the viscosity is higher in comparison with the usual spinning solution, dry/wet spinning, in which the spinning solution is extruded in air through a spinnerette and thereafter immersed in a coagulation solution, is preferable in respect of spinnability.
In order that the fiber can withstand the severe stretching in the succeeding steps, it is desirable to produce uniform, coagulated gel filaments. Therefore, it is important to establish a coagulation condition under which slow coagulation takes place. Especially recommended spinning method is the use of an inorganic solvent together with a low temperature coagulation below room temperature. When an organic solvent is used, it is preferable to use multistage coagulation in which the filaments are caused to pass successively through coagulation baths containing a non-solvent (precipitating agent) with gradually increased concentrations. The diameter of the coagulated filaments also has an influence on the uniformity of the gel filaments. The finer the better so far as filament breakage does not take place, and in general it is desirable to control the diameter to within the range of from 50 to 300 μ.
In the following, an explanation will be given on stretching, which is the most important step in revealing the latent high strength fiber properties which have been given in the previous steps such as polymer solution preparation, spinning coagulation, etc.
For such a stretching means, it is necessary to conduct multistage stretching under the temperature condition that the later the stretching stage the higher the temperature. An example of preferred embodiment of such multistage stretching is to carry out stretching operations in succession comprising stretching gel filaments containing residual solvent (the so-called plastic stretching), stretching in hot water, once drying as required, and stretching in steam or in a high boiling point medium having a boiling point higher than 100° C. Also, multistage stretching in the same medium at different temperatures is effective in the improvement of stretchability.
Since the stretching in steam generally tends to form voids in the filaments, it is preferable to carry out stretching in a high boiling point medium having a boiling point higher than 100° C., at a temperature from 100° to 180° C., preferably from 120° to 170° C. As such high boiling point mediums, water-soluble polyhydric alcohols are preferable, and examples of such alcohols are ethylene glycol, diethylene glycol, triethylene glycol, glycerin, 3-methylpentane-1,3,5-triol, etc. Among others, ethylene glycol and glycerin are especially recommended. When the stretching temperature exceeds the upper limit of abovementioned range, the filaments will be broken by fusion, so that such a stretching temperature must be avoided.
Dry heat stretching in the temperature range of from 150° to 230° C. may be employed, but is not an advantageous means in respect of stretchability.
When the stretching operation in a high boiling point medium is employed, the filaments are dried after water-washing, and when said stretching operation is not employed the filaments are dried without treatment. When a polyhydric alcohol remains in the finally obtained filaments, it acts as a plasticizer and lowers the strength. Therefore, the filaments must be washed to an alcohol content less than 5 weight %.
The drying operation must be conducted under tension (limited shrinkage, preferably constant length) because when heat relaxation occurs the strength will be lowered. Even under tension, too high a temperature causes a decrease in strength, so that it is necessary to carry out drying at a temperature lower than 130° C., preferably lower than 120° C.
Thus by integrally combining the technical means recommended in the present invention, it has become possible to obtain a PAN fiber, of which the polymer molecular chains are arranged in parrallel and highly oriented, and which has a strength level greatly improved over the conventional one, that is, a tensile strength not less than 20 g/d.
Such a high strength PAN fiber can be widely used as reinforcing fiber for tire cord and fiber-reinforced composite material, and a precursor for producing carbon fiber.
For a better understanding of the present invention, an example is shown in the following. However, the present invention is not limited in scope by the description of the example. In the example, percentages are by weight unless otherwise indicated.
EXAMPLE
Aqueous suspension polymerization of AN was conducted using 2,2'-azobis-(2,4-dimethylvaleronitrile) as the oil-soluble initiator. As the dispersion stabilizer, a partially saponified (the degree of saponification: 87%) polyvinyl alcohol having a degree of polymerization of 2000 was used. By varying the quantity of the initiator, four kinds of polymers (a-d) having various molecular weights shown in Table 1 were produced.
Each of the polymers thus obtained was washed with warm water at 50° C., and after drying and pulverization, it was dissolved in an aqueous 50% solution of sodium thiocyanate, while at the same time the solution was defoamed under reduced pressure. Thus four kinds of spinning solutions were produced.
After filtration, each of the spinning solutions was subjected to wet/dry spinning through a spinnerette having 0.15 mmφ orifices, with the distance between the coagulation bath surface and the spinnerette surface being maintained at 5 mm. The temperature of the spinning solution at the time of extrusion was kept at 80° C., and the coagulation bath was regulated to a sodium thiocyanate concentration of 15% and a temperature of 5° C.
The gel filaments which came out of the coagulation bath were stretched twice in length while washed with deionized water. The filaments which left the washing step were then stretched twice in hot water of 85° C., 2.5 times in boiling water and subjected to 2-stage stretching in ethylene glycol (EG). The first EG bath was maintained at 130° C. and the second bath at 160° C. The stretching ratio in each bath was varied as shown in Table 1.
The filaments which came out of the second EG bath were washed with warm water of 60° C. until the residual EG content in the filaments reached an amount less than 0.5 weight %, and were dried at 100° C. under tension. Thus four kinds of fibers (A-D) were produced. Fiber (E) was produced in the same way as Fiber (B) except that the drying temperature was 140° C.
The thus-obtained five kinds of fibers were measured for the tensile strength. The results are shown in Table 1. The tensile strength is a value measured by the constant speed elongation tester (UTM-II-type Tensilon) of the tensile testing method of fibers according to JIS L 1069, with a grip gap of 20 mm and an elongation speed of 100%/min.
TABLE 1______________________________________ Specimen of the present Specimen for invention comparisonFiber name A B C D E______________________________________Spinning Polymer a b c d esolution name Polymer 2280,000 450,000 320,000 120,000 450,000 molecular weight Polymer 5 11 15 24 11 concen- tration (%)Stretch- First bath 1.8 1.8 2.0 2.0 1.8ing ratio Second 1.6 2.0 3.0 4.0 2.0EG bathTotal stretching ratio 28.8 36.0 60.0 80.0 36.0Tensile strength (g/d) 25.1 20.5 15.5 8.6 15.3______________________________________
From the above Table, it is understood that, when a polymer of AN having a molecular weight less than 400,000 is employed, a PAN fiber having a sufficient strength cannot be obtained even by employing the spinning and after-treating methods recommended in the present invention, and also in the case of the fiber of which the drying temperature is outside of the upper limit of the range of the present invention (Fiber E), a high strength cannot be obtained, whereas the fibers of the present invention have excellent strength. | Polyacrylonitrile (PAN) fiber of high strength (tensile strength≧20 g/d) produced from a polymer composed mainly of acrylonitrile (AN) and having a weight average molecular weight not less than 400,000, and a method of producing said fiber characterized by a multistage stretching step and a drying step under particular conditions. | 3 |
The invention concerns a superimposed steering gear for tracklaying vehicles wherein the steering power required for turning is superimposed on the drive system via a neutral shaft and summarizing differentials and the neutral shaft is driven from a drive shaft of the steering gear via a hydrostatic-mechanical branching transmission which has a reversing transmission in its mechanical power branch and a hydrostatic unit of infinitely variable translation in its hydrostatic power branch. Both power branches being passed together into a summarizing transmission so that a desired steering radius can be adjusted within a mechanically shiftable radial range by changing the traverse angle of the hydrostatic unit.
In superimposed steering gears of the kind mentioned (German Patent No. 24 12 562), when using a hydrostatic-mechanical power branching steering, the radii both for left-hand and right-hand turns can be respectively adjusted within two mechanically shiftable radial ranges by infinite variation of the hydrostatic unit. Departing from the straight-ahead drive of the tracked vehicle, there is provided first in both steering directions a first radial range in which the whole steering power is conveyed via a hydrostatic unit and a stepdown gear rear-mounted on the neutral shaft. To this first radial range, which is delimited by the maximum negative and the maximum positive angle of the hydrostatic unit, there is attached at any given time an additional radial range which reaches down to the smallest steering radius and in which there takes place, by shifting two planetary transmissions, a summarization of the powers flowing in different directions of rotation over the hydrostatic and over the mechanical part.
Although only a small part of the steering power flows through the hydrostatic unit that works with poor efficiency, the required volume of construction of said unit and its power losses still are too great.
SUMMARY OF THE INVENTION
Therefore, the problem to be solved by the invention is to overcome said disadvantages and thus to accommodate in a given space an infinite hydrostatic-mechanical steering gear with the best possible efficiency.
This problem is solved by the fact that the summarizing transmission has at least two shiftable planetary-gear sets, one transmission component of each being connected with the drive shaft, via the reversing transmission, and one transmission component of each being connected with a hydrostatic shaft of the hydrostatic unit; the remaining transmission components can be coupled with the neutral shaft, by means of coupling shafts, for shifting at least two radial ranges according to the steering direction, the respective coupling shafts having equal speeds for infinite switching from one radial range to the next at a positive and negative maximum translation of the hydrostatic unit. Due to the fine distribution of the whole steering radius in individual radial ranges, on one hand, it is possible to minimize the power losses of the hydrostatic unit, which can also have a smaller volume due to the low flow of power over said hydrostatic unit and, on the other hand, a quicker change of the steering radii is possible, since a quick switch to another steering radii can take place in the mechanical part of the branching transmission.
When the summarizing transmission has two shiftable planetary-gear sets and, in order to produce a first radial range departing from the straight-ahead driving of the tracked vehicle, between the output shaft and the neutral shaft a stepdown transmission is shiftable in parallel, then in the maximum translation of the hydrostatic unit both coupling shafts must have equal speeds at the shift point of the separating clutches coordinated with them, while when the translation changes in the direction of an opposite maximum value, the second coupling shaft becomes infinitely quicker for smaller steering radii and the first coupling shaft becomes infinitely slower for larger steering radii up to a speed value resulting from the speed of the output shaft reduced by the step-down transmission. A continuously infinite speed change of the neutral shaft can be produced even if, at the time, there is shift from one planetary-gear set to the other within the summarizing transmission. Due to the simultaneous reduction of speed in one planetary-gear set upon the increase of speed on the coupling shaft of the other planetary-gear set, it is possible to avoid great idling losses.
A simpler and more compact construction of the stepdown transmission results by designing it as planetary-gear step wherein a ring gear is directly fastened on the neutral shaft while the planetary gears, brakable with the housing via the stem, are driven by the output shaft of the hydrostatic unit. In this radial range, the required steering radius is purely hydrostatically adjusted in both steering directions.
A compact reversing transmission is produced by the fact that in a direct through-drive step a central intermediate shaft of said reversing transmission can be directly coupled with the drive shaft while a reversal in the direction of rotation is operated via two planetary-gear transmissions, the sun gears of which are non-rotatably connected with the intermediate shaft, there taking place a reversal in the direction of rotation of the intermediate shaft by the planetary gears of the first planetary transmission and the planetary gears of the second planetary transmission firmly coupled on the housing by their stems.
An alternative design of the reversing transmission, which presupposes small radial dimensions, has double planetary gears of which one meshes with an external central gear driven by the drive shaft and the other with an internal central gear non-rotatably situated on an intermediate shaft which leads to the summarizing transmission. In the direct through-drive of the reversing transmission, the spider shaft is coupled with the drive shaft while, in a reversing step, the spider shaft can be firmly braked with the housing.
A reversing transmission can be optionally provided which likewise has double planetary gears the spider shaft of which is driven by the drive shaft, one planetary gear of the double planetary-gear set being connected via an internal central gear with the intermediate shaft and the other planetary gear meshing with an internal central gear which can optionally be coupled with the spider shaft (direct through-drive) or be firmly braked with the housing (reverse step).
Finally, there is also the possibility of providing a planetary-gear transmission as a reversing transmission wherein the drive shaft and the intermediate shaft can be directly coupled with each other while a reversing step is effected by means of a regressing bevel-gear transmission driven by the drive shaft and apt to be coupled with the intermediate shaft.
When, as proposed below, in the summarizing transmission an external central gear of the planetary-gear set coordinated with the first coupling shaft and a stem of the planetary-gear set coordinated with the second coupling shaft are jointly operatively connected with the hollow shaft, and their sun gears are fastened on the output shaft, it is possible in this manner to produce in the transition, from one radial range to the next, in the maximum value of the translation of the hydrostatic unit, coinciding speeds of the two coupling shafts between which the shift is to be carried out.
Finally, the superimposed steering gear can be compactly designed in axial dimensions and the driving elements are eliminated when the stepdown transmission is directly situated on the transmission end of the hydrostatic unit.
The invention is not limited to the combination of features of the claims. Other logical possible combinations result for the expert from the claims and separate features of the claims when the problem arises.
For further explanation of the invention, reference is made to the drawings in which four embodiments are shown in a simplified manner.
BRIEF DESCRIPTION OF THE DRAWING
FIG. 1 is a diagrammatic illustration of a superimposed steering gear of a tracklaying vehicle according to the invention;
FIG. 2 is an enlarged section II from FIG. 1 in the area of a summarizing transmission of the superimposed steering gear;
FIG. 3 is a diagram where the course of the angle of tranverse of the hydrostatic unit is coordinated with the separate radial ranges;
FIG. 4 is a table from which result the shifting elements that are actuated in the individual radial range;
FIG. 5 is a alternative design of a reversing transmission;
FIG. 6 is an alternative design of a reversing transmission; and
FIG. 7 is an alternative design of a reversing transmission.
DESCRIPTION OF THE PREFERRED EMBODIMENT
In FIG. 1, a drive unit of a tracklaying vehicle is shown consisting of an internal combustion engine 1, a gear-shift part 2, a superimposed steering gear 3 and a left-hand and a right-hand summarizing differential 4 and 5, respectively. The superimposed steering gear 3 is driven by a drive shaft 6 at a speed which stays at a consistent ratio in relation to the drive speed of the internal combustion engine 1.
The drive shaft 6 is, on one side, connected via an impeller shaft 7 with a hydraulic pump 8 of a hydrostatic unit 9, and in addition a hydraulic motor 10 belonging to the hydrostatic unit 9. The delivery rate of the hydraulic pump 8 is preferably regulatable while the hydraulic motor 10 has a constant absorption volume. A hydrostatic shaft 11 which, on one side, communicates with a stepdown transmission 12, is attached to the hydraulic motor 10 on the exit side. Said stepdown transmission 12 is constructed as a simple planetary-gear set, the sun gear 13 of which is directly fastened on the hydrostatic shaft 11, while the planetary gears 15, that mesh with the sun gear 13 and with a ring gear 14, are supported on a stem 17 which can be firmly braked with the housing via a brake 16. The ring gear 14 of the stepdown transmission 12 is, for its part, fastened on a neutral shaft 18 which forms the output component of the superimposed steering gear 3.
On the other side, a reversing gear 19, which shifts translations of +1 an -1, can be coupled with the drive shaft. The reversing gear 19 has a first planetary transmission, the external central gear 20 of which is connected non-rotatably with the drive shaft 6, while the internal central gear 21 of which engages an intermediate shaft 22. Planetary gears 23, supported on a planetary-gear carrier 24, are meshed with both the internal central gear 21 and the external central gear 20, said planetary-gear carrier 24 being, in turn, non-rotatably connected with a ring gear 25 of a second planetary gear of the reversing transmission 19. Planetary gears 28, supported on a stem 27, mesh with said ring gear 25 of the second planetary transmission and with a sun gear 26 which is likewise non-rotatably connected with the intermediate shaft 22. The stem 27 can be firmly braked with the housing by means of a brake 29. The intermediate shaft 22 has, in addition, a clutch 30 by means of which it can be directly coupled with the drive shaft 6.
A summarizing transmission 31 is attached to the reversing gear 19, the construction of which is explained with reference to the enlarged segment of FIG. 2. According to FIG. 2, the external central gear 33 of a first planetary-gear set 32 of the summarizing transmission 31 is driven by the intermediate shaft 22. Planetary gears 34, the stem 35 of which is connected with a first coupling shaft 36, are coordinated with said external central gear 33.
Besides, an operative connection exists between the intermediate shaft 22 and a stem 37 of a second planetary-gear set 39 of the summarizing transmission 31. On said stem 37, planetary gears which mesh with an external central gear 40 connected with a second coupling shaft 41 are supported. Both the internal central gear 42 of the first planetary-gear set 32 and the internal central gear 43 of the second planetary-gear set 38 are non-rotatably connected with the hydrostatic shaft 11. Finally, the neutral shaft 18 can be coupled with the first coupling shaft 36 via a clutch 44 or the second coupling shaft 41 via a clutch 45.
According to FIG. 1, the neutral shaft 18 is connected at one end, via a gear 46 and intermediate gear 47, with the summarizing differential 4. At its other end, the neutral shaft 18 is connected, via a gear 28 and two intermediate gars 49 and 50, with the summarizing differential 5. Besides, the summarizing transmissions 4 and 5 designed as planetary-gear transmissions are driven, starting from the transmission part, via transmission output shafts 51 and, on the exit side, each are connected with a sprocket gear 52 of the tracklaying vehicle. When turning, the summarizing differentials 4 and 5 are thereby overlaid with the differently oriented steering power from the superimposed steering gear 3.
In the diagram of FIG. 3, the obtainable radial ranges for right-hand steering RI to RIII and for the left-hand steering LI to LIII are coordinated with the angle of traverse, that is, the changed flow rate of the hydraulic pump 8. There exists here a direct connection with the table of FIG. 4. In the table, the shifting elements of the reversing transmission 19, of the stepdown transmission 12 and of the summarizing transmission 31 are set forth to be acutated upon each change of the radial range. The shift elements to be actuated into the respective radial range are marked with dots.
The operation of the superimposed steering gear is explained with reference to the diagram of FIG. 3, to the table of FIG. 4 and to the diagrammatic illustration of the drive unit in FIG. 1:
When the tracklaying vehicle travels straight ahead, the hydrostatic unit 9 is in a position in which no power is transmitted from the drive shaft 6 to the neutral shaft, that is, the positioning angle of the hydraulic pump amounts to 0°. Since neither the shifting elements in the reversing transmission nor in the summarizing transmission are actuated over said power branch no power likewise is transmitted to the neutral shaft 18. The brake 16 of the stepdown transmission 12 is engaged for steering away from the neutral position.
If the superimposed steering gear 3 is now actuated in direction of a right-hand turn by adjusting the steering element, not shown, of the tracklaying vehicle, then the flow rate of the hydraulic pump changes by the change of its angle of traverse until reaching a maximum negative value -γ max . The consequence of this is that the speed of the neutral shaft 18 changes in proportion to the change of the angle of traverse up to a negative value determined by the output speed of the hydrostatic unit 9 and the translation ratio of the stepdown transmission 12. The clutch 30 of the reversing transmission 19 is already actuated during said phase. In the radial range RI, with a maximum angle of traverse of the hydrostatic unit 9, the stepdown transmission 12 limits in the negative direction the speed of the neutral shaft 18 to a maximum value which corresponds to the speed of the first coupling shaft 36 driven with branched power via the hydrostatic shaft 11, the intermediate shaft 22 and the first planetary-gear set 32. An infinite changeover from the radial range RI to the radial range RII thus results by the fact that the first coupling shaft 36 is coupled by the clutch 44 with the neutral shaft 18 whereupon the brake 16 of the stepdown transmission 12 is released.
In the second radial range for right-hand steering RII, the speed of the intermediate shaft 22 corresponds to the speed of the drive shaft 6 since the reversing transmission is directly shifted through the actuation of the clutch 30. The steering power flows, branched over the hydrostatic unit 9 and the hydrostatic shaft 11, to the first planetary-gear set 32 of the summarizing transmission 31 while the mechanical portion of the steering power flows over the reversing transmission 19 and the intermediate shaft 22 to the first planetary-gear set 32. Within said radial range RII, the hydrostatic unit 9 is again adjusted to its maximum positive angle of traverse +γ max . On the second coupling shaft 41 of the second planetary-gear set 38 there becomes adjusted, due to the power-branched drive of the stem 37 of the intermediate shaft 22 and of the internal central gear 43 of the hydrostatic shaft 11, at a maximum angle of traverse +γ max , a speed corresponding to the speed of the neutral shaft 18 at that moment.
The clutch 45 is actuated in this state, that is, at a maximum positive angle of traverse of the hydrostatic unit 9, so that the second coupling shaft 41 is coupled with the neutral shaft 18. The clutch 44 of the first coupling shaft is then opened. In this third radial range, which includes the smallest turning radii, the hydrostatic unit 9 is again adjusted up to a maximum negative angle of traverse, the absolutely highest speed of the neutral shaft 18 resulting finally in this maximum value -γ max of the shifted radial range RIII so that by virtue of the high superimposed speed of different directions of rotation on the summarizing differentials 4 and 5, a smallest steering radius for the right-hand steering results.
In a left-hand turn of the tracklaying vehicle, the hydrostatic unit 9 and the summarizing transmission 31 act together basically in the same manner only that in the comparable radial range LI to LIII the angle of traverse of the hydrostatic unit is adjusted in an opposite direction. Besides, in said radial ranges LI, LII and LIII, unlike in the right-hand steering, it is the brake 29 instead of the clutch 30 that is actuated in the reversing transmission. Thus, a reversal in the direction of rotation on the mechanical power portion transmitted to the intermediate shaft 22 occurs in the reversing transmission 19. From FIG. 2, it can be seen that with the superimposed steering gear 3 built according to the invention, both the whole right and left turning radii of a tracklaying vehicle can be divided in three sections. The mechanical part (summarizing transmission 31, stepdown transmission 12 and reversing transmission 19) is selected in a manner such that the hydrostatic portion of the power branching is equally large in each section and thereby it is possible optimally to utilize the hydrostatic transmission unit in relation to its efficiency. Each whole radial range can basically be divided in more than three sections when deemed convenient by enlarging the summarizing transmission 31.
In FIG. 5 to 7, three other variants of the construction of the reversing transmission 19 are shown. According to FIG. 5, the reversing transmission 19 has double planetary gears 53 of which one planetary gear 53A is engaged with an external central gear 54 driven by the drive shaft 6. The other planetary gear 53B is engaged with an internal central gear 55 situated on the intermediate shaft 22. A spider shaft 56, which is attached to an element that supports the double planetary gears 53, can be connected with the drive shaft 6 for a direct through-drive by means of a clutch 57 or can be braked firmly with the housing by means of a brake 53 for shifting of a reversing step.
In the embodiment of the reversing transmission 19 of FIG. 6, double planetary gears designated by 59 are provided, the planetary gear 59A of which meshes with an internal central gear 60 non-rotatably situated on the intermediate shaft 22. The other planetary gear 59B meshes with an internal central gear 62. The reversing transmission 19 of the drive shaft 6 is driven via a spider shaft 61, it being possible to couple the internal central gear 62 with the spider shaft 61 for shifting a direct through-drive and to brake the internal central gear 62 firmly with the housing for a reverse step.
Finally, in the embodiment of FIG. 7 the drive shaft 6 can be coupled with the intermediate shaft 22 via a clutch 64. To shift a reverse step, a regressing bevel-gear drive 63 is available, which is driven by the drive shaft 6 and can be coupled with the intermediate shaft 22 via another clutch 65.
Referenced numerals
1 internal combustion engine
2 gear shift part
3 superimposed steering gear
4 summarizing differential
5 summarizing differential
6 drive shaft
7 impeller shaft
8 hydraulic pump
9 hydrostatic unit
10 hydraulic engine
11 hydrostatic shaft
12 stepdown gear
13 sun gear
14 ring gear
15 planetary gears
16 brake
17 stem
18 neutral shaft
19 reversing transmission
20 external central gear
21 internal central gear
22 intermediate shaft
23 planetary gears
24 planetary-gear carrier
25 ring gear
26 sun gear
27 stem
28 planetary gears
29 brake
30 clutch
31 summarizing transmission
32 first planetary-gear set of 31
33 external central gear of 32
34 planetary gears of 32
35 stem of 32
36 first coupling shaft
37 stem of 38
38 second planetary-gear set of 31
39 planetary gears of 38
40 external central gear of 38
41 second coupling shaft
42 internal central gear of 32
43 internal central gear of 38
44 clutch
45 clutch
46 gear
47 intermediate gear
48 gear
49 intermediate gear
50 intermediate gear
51 transmission output shafts
52 sprocket gear
53 double planetary gears
53A planetary gears of 53
53B planetary gears of 53
54 external central gear
55 internal central gear
56 spider shaft
57 clutch between 6 and 56
58 brake
59 double planetary gears
59A planetary gears of 59
59B planetary gears of 59
60 internal central gear on 22
61 spider shaft
62 internal central gear
63 regressing bevel-gear drive
64 clutch between 6 and 22
65 clutch between 63 and 22 | In a superimposed steering gear (3) for tracklaying vehicles in which the steering power needed for turning is superimposed on the drive system via summarizing differentials and which has a hydrostatic-mechanical power branching summed up in a summarizing transmission (31), the power losses of the hydrostatic branch that works with poor efficiency are kept as small as possible and, at the same time, an infinite steering is made possible over all radial ranges. For this purpose, the summarizing transmission (31) is shiftable into steps that cover at least two radial ranges, a speed adaptation to the transmission components taking place at any given time in the shift points for an infinite transition. | 5 |
CLAIM OF PRIORITY
[0001] This application claims priority to Japanese Patent Application No. 2001-218949 filed on Jul. 19, 2001.
BACKGROUND OF THE INVENTION
[0002] 1. Field of the Invention
[0003] The present invention relates to an identification apparatus for identifying an individual using vital information, and, more particularly, the present invention relates to a finger identification apparatus that utilizes a hemal pattern of a finger and methods therefor.
[0004] 2. Description of the Background
[0005] An individual identification technology is expected to enable the safe management of property and/or information. In particular, living body (personal) identification technologies that utilize parts of a human body as a key are beginning to attract attention. One reason for this is because a living body identification technology has a reduced chance for an illegal access to property or information resulting in a loss or robbery as compared to conventional technologies for managing property and information using a password or a key. Living body identification technologies include various techniques based on a fingerprint, a face, an iris, or a hemal pattern of a hand or a finger.
[0006] Among these techniques that are currently under study, the identification technique utilizing a hemal pattern of a finger is advantageous in that: (1) the technique reduces a user's reluctance to undergo identification because the technique is not associated with crime (unlike a technique utilizing a fingerprint); (2) the technique does not require direct irradiation of light into an eye (unlike a technique utilizing an iris); and (3) the technique reduces the possibility of forgery because it reads an internal feature of a living body instead of a superficial feature thereof.
[0007] The process for identifying an entity utilizing a hemal pattern of a finger will be described below. Initially, a light source for radiating near-infrared light is made available, and a camera is placed facing the light source so that the camera can pick up only light emanating from the light source image. The camera is provided with an optical filter that passes light with wavelengths which fall within the near-infrared band. For identification, a finger is interposed between the camera and light source in order to image the finger. Since hematic components absorb near-infrared light efficiently, the digital blood vessels do not transmit light and are therefore visualized dark (i.e., appear dark in the resultant image). The resultant image of a hemal pattern is then compared with an image of a registered pattern, whereby individual identification may be performed.
[0008] In order to correctly determine a correspondence between a hemal pattern and a registered pattern, an image must be produced under the same conditions for imaging between registration and identification. For example, if a finger is turned, a visualized hemal pattern is quite different from a registered pattern. As long as a finger is displaced or turned with its surface to be imaged held unchanged, an image of a hemal pattern produced during identification can be corrected readily through image processing. However, if a finger is so turned that the surface thereof is reversed from the dorsal side to the ventral side or vice versa, an image of a hemal pattern cannot easily be corrected because some blood vessels are unknown.
[0009] For example, an identification apparatus that utilizes the hemal pattern of the palm of a hand directs a user to hold a guide bar with his/her four fingers for positioning. The position of the palm of an individual's hand to be imaged is thus made invariable. However, as far as the digital blood vessels are concerned, if a user holds the bar or the like with his/her fingers, or, if a user stresses his/her fingers in some way, the digital blood vessels are compressed (as described above). Consequently, part of a hemal pattern may be missing or obscured. Another conceivable method is such that a guide rail or the like is included and a user is asked to place his/her fingers at a specified position on the guide rail. However, this method requires a user to learn how to place his/her fingers correctly. This means that not everybody can easily use the apparatus.
[0010] Moreover, a visualized hemal pattern varies depending on the posture of a finger inserted in an identification apparatus. For example, when a finger extended excessively with force has the blood vessels thereof compressed due to the epidermal stress, part of a hemal pattern may be missing. When extraneous light illuminating the entire identification apparatus changes, the brightness or contrast of a produced image varies. This may adversely affect precision in identification. Specifically, near-infrared light contained in ordinary sunlight or illumination light may adversely affect visualization of a hemal pattern.
SUMMARY OF THE INVENTION
[0011] Accordingly, the present invention preferably provides a low-cost identification apparatus that keeps the conditions for imaging uniform among identifications and directs a user to perform only a series of simple maneuvers. The related arts fail to guarantee that the conditions for imaging are the same among identifications.
[0012] In order to address one or more of the above objectives, according to the present invention, there is provided a finger identification apparatus comprising: a guide unit; a switch member; a light source; an imaging unit; and an identifying unit. The guide unit helps position a finger for identification. The switch member is preferably turned on or off with the fingertip. The light source that radiates transmissive light which is transmitted through a finger is placed opposite the imaging unit with a space for finger insertion located therebetween. When the switch member is turned on, the identifying unit performs identification on an image produced by the imaging unit.
[0013] Additionally, according to the present invention, there is preferably provided a finger identification apparatus comprising: a guide unit; a light source; an imaging unit; and an identifying unit. The guide unit helps position a bent finger. The light source that radiates transmissive light which is transmitted through a finger is placed opposite the imaging unit with a space for finger insertion located therebetween. The identifying unit performs identification on an image produced by the imaging unit.
[0014] The use of the present invention preferably leads a finger smoothly (and repeatably) to a specific position and orientation. Furthermore, since the digital blood vessels are not compressed, a resultant image may be collated with a registered image on a stable basis. This results in markedly improved precision in identification.
BRIEF DESCRIPTION OF THE DRAWINGS
[0015] For the present invention to be clearly understood and readily practiced, the present invention will be described in conjunction with the following figures, wherein like reference characters designate the same or similar elements, which figures are incorporated into and constitute a part of the specification, wherein:
[0016] FIG. 1 shows an example of an apparatus according to the present invention;
[0017] FIG. 2 shows an example of the configuration of an apparatus according to the present invention;
[0018] FIG. 3 shows an example of a process flow performed by software used to implement the present invention;
[0019] FIG. 4 shows an exemplary cross-section of a structure which is included in an apparatus and into which a finger is inserted;
[0020] FIG. 5 shows an exemplary button switch;
[0021] FIG. 6 shows an exemplary finger rest;
[0022] FIG. 7 shows another example of an apparatus according to the present invention;
[0023] FIG. 8 shows an example of the elements included in an optical system used to implement the present invention;
[0024] FIG. 9 shows an example of a processing flow performed by software used to perform light level control according to the present invention;
[0025] FIGS. 10A and 10B show an exemplary device for measuring the thickness of a finger according to the present invention;
[0026] FIG. 11 includes three side views of a finger identification apparatus according to the present invention;
[0027] FIG. 12 is a perspective view showing the assembly of components of a finger identification apparatus according to the present invention;
[0028] FIG. 13 shows a cross-section of a structure which is included in an apparatus in accordance with a second embodiment and into which a finger is inserted; and
[0029] FIG. 14 shows an example of a finger identification apparatus including a keypad.
DETAILED DESCRIPTION OF THE INVENTION
[0030] It is to be understood that the figures and descriptions of the present invention have been simplified to illustrate elements that are relevant for a clear understanding of the present invention, while eliminating, for purposes of clarity, other elements that may be well known. Those of ordinary skill in the art will recognize that other elements are desirable and/or required in order to implement the present invention. However, because such elements are well known in the art, and because they do not facilitate a better understanding of the present invention, a discussion of such elements is not provided herein. The detailed description will be provided hereinbelow with reference to the attached drawings.
[0031] FIG. 1 schematically shows an identification apparatus 100 according to the present. The body of the apparatus is broadly divided into a light source unit 102 and an imaging unit 104 . A space is created between the light source unit 102 and the imaging unit 104 . For identification, a finger is inserted into this space. The light source unit 102 preferably covers over the space into which a finger is inserted and intercepts (shields) illumination light radiated from the ceiling or other external source to prevent a direct invasion of the light into the imaging unit. In the FIG. 1 embodiment, the space is not enclosed with a side wall. Alternatively, the space may be enclosed with one or more side walls in order to hinder lateral invasion of extraneous light. In this case, the side walls are preferably coated with a dye such as an anti-reflection coat in order to prevent irregular reflection of near-infrared light, or the side walls are preferably made of an anti-reflection material. This is intended to improve precision in identification.
[0032] The light source unit 102 has a light source 106 which radiates near-infrared light whose wavelengths are about 810 nanometers (nm) towards a camera 114 included in the imaging unit 104 . A finger is inserted into the space between the light source 106 and camera 114 , whereby near-infrared light is transmitted through the finger and picked up the camera 114 . Consequently, the hemal pattern of the finger is imaged. A guide groove 112 helps the user intuitively understand the correct position at which a finger should be located and the direction in which the finger should be oriented. A button switch 108 is preferably located at a position at which a fingertip reaches when a finger is placed along the guide groove 112 .
[0033] An opening 110 is located to coincide with a portion of the finger including the first and second joints thereof. The opening 110 is covered with a transparent glass plate, a transparent acrylic plate, or other material which passes light and prevents invasion of foreign objects into the inside of the identification apparatus. The camera 114 requires an optical filter that transmits only light whose wavelengths fall within the near-infrared band. An optical filter plate may be substituted for the glass or acrylic plate, whereby the capabilities of the glass or acrylic plate and of the optical filter can be integrated.
[0034] The identification process is initiated when a user presses the button switch 108 . The maneuver of pressing a button is an action people perform frequently in their daily lives. Therefore, a user should quickly get accustomed to this maneuver of pressing a button. Every time a user places his/her finger in a natural manner so as to press the button 108 , the user's fingertip is located at a substantially fixed position. In this way, the finger can be smoothly placed at a position which can be repeated by the finger.
[0035] Once the fingertip is positioned, the finger is guided along the guide groove 112 . The direction in which the entire finger is oriented is determined accordingly. A region of the finger lying over the opening 110 is thereby determined, and a range thereof to be imaged is nearly uniquely determined. Moreover, when the user presses the button 108 , the finger joints are bent in a fixed direction. The ventral part of the fingertip is naturally oriented in a direction perpendicular to a direction in which the button is dented. If a finger is turned sideways, the surface of the finger to be imaged may be changed, that is, the dorsal part of the finger may be imaged at one time, and the ventral part thereof may be imaged at another time. However, this will not take place because of the bending action.
[0036] When a user presses the button 108 with his/her finger, the finger is bent naturally. The epidermis of the user's hand other than the epidermis of the finger will not be stressed. Therefore, the digital blood vessels will not be compressed, and no part of the hemal pattern will be missing. Moreover, as long as the finger is bent naturally, the finger will not touch the glass plate covering the opening 110 . Therefore, the possibility that a finger touches the glass plate and that the digital blood vessels are compressed or the glass plate gets dirty will be reduced.
[0037] As long as the position at which a finger is placed is nearly fixed, the area of the opening 110 may be made sufficiently small so that the opening 110 is blocked with a finger. If extraneous (external) light can be blocked, a change in brightness or contrast caused by the extraneous light can be prevented. In the conventional methods, because the position at which a finger is placed is not fixed, the opening is made rather large in order to image a wide area on the finger. A portion of the image depicting the same hemal pattern as the one visualized during registration must then be searched. Therefore, high-cost hardware for computation is needed to search the same hemal pattern as the one visualized during registration. Since the conventional opening is large, extraneous light easily enters. An identification apparatus in accordance with the conventional method is therefore susceptible to “noise”. This drawback is addressed through the inclusion of the button 108 .
[0038] Moreover, the conventional identification technique based on a hemal pattern of a finger does not present a means for requesting the start of the identification process such as a switch to be manipulated by a user. The identification apparatus itself determines the start of the identification, which may confuse some users. The inclusion of the button switch 108 itself is therefore effective in improving maneuverability.
[0039] It should be noted at this time that the guide groove 112 is not limited to the illustrated shape. Moreover, a finger need not always touch the guide groove 112 . For example, a wire-like guide or a guide shaped (e.g., like a finger rest) will do. In short, something capable of guiding a finger unidirectionally is sufficient for the present invention.
[0040] FIG. 11 includes a top and two side views of an alternative embodiment of the present invention from that shown in FIG. 1 . As shown in FIG. 11 , the distance from the upper part of the structure to the lower part thereof at the apparatus opening is different from the space created between the upper and lower parts at the deep end of the apparatus. Moreover, the surfaces of a light source 106 included in the upper part and of the opening 110 included in the lower part are arched in this embodiment. The curvature of the arched surface of the upper part is preferably larger than that of the arched surface of the lower part. Because of this design, when a finger is inserted into the structure, even if the ventral part of the finger is oriented sideways or obliquely, the orientation of the finger is corrected smoothly so that the ventral part of the finger will face down as the finger is advanced to the deep end of the space. This is because the space gets narrower towards the deep end thereof. Furthermore, near-infrared light emanating from the light source 106 is radiated evenly because of the curvature. Moreover, the distance from a camera 114 to any point in the opening 110 is uniform. This leads to identification with higher precision.
[0041] FIG. 2 is a schematic block diagram showing the configuration of an identification apparatus according to the present invention. A finger of a hand 200 is inserted in a space created between a light source 106 and a camera 114 . With a press of a switch 108 , an image signal representing a hemal pattern is acquired. The image signal transferred from the camera 114 is converted into digital data by an image capturing device 202 and is stored in a memory 210 via an input/output interface 206 of a computer 204 . The switch 108 is connected to the computer via an input/output interface. The on/off state of the switch 108 is stored in the memory 210 .
[0042] The instant the switch 108 is turned on, an interrupt signal is generated and transmitted to a CPU 208 . When the CPU 208 confirms that the switch 108 is turned on, or when the CPU 208 senses generation of the interrupt signal indicating that the switch 108 is turned on, the CPU 208 activates and runs a software program that performs identification. Based on the results of the identification performed by the program, the CPU 208 executes any of various control sequences. Namely, the CPU 208 may display the result on a display device 212 or transmit an appropriate instruction signal to a control target 216 , for example, that a door should be opened or closed. A keyboard 214 may be used to enter auxiliary information concerning identification, for example, a password.
[0043] FIG. 12 is a perspective view showing exemplary components of the finger identification apparatus shown in FIG. 11 and FIG. 2 which are to be assembled.
[0044] FIG. 3 shows an example of a processing flow performed by software run by the hardware, or especially, the CPU 208 . During processing 300 , the entire hardware is initialized, and initial values are assigned to temporal variables needed to run the program. Once hardware initialization is complete, the program preferably becomes idle and waits until the switch 108 is turned on ( 302 ). When the switch 108 is turned on, an image of a finger picked up by the camera 114 is stored in the memory 210 ( 304 ). Image processing is performed on the stored image data in order to extract the features of a hemal pattern ( 306 ). A registered pattern to which the hemal pattern corresponds is searched for, or in other words, the hemal pattern is collated with registered patterns ( 308 ). If any registered pattern corresponds to the hemal pattern ( 310 ), a signal indicating that a correct access authority is identified or identification data concerning an identified individual is transmitted to a control target such as equipment or a software program that requires identification ( 312 ).
[0045] A standby state is then preferably re-established and retained until the switch is activated again. The power supply of the hardware may also be turned on or off responsive to the on/off operation of the button switch 108 . When the button switch 108 is pressed, the power supply is preferably turned on. The foregoing processing flow is performed except step 302 until step 310 is completed. If identification succeeds, the steps ending with step 312 are executed successively. Thereafter, the power supply is turned off again. Thus, power consumption required in a standby state can be minimized.
[0046] The on/off operation of the light source may also be controlled. When the button switch 108 is turned on, the light source is preferably turned on at the same time. When identification is completed, the light source is turned off at the same time. With respect to the on/off operation of the power supply of the apparatus, it may take an extended amount of time to activate the apparatus, although this factor depends on the configuration of the apparatus. Therefore, when an emphasis is put on timing, efforts should be made to save power required by the light source alone. The on/off operation of the light source may be physically interlocked with the on/off operation of the switch 108 . A switching circuit including relays and transistors may be connected to the input/output interface 206 of the computer 204 , whereby a switch used to turn on or off the light source may be electronically controlled.
[0047] The above type of electronic control circuit having a switch turned on or off quickly can also be used to control so-called “pulse width modulation” (PWM). Consequently, the brightness of the light source can be controlled stepwise. The thickness of a finger differs from person to person. As long as an amount of light is fixed, whether a hemal pattern is successively visualized depends on the person. Through the step-wise control of the amount of light, a finger may be imaged continuously until the hemal pattern is successfully visualized. This leads to improved precision in identification. In addition, if a sensor for measuring the thickness of a finger is included is in the apparatus, the relationship between the thickness of a finger and an optimal amount of light is calculated in advance and stored. Thus, an optimal hemal pattern can be visualized by picking up the least number of images.
[0048] FIG. 9 is a flowchart describing light level control dependent upon the thickness of a finger. During processing 900 , the entire hardware is initialized, and initial values are assigned to temporal variables needed to run the program. When hardware initialization is completed the program becomes idle and waits until the switch 108 is turned on (step 902 ). When the switch is turned on, a sensor or the like is used to measure the thickness of a finger. A look-up table in which a set of the thickness values and initial light level values is recorded in advance is preferably used to determine an initial amount of light that is to emanate from the light source 106 . Thereafter, a finger is imaged using the camera 114 , and the image data is stored in the memory 210 (step 906 ). The stored image data is subjected to feature extraction 908 that extracts the features of a hemal pattern, and a determination is made as to whether a hemal pattern was correctly visualized (step 912 ).
[0049] If a hemal pattern is not visualized, the amount of light is changed (step 910 ), and image data is fetched from the camera again. As for the direction in which the amount of light is changed (e.g., up or down), when an image of a finger is too bright, it signifies that the amount of light is so large as to cause saturation. The amount of light is therefore reduced. In contrast, when the image of a finger is too dark, it signifies that the amount of light is presumably so small as to lower a signal-to-noise ratio relative to transmissive light. The amount of light is therefore increased. The brightness of a finger image is preferably calculated using an average of pixel values.
[0050] Thereafter, a registered pattern to which the visualized hemal pattern corresponds is searched for, that is, the visualized hemal pattern is collated with the registered patterns (step 914 ). If the visualized hemal pattern corresponds to any registered pattern (step 916 ), a signal indicating that a correct access authority is identified or identification data concerning an identified individual is transmitted to a control target, that is, equipment or a software program that requires identification (step 918 ). A standby state is then established again and retained until the switch is activated.
[0051] FIG. 10A and FIG. 10B illustrate an exemplary method for measuring the thickness of a finger without using a sensor. FIG. 10A shows a plane that contains a light source 106 and that is imaged by a camera opposed to the light source. A light source 106 is located in the center of the plane and enclosed with a coating 1000 of a dye that suppresses reflection of near-infrared light or absorbs near-infrared light. Bar-shaped markings 1002 made of a material that efficiently reflects near-infrared light are formed on the coating 1000 . When the light source glows, the contrast between the coating 1000 and the markings 1002 becomes distinct. When the plane containing the light source is imaged using the camera, the difference in luminance between the coating 1000 and the markings 1002 is intensified.
[0052] When a finger 200 is placed in front of the light source as shown in FIG. 10B , an area behind which the markings are hidden by the finger varies depending on the thickness of the finger. The difference in luminance between a portion of an image of a finger depicting a blood vessel and another portion thereof depicting no blood vessel is not intensified to a large degree. When a finger hides part of the markings 1002 , the difference in luminance of the part of the markings from the coating is nullified. Coordinates indicating each point at which the intense difference in luminance terminates delineate the finger. This is achieved through very simple difference processing.
[0053] In order to measure the thickness of a finger, at least two markings are preferably needed. Since a finger has joints, the thickness thereof is uneven. Therefore, when four markings are used as illustrated, the thickness of a finger can be determined more accurately. Moreover, when the four markings are used, even if a finger is inserted while being slightly inclined, the inclination can be detected.
[0054] FIG. 4 is an enlarged view of a structure into which a finger is inserted that is included in an identification apparatus according to an embodiment of the invention. A near-infrared light source 106 is located in the upper part of the structure, and an optical opening 110 is formed in the lower part thereof. A camera 114 is located below the opening. A touch portion 400 of a button switch is pressed with a finger. When the touch portion 400 is pressed while being touched directly with a finger, a contact switch 108 is turned on. The contact switch 108 is preferably realized with a pushbutton with a spring. When the contact switch 108 is pressed, the contact switch conducts. When the contact switch 108 is released, the spring automatically returns the switch to the initial position, isolating the contacts. When the opening 110 and button 400 are arched as illustrated so that a finger will be bent naturally, a finger is bent without fail. Consequently, the probability that part of a hemal pattern is missing because the digital blood vessels are compressed is greatly reduced. Moreover, when a glass plate covering the opening 110 is located at a lower position or a finger rest 402 is formed, the root of the finger floats relative to the opening 110 . Consequently, compression of the blood vessels occurring when a finger comes into contact with the opening 110 can be more effectively prevented.
[0055] FIG. 13 is an enlarged view showing a lateral side of another embodiment of the present invention having a structure in which a finger is inserted. Compared with the structure shown in FIG. 4 , the position of a button switch 1301 is different from the position of the button switch 400 . Unlike the button switch 400 shown in FIG. 4 , the contact switch 108 of the button switch 1301 is pressed with a forward thrust of a finger. Compared with the press of the button switch 400 shown in FIG. 4 , the press of the button switch 1301 results from an unnatural movement of a finger. When the button switch 1301 is realized with a switch means that is not clicked on or off, such as, a touch sensor, a user can maneuver the button switch with a good sense of touch.
[0056] FIG. 5 is an enlarged view of an exemplary button 400 . The button 400 has a concave part 500 formed in a side thereof to contact a finger so that the fingertip will fit within the concave part. Consequently, every time a finger is inserted, the fingertip is relocated at the same position with higher accuracy. A positional deviation caused by a press of the button 400 will not occur. As also shown in FIG. 4 , the height of the button 400 is preferably limited to a value permitting only the ventral part of a fingertip to lie on the button. A space is created above the button 400 so that the button can be pressed with a finger having a long nail or having a false nail attached thereto.
[0057] FIG. 6 is an enlarged view showing an exemplary finger rest 402 formed to bear the root of a finger. The finger rest 402 may be a simple plate-like projection. The simple plate-like projection is preferably machined to have one side thereof dented like a semicircular recess so that the depth of the semicircular recess will be a bit larger than the thickness of a finger. Consequently, a sideways displacement of a finger can be naturally prevented. In this case, the finger rest 402 is not exactly an independent means but is a variant of the aforesaid guide groove 112 . The finger rest 402 thus fills the role of a guide that directs a user to place his/her finger in an appropriate position.
[0058] FIG. 7 shows an example of another variant of the identification apparatus 100 . In the example shown in FIG. 1 , the light source unit 102 is shaped like a roof in order to intercept illumination light coming from the ceiling or other external source. In the FIG. 1 case, however, since a user is asked to insert his/her finger in a shielded space, the user may feel uneasy. For this reason, as shown in FIG. 7 , the light source may be located obliquely above a finger, and a cover obstructing the user's view of his/her finger is thus excluded. In the illustrated example, a roof-like light source unit is extended obliquely from both sides of an opening. A light source 106 is incorporated in each of the light source units. The two light sources are distributed evenly around the opening. This is because when one light source is included, light transmitted by a finger is polarized to create a light spot. Consequently, a correct hemal pattern may not be visualized.
[0059] FIG. 8 shows an example of another arrangement of optical elements included in the identification apparatus 100 . A light source 800 provides reflective light while a light source 106 provides transmissive light. These two light sources 106 , 800 are turned on or off under the control of a computer 204 . At this time, the on or off states of the light sources may be combined arbitrarily. For example, the reflective light source 800 generates visible light, and a camera 114 images the surface of a finger. In the aforesaid embodiment, an optical filter transmits near-infrared light alone. Instead, an optical filter 802 of a variable or switchable type is included herein. Namely, the operating modes of the optical filter 802 may be switched so that visible light will also be passed if necessary. This makes it possible to visualize the features of a living body including the fingerprint on the surface of a finger. The feature of a living body detectable on the surface of a finger and a hemal pattern may be used in combination for identification. This leads to improved precision in identification.
[0060] The advantages provided by the employment of the button switch in the identification apparatus have been previously described. The action of pressing a button signifies that a user touches the apparatus. It cannot be said that there is no possibility that a user may loathe touching the apparatus from a sanitary viewpoint. This kind of a user's feeling can be alleviated by the adoption of a generally used antibacterial material for the apparatus body or the button. Letters “antibacterial” to be inscribed in the apparatus body will produce a good psychological effect on a user. According to the configuration in which the present invention is implemented, the sensor used to acquire a hemal pattern need not be exposed on the surface of the apparatus body. The surface of the apparatus can therefore be readily processed to be antibacterial. Living-body identification methods according to which a sensor must be brought into direct contact with a living body have difficulty in making the sensor antibacterial. The present invention has overcome the difficulty.
[0061] In the aforesaid embodiment, the button switch is realized with a mechanical pushbutton. Alternatively, for example, electrostatic switches that conduct when touched with a finger may be substituted for the switches 400 and 108 . Additionally, a combination of a light source and an optical sensor may be used so that when a fingertip comes to a predetermined position to thus intercept light, a switch will be turned on. In this case, various types of sensors including a sensor sensitive to presence of a human being can be utilized.
[0062] FIG. 14 shows a finger identification apparatus having a keypad. Even if identification using a finger fails, identification can be retried by entering a password, which is registered in advance, using keypad 140 . Moreover, when identification using a finger and identification using a password may be combined, more reliable identification can be achieved. Furthermore, an action to be performed after identification may be differentiated between identification using a finger and identification using a password.
[0063] According to the present invention, a finger is smoothly led to a specific position, a hemal pattern of the finger is visualized, a visualized pattern in a produced image can be collated with registered patterns on a stable basis without the necessity of alignment or correction that is required due to turning of a finger. Moreover, the probability that part of a hemal pattern is missing because a finger is compressed will be reduced. This leads to improved precision in identification.
[0064] Nothing in the above description is meant to limit the present invention to any specific materials, geometry, or orientation of parts. Many part/orientation substitutions are contemplated within the scope of the present invention. The embodiments described herein were presented by way of example only and should not be used to limit the scope of the invention.
[0065] Although the invention has been described in terms of particular embodiments in an application, one of ordinary skill in the art, in light of the teachings herein, can generate additional embodiments and modifications without departing from the spirit of, or exceeding the scope of, the claimed invention. Accordingly, it is understood that the drawings and the descriptions herein are proffered by way of example only to facilitate comprehension of the invention and should not be construed to limit the scope thereof. | An identification apparatus that keeps the conditions for imaging uniform among successive identifications and requires a user to perform only a series of simple maneuvers. An identification apparatus comprising a guide member, a light source, and an imaging unit. The guide member includes a pattern or a structure that inspires a user to position his/her finger thereon or to approach his/her specific finger region thereto. A contact member such as a button switch is preferably located at a position in the guide member at which a fingertip is to be positioned. An optical opening is formed at a position coincident with a position at which a portion of a finger to be imaged for identification should be placed. The light source radiates near-infrared light through the portion of the finger to be imaged. The imaging means acquires an image of the finger, and the apparatus compares the image to previously registered images. The apparatus may also include dual light sources power saving functionality, and means for limiting the interference of external light sources. | 6 |
BACKGROUND OF THE INVENTION
1. Field of the Invention
The method relates to a method for removing and drawing a synthetic thread to form a fully drawn yarn (FDY) as well as a device for performing the method.
2. Description of Related Art
For the manufacture of synthetic threads especially for textile applications it is generally known that the multifilament threads are drawn to a lesser or greater extent after the melt spinning process, depending on the yarn types to be manufactured. Depending on the degree of drawing, we distinguish between so-called POY yarns or FDY yarns. POYs (pre-oriented yarns) have a pre-oriented, not yet completely drawn structure and are normally further processed into the finished yarn during a second process step, such as false turn texturizing. In contrast, FDYs (fully drawn yarns) are fully drawn and can be used directly for the subsequent processing of a large-size textile product.
The synthetic threads are drawn by means of driven guide jackets of several galettes, wherein the threads are guided with contact along the circumference of the guide jackets. The guide jackets of the galettes are at least partly heated to heat the threads for drawing or relaxing. Because strong drawing analogously requires high differential speeds between the guide jackets and the galettes on the one hand and the threads are heated by way of contact with the heated guide jackets on the other hand, long contact lengths between the thread and guide jacket are required to heat the threads with high speeds. For this reason, a galette pair is normally used for removing and drawing synthetic threads to form fully drawn yarns, said galettes having two guide jackets driven with identical circumferential speeds and guiding the thread with several loops. Said method and said device have been disclosed for example in DE 199 58 245 A1.
With respect to the disclosed method and the disclosed device, each of the galette pairs comprises two driven guide jackets, on which the thread is guided with a plurality of loops. In this respect the guide jackets of a galette pair interact in order to carry out the thermal treatment on the thread and to pull the thread out of a spinning zone or to draw it in a drawing zone. The number of loops on the guide jackets is selected in such a way according to the ratio of speeds that the desired drawing temperature is reached when the thread has run off of the guide jacket. However, any contact between the thread and a guide surface generally generates friction effects which may result in irregularities of the individual filaments due to the multifilament structure of the thread.
A method and a device for removing and drawing a multifilament thread has been disclosed in DE 31 46 054 A1, in which the thread is guided along the guide jacket of a galette with a single loop for removing the thread. However, the guide jacket is not heated and therefore, the thread is drawn cold in the subsequent zone. However, said cold drawn threads generally have the disadvantage that extremely high drawing forces need to be generated, resulting in considerable problems especially in connection with the manufacture of a plurality of simultaneously guided threads. Another disadvantage of the method is that the consistently slip-free transmission of the drawing forces is extremely difficult with a single loop on the guide jacket of the galette.
However, methods and devices have generally been disclosed in the prior art in which the thread is heated contactless by means of a radiant panel. For example, a method and a device for removing and drawing a multifilament thread are described in WO 2007/115703 A1 in which the thread is guided on the guide jackets of the galettes with a single loop. In the process, free treatment zones used to heat the thread with radiant panels are formed between the guide jackets. Consequently, said methods and devices require longer free guide pathways of the thread to allow adequate temperature equalization with high speeds.
SUMMARY OF VARIOUS EMBODIMENTS
The object of the invention is to create a method and a device for removing and drawing a multifilament thread to form a FDY yarn of the type according to its genre which allows gentle heating of the thread with high removal speeds and relatively short contact lengths between the thread and the guide jackets.
Another object of the invention is to provide a method and a device of the type according to its genre which allows the heat treatment and drawing on the smallest possible installation space.
According to the invention, this object is solved with the various method embodiments described herein as well as with the various embodiments of a device for performing the method described herein.
Preferred upgrades of the invention are defined by the characteristics and combination of characteristics of the various alternate embodiments described herein.
The invention is based on the know-how that the type of thread guidance of synthetic threads affects the heating of the thread for textile applications with fine titers. In the prior art, the threads are generally looped multiple times in the same looping direction around galette pairs with two driven and heated guide jackets. As a result of said type of thread guidance, the multifilament thread has an inner side and an outer side and the filament strands arranged on the inner side of the thread are recurrently guided past the heated surface of the guide jackets of the galette pair. As a result, the filament strands of the thread arranged on the outer side are exclusively heated by way of heat transport within the filament bundle. However, as a result of this effect, the heat treatment of the individual filaments within the filament bundle of the thread is uneven, thus causing irregularities for example in connection with the staining during a subsequent process.
The invention has the particular advantage that the thread on the guide jackets of the galette pair is heated uniformly from both sides. For this purpose, the thread is guided in an S-shaped or Z-shaped thread course through a first galette pair having two guide jackets driven in opposite directions during the removal from a spinning zone and before the drawing. This achieves a high uniformity for heating the filaments of the thread on the one hand and allows the realization of a relatively short contact length with high speeds of the guide jackets on the other hand. In particular, this makes it possible to essentially homogenize the history of the thread filaments. The filament strands arranged both on the inner side as well as on the outer side of the thread come into contact with the heated surface of one of the guide jackets.
For this purpose, the device for performing the method according to the invention comprises a galette pair, in which the drives of the guide jackets are formed with two electric motors with a different sense of rotation and which are driving the guide jackets with identical circumferential speeds. Thus, the guide jackets can optimally interact with each other in order to remove the thread or a plurality of threads guided parallel side by side from a spinning zone.
The upgrade of the method in which the thread is guided through a second galette pair in an S-shaped or Z-shaped thread course with guide jackets driven in opposite directions after the drawing, whereby the thread is drawn in a drawing zone formed between the galette pairs, is particularly suitable for the thermal after-treatment of the thread to achieve a relaxation. In spite of the high circumferential speeds of the guide jackets of the second galette pair due to the drawing, a uniform heating of the thread can be achieved with a relatively short contact length. Again the thread from an inner side and an outer side alternately comes into contact with the heated surface of the guide jackets. This results in a particularly even treatment of all filament strands within the thread and rapidly achieves the thermodynamic end status of the thread.
In order to obtain a high loop-related friction for establishing high drawing forces with a single looping of the guide jackets aside from an adequate contact length for heating up the thread, the upgrade of the invention is particularly advantageous in which the thread is guided past the guide jackets of the galette pair with a single partial loop with a looping angle of at least 180o. With common galette diameters with a range of for example 150 to 250 mm, this allows the safe drawing of all common titer ranges of FDY yarns, irrespective of the polymer material.
In order to draw one or a plurality of threads simultaneously to form an FDY yarn, the heat is matched to the respective thread material, so as to reach the range of uniformly flowing drawing depending on the polymer type, so that a uniform molecular structure can be created during the drawing process.
In order to achieve adequate heat with alternating contact of the thread with the heated surfaces of the guide jackets irrespective of the number of filaments combined to form the thread and irrespective of the filament titers, the upgrade of the invention is preferably used in which the two guide jackets of the first galette pair are heated to the same surface temperature or the respective different surface temperatures for heating the thread before the drawing.
This effect is provided in particular also for the thermal after-treatment following the drawing of the thread, so that according to an upgrade of the invention the two guide jackets of the second galette pair are heated to the same surface temperature or to different surface temperatures for heating the thread after the drawing procedure.
For performing the method variant, the device according to the invention preferably has a separate heating system for every guide jacket, which can be controlled independently from each other by means of a plurality of control devices provided for setting a surface temperature on the respective guide jacket.
However, it is generally also possible to heat one of the guide jackets, preferably the guide jacket of the galette pair downstream of the thread course passively, for example by means of the thermostated ambient air present within the galette box.
Furthermore, the separate heating of the guide jackets for generating different surface temperatures is particularly advantageous to obtain a uniform heating of all filaments on one galette pair with different contact lengths between thread and guide jacket and with identical guide speeds of the two guide jackets.
This also makes it possible to use guide jackets with different diameters for alternately heating the inner side and the outer side of the thread. For example, the surface temperature of the guide jacket with a smaller exterior diameter would be set higher. The differences in diameter of the guide jackets of one of the galette pairs can at the same time be used to set a speed difference. In particular, this triggers a shrinkage process in the filaments of the thread in connection with the after-treatment of the thread after the drawing, which is formed in particular in the last galette pair between the guide jackets.
However, for performing the method the device variant is preferably selected in which the guide jackets of one of the galette pairs have an identical outer diameter for the formation of identical contact lengths between thread and guide jacket with the same size partial loop. However, the contact lengths can also be varied with different partial loops on the guide jackets.
In order to heat the thread material with surface temperatures of the guide jackets that are as low as possible and hence with as little energy as possible, the method variant is particularly advantageous in which the thread is removed in dry status or in a wet status with a low water content of <20%, preferably <10%. Consequently, the thermal energy provided on the surface of the guide jacket is utilized directly to heat the thread material. This helps completely prevent or minimize foreign components on a thread, so that no energy is wasted to heat said foreign components of a thread.
The uniformity of the filaments respective to the thread length can be optimized with the method variant in which the filaments of the thread are guided into a ribbon-shaped arrangement before a first contact with the guide media. Thus, all filaments combined in one thread can come into contact with the guide jackets of the galette pair so that each of the filaments essentially has the same history with respect to the heating of the surface contact.
For performing this method variant, the device according to the invention comprises a guide medium upstream of the thread course of the first galette pair and through which the filaments of the thread can be transferred into a ribbon-shaped arrangement.
In order to be able to set the drawing ratios common for FDY yarns flexibly, the method variant is provided in which the thread is guided along the circumference of the guide jackets of the first galette pair with a circumferential speed of the guide jackets in the range of 1,200 m/min to 3,500 m/min and along the circumference of the guide jackets of the second galette pair with a circumferential speed of the guide jackets in the range of 3,500 m/min to 6,000 m/min. Thus, all common polymer types with different thread titers can be made into an FDY yarn. Especially with thicker thread titers, the method according to the invention can be improved by additionally heating the thread contactless by means of infrared irradiation. Said additional heating can be performed both before drawing as well as after drawing the thread, wherein preferably free thread lines are used for this purpose.
BRIEF DESCRIPTION OF THE SEVERAL VIEWS OF THE DRAWINGS
The method according to the invention as well as the device according to the invention for performing the method are explained in detail below by means of an exemplary embodiment with reference to the enclosed figures.
In the figures:
FIG. 1 shows a schematic representation of a galette arrangement of a first exemplary embodiment of the device according to the invention for performing the method according to the invention
FIG. 2 shows a schematic cross-section of a galette pair pursuant to the exemplary embodiment according to FIG. 1
FIG. 3 shows an additional galette arrangement of another exemplary embodiment of the device according to the invention
FIG. 4 shows a schematic representation of the spinning system with an exemplary embodiment of the device according to the invention.
DETAILED DESCRIPTION
FIG. 1 shows a galette arrangement of a first exemplary embodiment of the device according to the invention for performing the method according to the invention.
The exemplary embodiment is formed with two galette pairs 1 . 1 and 1 . 2 , which are arranged side by side. The first galette pair 1 . 1 . has two guide jackets 2 . 1 and 2 . 2 driven at the same circumferential speed. The guide jackets 2 . 1 and 2 . 2 of the galette pair 1 . 1 are arranged on top of each other and are each driven by a separate electric motor 3 . 1 and 4 . 1 . The electric motor 3 . 1 of the guide jacket 2 . 1 is designed with left-hand rotation and drives the guide jacket 2 . 1 in a counter clockwise direction. The electric motor 4 . 1 is designed with right-hand rotation and drives the guide jacket 2 . 2 in a clockwise direction. Consequently, the guide jackets 2 . 1 and 2 . 2 are turning in opposite directions. The electric motors 3 . 1 and 4 . 1 are preferably driven by a common motor control device. Each of the guide jackets 2 . 1 and 2 . 2 comprises a heating system not illustrated here, provided to heat the guide jackets 2 . 1 and 2 . 2 . Thus, the guide jacket 2 . 1 is heated to a surface temperature T 1 and the guide jacket 2 . 2 to a surface temperature T 2 .
In this case, the second galette pair 1 . 2 is designed identically to the first galette pair 1 . 1 . This means that the guide jackets 2 . 3 and 2 . 4 are driven by the electric motors 3 . 2 and 4 . 2 , wherein a speed difference for the shrinkage treatment can be set between the guide jackets 2 . 3 and 2 . 4 . The electric motor 3 . 2 is designed with left-hand rotation and drives the guide jacket 2 . 3 in a counterclockwise direction. The electric motor 4 . 2 is designed with right-hand rotation and drives the guide jacket 2 . 4 in a clockwise direction. Again, both guide jackets 2 . 3 and 2 . 4 of the galette pair 1 . 2 are driven in opposite directions, wherein the electric motors 3 . 2 and 4 . 2 are preferably driven by a motor control device. Furthermore, a separate heating system (not illustrated here) is assigned to each guide jacket 2 . 3 and 2 . 4 , so that the guide jackets 2 . 3 and 2 . 4 can be heated with different temperatures. As a result, the guide jacket 2 . 3 has a surface temperature T 3 and the guide jacket 2 . 4 a surface temperature T 4 .
In order to remove a multifilament thread from a spinning device and to draw it to form an FDY yarn, a thread 5 is first removed from the guide jacket 2 . 1 of the galette pair 1 . 1 and guided in an S-shaped thread course around the guide jacket 2 . 1 and the adjacent guide jacket 2 . 2 . In the process, the thread 5 is first brought into contact with one inner side on the guide jacket 2 . 1 with a single loop and then brought into contact with its outer side on the surface of the guide jacket 2 . 2 by changing the loop direction. This way, the filaments on the inner side and outer side of the thread 5 can alternately be brought into direct contact with the heated surface of the guide jackets 2 . 1 and 2 . 2 .
In this exemplary embodiment the guide jackets 2 . 1 and 2 . 2 are designed with an outer diameter of identical size, wherein the arrangement of the galette pairs 1 . 1 and 1 . 2 is selected in such a way that the looping angle of the thread 5 on the guide jackets 2 . 1 and 2 . 2 each exceeds a value of 180o. In FIG. 1 , the loop angle is labeled with the letter a. It is basically possible to form different loop angles, depending on the galette arrangement on the guide jackets 2 . 1 and 2 . 2 . Furthermore, a Z-shaped looping of the guide jackets 2 . 1 and 2 . 2 would be possible with the mirror-inverted feed of the thread.
In order to heat the thread material to a temperature within the range of the gas conversion temperature or also above the gas conversion temperature, the guide jackets 2 . 1 and 2 . 2 are heated with identical surface temperatures in this exemplary embodiment. As a result, the surface temperature T 1 of the guide jacket 2 . 1 is identical to the surface temperature T 2 of the guide jacket 2 . 2 and could be within the range of 60° C. to 200° C.
However, it is also possible to set different surface temperatures T 1 and T 2 on the guide jackets 2 . 1 . and 2 . 2 . This is necessary in particular in cases where the single looping of the thread 5 on the guide jackets 2 . 1 and 2 . 2 results in different contact lengths, for example because of different diameters of the guide jackets or due to different loop angles on the guide jackets.
The second galette pair 1 . 2 is arranged next to the first galette pair 1 . 1 wherein the thread 5 is directly guided to the lower guide jacket 2 . 3 of the galette pair 1 . 2 after coming off the guide jacket 2 . 2 . As a result, a drawing zone is formed between the guide jackets 2 . 2 of the first galette pair 1 . 1 and the guide jacket 2 . 3 of the second galette pair 1 . 2 , in which the multifilament thread 5 is drawn. For this purpose, the guide jackets 2 . 3 and 2 . 4 of the second galette pair 1 . 2 are driven with a higher circumferential speed than the guide jackets 2 . 1 and 2 . 2 of the first galette pair 1 . 1 . The thread 5 is guided around the guide jackets 2 . 3 and 2 . 4 of the second galette pair with an S-shaped loop, so that the thread 5 can be guided with a single loop inside the galette arrangement. This allows the realization of extremely compact and short guide jackets within the galette pair 1 . 1 and 1 . 2 .
The galette pair 1 . 2 is essentially designed identical to galette pair 1 . 1 , and therefore, the outer diameters of the guide jackets 2 . 3 and 2 . 4 are identical. However, it is also possible to obtain a speed difference on the galette pair 1 . 2 desired for the after-treatment of the thread where the rotational speed is the same and the outer diameters of the guide jackets 2 . 3 and 2 . 4 are different. Irrespective of the size of the outer diameter, a loop angle a is formed on each of the guide jackets 2 . 3 and 2 . 4 , which normally exceeds the value of 180o. In order to introduce a thermal after-treatment of the drawn thread directly inside the second galette pair 1 . 2 , the guide jackets 2 . 3 and 2 . 4 are heated to a surface temperature in the range of 80 to 200o C. In this exemplary embodiment, the surface temperatures T 3 of the guide jacket 2 . 3 and the surface temperature T 4 of the guide jacket 2 . 4 are set to identical values. However, it is basically again possible to create different surface temperatures on the guide jackets 2 . 3 and 2 . 4 , in order to equalize for example the contact lengths between the thread and the guide jackets. Normally, the surface temperatures of the guide jackets 2 . 3 and 2 . 4 are set higher than the surface temperatures of the guide jackets 2 . 1 and 2 . 2 . This is due to the fact that different temperatures are required to initiate certain thread-specific processes and that the circumferential speeds of the guide jackets 2 . 3 and 2 . 4 are naturally considerably higher than the guide speeds of the guide jackets 2 . 1 and 2 . 2 and therefore realize different direct contact times. The galette pair 1 . 1 is preferably driven with a guide speed in the range of 1,200 in/min to 3,500 in/min. The second galette pair 1 . 2 is driven with a guide speed ranging between 3,500 and 6,000 in/min.
FIG. 2 . illustrates a schematic cross section of a galette pair, such as it could be used for instance as galette pair 1 . 1 or as galette pair 1 . 2 in the exemplary embodiment according to FIG. 1 . In this case, galette pair 1 . 1 is illustrated. The galette pair 1 . 1 is fastened on a machine rack 6 . For this purpose, two galette retainers 11 . 1 and 11 . 2 are arranged at a distance from each other on the machine rack 6 on which the guide jackets 2 . 1 and 2 . 2 are pivotably retained. The design of the guide jackets 2 . 1 and 2 . 2 is identical and therefore, only guide jacket 2 . 1 is illustrated as a cross-sectional representation in FIG. 2 . The guide jacket 2 . 1 is connected with a drive shaft 8 which is driven by the electric motor 3 . 1 . The guide jacket 2 . 1 is designed as a hollow cylinder and its jacket is put over a heating system 7 . 1 . The heating system 7 . 1 which can be formed for instance with an induction coil, is retained on a heating retainer 10 and electrically connected with an external control device 9 . 1 . The control device 9 . 1 is used to set a desired surface temperature on the guide jacket 2 . 1 . The sensors intended to control and monitor the surface temperature are not illustrated in this exemplary embodiment.
Consequently, the galette pair 1 . 1 comprises control devices 9 . 1 and 9 . 2 used for the independent control and regulation of the connected heating systems 7 . 1 and 7 . 2 of the assigned guide jackets 2 . 1 and 2 . 2 .
In order to drive the guide jackets 2 . 1 and 2 . 2 , the electric motor 3 . 1 with left-hand rotation and the electric motor 4 . 1 with right-hand rotation are operated jointly by means of a motor control device 35 with identical rotational speeds. If the outer diameters of the guide jackets 2 . 1 and 2 . 2 are identical, the latter are driven with identical circumferential speeds. For this purpose, the electric motors 3 . 1 and 4 . 1 of the galette pair 1 . 1 are connected with the motor control device 35 .
We would like to point out that the structural design of the galette pair according to FIG. 2 is exemplary. Other structural principles can generally also be used to drive and heat a guide jacket. For example, passive heating of at least one of the guide jackets by way of thermal convection and external heat irradiation is also possible. The galette pairs are normally arranged inside a galette box to prevent in particular the loss of heat. The thermal energy built up within the galette box due to an actively heated guide jacket could be used to heat the neighboring not actively heated guide jacket. Furthermore, it is also possible to arrange additional heat sources within the galette box, such as for instance an infrared radiator used to heat a thread or the thread on the surface of the guide jacket directly.
In addition, simulation calculations revealed that the surface temperatures of the guide jackets of a galette pair must be selected depending on the free thread distance between the guide jackets. The introduced thermal energy which is additionally influenced by the surroundings is equalized within the filament bundle. Long thread distances between the guide jackets result in a better distribution of the thermal energy in the multifilament thread and so the surface temperature on the subsequent guide jacket of the galette pair can be kept below the surface temperature of the first guide jacket. The method according to the invention and the device according to the invention can also be operated in a variant in which one of the guide jackets of the galette pair is kept mobile in order to change the free thread distance between the guide jackets. Aside from the length of the free thread distance, it is also possible to influence the loop degree and hence the contact lengths between the thread and the guide jacket with the mobility of the guide jacket. Therefore, the invention offers a number of many flexible uses in order to create an FDY yarn.
Another exemplary embodiment of a galette arrangement is illustrated in FIG. 3 , used to perform the method according to the invention. In this exemplary embodiment the galette pairs 1 . 1 and 1 . 2 are arranged underneath each other. The design of the galette pairs 1 . 1 and 1 . 2 is identical to the exemplary embodiment according to FIG. 1 . Therefore, we are referring to the description above and only explain the differences below.
To remove the multifilament thread from a spinning device, a guide medium 12 is arranged in front of the thread course in the first galette pair 1 . 1 . In this exemplary embodiment, the guide medium 12 is formed with two return pulleys 13 . 1 and 13 . 2 mounted freely pivotable. The thread 5 is guided along the return pulleys 13 . 1 and 13 . 2 .with one partial loop each, whereby the filaments of the thread 5 create a ribbon-shaped arrangement. Insofar, the thread 5 is guided to the guide jacket 2 . 1 of the first galette pair 1 . 1 with a ribbon-shaped filament arrangement. The thread 5 is looped around the guide jackets 2 . 1 and 2 . 2 of the first galette pair 1 . 1 in an S-shape with identical circumferential speed and driven in opposite directions. The ribbon-shaped filament alignment achieves a high homogenization for the heating and guidance of the thread. It also continues after the thread 5 has been drawn in the drawing zone and results in a homogeneous after-treatment on the guide jackets 2 . 3 and 2 . 4 of the second galette pair 1 . 2 . The arrangement of the galette pairs 1 . 1 and 1 . 2 among each other creates an extended drawing zone, which runs in between the guide jackets 2 . 2 and 2 . 3 . In this arrangement, the thread is looped around the guide jackets 2 . 3 and 2 . 4 of the second galette pair 1 . 2 in a Z-shape. For this purpose, the guide jacket 2 . 3 is driven in a clockwise direction by an electric motor with right-hand rotation (not illustrated here). The second guide jacket of the second galette pair 1 . 2 is therefore driven in a counterclockwise direction by an electric motor with left-hand rotation with identical circumferential speed.
Here we would like to emphasize explicitly that the design of the galette pairs 1 . 1 and 1 . 2 in the exemplary embodiment according to FIG. 1 and FIG. 3 is exemplary. The guide jackets 2 . 1 to 2 . 4 can basically also be designed with different sizes. Furthermore, it is also possible to design the second galette pair 1 . 2 with guide jackets 2 . 3 and 2 . 4 driven in the same direction. Alternatively, the guide jackets could also be assigned and driven in such a way that the thread is looped around both galette pairs in a Z-shape.
FIG. 4 shows an exemplary embodiment of the device according to the invention for performing the method according to the invention within a spinning system.
A heated spinning beam 14 is provided for melt spinning of preferably a plurality of multifilament threads, having a plurality of spinning nozzles 15 on its underside. The spinning beam 14 is aligned diagonally to the drawing plane, so that only one of the spinning nozzles 15 is visible in FIG. 4 . Each of the spinning nozzles 15 has a multitude of nozzle openings on its underside, through which a polymer melt is extruded to form filaments 17 for example from a polyester or a polyamide. The spinning nozzles 15 are connected with a molten material inlet 16 . The molten material inlet 16 is coupled to a molten material source not illustrated here, for example an extruder. Other molten material-carrying and molten material-transporting components can be arranged within the spinning beam 14 , which are not discussed in more detail here.
A cooling system 18 is provided underneath the spinning beam 14 , consisting of a cooling shaft 20 and an airflow device 19 . The cooling shaft 20 is arranged underneath the spinning nozzles 15 in such a way that the plurality of filaments 17 extruded through the spinning nozzles 15 pass through the cooling shaft 18 . A cool air flow can be generated by means of the airflow device 18 , which is directed into the cooling shaft 20 so that the filaments 17 extruded through the spinning nozzles 15 are cooled off uniformly. A shared thread guide 21 is provided underneath the cooling shaft 20 to combine the filaments 17 to a thread 5 . For this purpose, the shared thread guide 21 is arranged in the center underneath the spinning nozzles 14 so that the filaments 17 are uniformly brought together in the shared thread guide 21 .
The device according to the invention for drawing the threads is arranged underneath a fall shaft 34 adjacent to the cooling shaft 20 . For this purpose, the threads 5 are first brought to a treatment distance from each other through the intake thread guide 22 , so that the threads 5 are guided parallel side by side with a short distance ranging from 3 to 8 mm above the guide jackets 2 . 1 to 2 . 4 of the galette pairs 1 . 1 and 1 . 2 . The design of the galette pairs 1 . 1 and 1 . 2 arranged underneath the fall shaft 34 is identical to the exemplary embodiment according to FIG. 1 mentioned above and therefore, no further explanation is provided here.
We would only like to mention that the electric motors of the galette pairs 1 . 1 and 1 . 2 are controlled with two separate motor control devices, allowing the setting of a different speed between the first galette pair 1 . 1 and the second galette pair 1 . 2 for drawing the threads. However, the guide jackets 2 . 3 and 2 . 4 of the second galette pair 1 . 2 may have different exterior diameters in order to obtain a minor speed difference for a shrinkage treatment with identical rotational speeds.
A guide medium 12 in the form of a thread brake is arranged in the thread course in front of the first galette pair 1 . 1 through which the filaments 17 of a thread 5 can be spread to form a ribbon.
A preparation system 23 and a swirling system 24 are arranged between several individual galettes 25 . 1 , 25 . 2 and 25 . 3 underneath the galette pairs 1 . 1 and 1 . 2 . Filament cohesion is created on the threads 5 by means of preparation and swirling before they are wound up.
A winding device 26 is provided for winding up the drawn threads, which comprises a pivotable spindle rest 30 having two projecting winding spindles 29 . 1 and 29 . 2 . The spindle rest 30 is retained in a rack 31 . In the process, the winding spindles 29 . 1 and 29 . 2 can alternately be guided into an operating area for winding a spool and into an exchange area for exchanging the spools. An exchange device 27 and a pressure roller 28 are provided in the rack 31 , for winding the threads 5 to one spool 33 each. A return pulley 32 is assigned to each winding spot above the exchange device 27 , through which the inlet of the threads 5 is guided through the winding spots.
In the exemplary embodiment of the spinning machine illustrated in FIG. 4 , the freshly extruded thread 5 is guided directly to the galette pairs 1 . 1 and 1 . 2 after the melt spinning process with the filaments 17 in dry condition and drawn to form an FDY yarn.
However, alternatively it is also possible to moisturize the thread 5 with a preparation agent prior to the drawing process when the filaments are gathered, said preparation agent being as dry as possible. It has been determined, that especially the water content in the preparation agent requires more energy to heat the thread to a gas conversion temperature. Insofar, preparation agents have proven suitable which have a water content of less than 20%, preferably less than 10%.
However, it is also possible to add the quantity of preparation agent to the thread with several partial preparation applications. For example, a first part of the preparation could be added to the thread directly after the spinning and before the drawing process. A very tiny quantity of preparation agent would be used to improve the gliding properties of the thread on thread guides and the guide jackets. The moistening required for the after-treatment of the thread could then be added after the drawing and before the winding process with a second part of the preparation. | The invention relates to a method and a device for removing and drawing a synthetic thread to form a fully drawn yarn. The thread is formed by joining a plurality of extruded filaments and is guided by contact on the circumference of heated guide jackets of several driven galette pairs. In order to obtain a gentle and highly homogenized treatment of the filaments, the thread is guided in an S-shaped or Z-shaped thread course by a first galette pair having two guide jackets driven in opposite directions during the removal from a spinning zone and before the drawing. Thus, both sides of the thread can be brought directly into circumferential contact with the guide jackets for in order to heat the thread. | 3 |
CROSS REFERENCE TO RELATED APPLICATIONS
This application is a National Phase filing under 35 U.S.C. § 371 of PCT/SG2009/000474 filed on Dec. 9, 2009; and this application claims priority to U.S. Provisional Application No. 61/121,676 filed on Dec. 11, 2008 under 35 U.S.C. § 119; the entire contents of all are hereby incorporated by reference.
FIELD
The present invention relates to the maleate salt of 11-(2-pyrrolidin-1-yl-ethoxy)-14,19-dioxa-5,7,26-triaza-tetracyclo[19.3.1.1(2,6).1(8,12)]heptacosa-1(25),2(26),3,5,8,10,12(27),16,21,23-decaene. In addition the present invention relates to pharmaceutical compositions containing the maleate salt and methods of use of the salt in the treatment of certain medical conditions.
BACKGROUND
The compound II-(2-pyrrolidin-1-yl-ethoxy)-14,19-dioxa-5,7,26-triaza-tetracyclo[19.3.1.1(2,6).1(8,12)]heptacosa-1(25),2(26),3,5,8,10,12(27),16,21,23-decaene (Compound I) was first described in PCT/SG2006/000352 and shows significant promise as a pharmaceutically active agent for the treatment of a number of medical conditions and clinical development of this compound is underway based on the activity profiles demonstrated by the compound.
In the development of a drug suitable for mass production and ultimately commercial use acceptable levels of drug activity against the target of interest is only one of the important variables that must be considered. For example, in the formulation of pharmaceutical compositions it is imperative that the pharmaceutically active substance be in a form that can be reliably reproduced in a commercial manufacturing process and which is robust enough to withstand the conditions to which the pharmaceutically active substance is exposed.
In a manufacturing sense it is important that during commercial manufacture the manufacturing process of the pharmaceutically active substance be such that the same material is reproduced when the same manufacturing conditions are used. In addition it is desirable that the pharmaceutically active substance exists in a solid form where minor changes to the manufacturing conditions do not lead to major changes in the solid form of the pharmaceutically active substance produced. For example it is important that the manufacturing process produce material having the same crystalline properties on a reliable basis and also produce material having the same level of hydration.
In addition it is important that the pharmaceutically active substance be stable both to degradation, hygroscopicity and subsequent changes to its solid form. This is important to facilitate the incorporation of the pharmaceutically active substance into pharmaceutical formulations. If the pharmaceutically active substance is hygroscopic (“sticky”) in the sense that it absorbs water (either slowly or over time) it is almost impossible to reliably formulate the pharmaceutically active substance into a drug as the amount of substance to be added to provide the same dosage will vary greatly depending upon the degree of hydration. Furthermore variations in hydration or solid form (“polymorphism”) can lead to changes in physico-chemical properties, such as solubility or dissolution rate, which can in turn lead to inconsistent oral absorption in a patient.
Accordingly, chemical stability, solid state stability, and “shelf life” of the pharmaceutically active substance are very important factors. In an ideal situation the pharmaceutically active substance and any compositions containing it, should be capable of being effectively stored over appreciable periods of time, without exhibiting a significant change in the physico-chemical characteristics of the active substance such as its activity, moisture content, solubility characteristics, solid form and the like.
In relation to 11-(2-pyrrolidin-1-yl-ethoxy)-14,19-dioxa-5,7,26-triaza-tetracyclo[19.3.1.1(2,6).1(8,12)]heptacosa-1(25),2(26),3,5,8,10,12(27),16,21,23-decaene initial studies were carried out on the hydrochloride salt and indicated that polymorphism was prevalent with the compound being found to adopt more than one crystalline form depending upon the manufacturing conditions. In addition it was observed that the moisture content and ratio of the polymorphs varied from batch to batch even when the manufacturing conditions remained constant. These batch-to-batch inconsistencies and the exhibited hygroscopicity made the hydrochloride salt less desirable from a commercial viewpoint.
Accordingly it would be desirable to develop one or more salts of 11-(2-pyrrolidin-1-yl-ethoxy)-14,19-dioxa-5,7,26-triaza-tetracyclo[19.3.1.1(2,6).1(8,12)]heptacosa-1(25),2(26),3,5,8,10,12(27),16,21,23-decaene which overcome or ameliorate one or more of the above identified problems.
SUMMARY
The present invention provides a maleate salt (maleic acid salt) of 11-(2-pyrrolidin-1-yl-ethoxy)-14,19-dioxa-5,7,26-triaza-tetracyclo[19.3.1.1(2,6).1(8,12)]heptacosa-1(25),2(26),3,5,8,10,12(27),16,21,23-decaene.
In some embodiments the salt is crystalline. In some embodiments the salt is the 1:1 maleate salt.
In some embodiments the salt shows on X-ray diffraction a peak on the 2theta scale at 17.5°±0.5°.
In some embodiments the salt shows on X-ray diffraction a peak on the 2theta scale at 21.3°±0.5°.
In some embodiments the salt shows on X-ray diffraction at least two peaks on the 2theta scale selected from the group consisting of 8.3°±0.5°, 8.8°±0.5°, 16.9°±0.5°, 17.5°±0.5°, 19.0°±0.5°, 21.3°±0.5°, 23.8°±0.5°, 25.3°±0.5°, 25.8°±0.5° and 26.8°±0.5°.
In some embodiments the salt shows on X-ray diffraction at least 4 peaks on the 2theta scale selected from the group consisting of 8.3°±0.5°, 8.8°±0.5°, 16.9°±0.5°, 17.5°±0.5°, 19.0°±0.5°, 21.3°±0.5°, 23.8°±0.5°, 25.3°±0.5°, 25.8°±0.5° and 26.8°±0.5°.
In some embodiments the salt shows on X-ray diffraction at least 6 peaks on the 2theta scale selected from the group consisting of 8.3°±0.5°, 8.8°±0.5°, 16.9°±0.5°, 17.5°±0.5°, 19.0°±0.5°, 21.3°±0.5°, 23.8°±0.5°, 25.3°±0.5°, 25.8°±0.5° and 26.8°±0.5°.
In some embodiments the salt shows on X-ray diffraction peaks on the 2theta scale at 8.3°±0.5°, 8.8°±0.5°, 16.9°±0.5°, 17.5°±0.5°, 19.0°±0.5°, 21.3°±0.5°, 23.8°±0.5°, 25.3°±0.5°, 25.8°±0.5° and 26.8°±0.5°.
In some embodiments the salt shows on X-ray diffraction at least 1 peak on the 2theta scale selected from the group consisting of 10.6°±0.5°, 13°±0.5°, 14.1°±0.5°, 17.5°±0.5°, 18.3°±0.5°, 20.7°±0.5°, 22.3°±0.5°, 22.7°±0.5°, 23.1°±0.5°, 28.2°±0.5°, 28.5°±0.5°, 29.1°±0.5°, 30.5°±0.5°, 31.3°±0.5°, 35.0°±0.5° and 36.8°±0.5°.
In some embodiments the salt shows on X-ray diffraction peaks on the 2theta scale at 7.0°±0.5°, 9.2°±0.5°, 11.4°±0.5° and 27.5°±0.5°.
The present invention also provides a pharmaceutical composition comprising a salt as described above.
In another embodiment the present invention provides a method of treating or preventing a proliferative disorder comprising administration of a therapeutically effective amount of a salt of the invention to a patient in need thereof. In some embodiments the proliferative disorder is cancer.
In another embodiment the present invention provides the use of a salt of the invention in the treatment of a proliferative disorder. In some embodiments the proliferative disorder is cancer.
In another embodiment the present invention provides the use of a salt of the invention in the manufacture of a medicament for the treatment of a proliferative disorder. In some embodiments the proliferative disorder is cancer.
BRIEF DESCRIPTION OF THE DRAWINGS
Table 1 summarises the solid form results of various batches of hydrochloride salt.
FIG. 1 shows the XRPD Diffractogram of Batch HCl 1: low resolution trace (C2, above) and high resolution trace (D5000, below).
FIG. 2 shows the results of differential scanning calorimetry (DSC) (top) and thermal gravimetric analysis (TGA) (bottom) of Batch HCl 1.
FIG. 3 shows the results of Gravimetric Vapour Sorption (GVS) of Batch HCl 1.
FIG. 4 shows the XRPD Diffractograms of Batch HCl 1 pre- and post-GVS.
FIG. 5 shows the XRPD Diffractogram of Batch HCl 2.
FIG. 6 shows the results of TGA (top) and DSC (bottom) of the Batch HCl 2.
FIG. 7 shows the XRPD Diffractogram of Batch HCl 3.
FIG. 8 shows the results of TGA (top) and DSC (bottom) of the Batch HCl 3.
FIG. 9 shows the XRPD Diffractogram of Batch HCl 4.
FIG. 10 shows the results of DSC (top) and TGA (bottom) of the Batch HCl 4.
FIG. 11 shows the results of GVS of Batch HCl 4.
FIG. 12 shows the XRPD Diffractogram of Batch HCl 5 (2 conditions).
FIG. 13 shows the results of the DSC thermogram of the Batch HCl 5 (prepared from Ethanol).
FIG. 14 shows the XRPD Diffractogram of Batch HCl 6: low resolution trace (C2, above) and high resolution trace (D5000, below).
FIG. 15 shows the results of TGA (top) and DSC (bottom) of the Batch HCl 6.
FIG. 16 shows the results of GVS of Batch HCl 6.
FIG. 17 shows the results of thermal gravimetric analysis (top) and differential scanning calorimetry (bottom) of the maleate salt.
FIG. 18 shows the X-ray diffraction pattern (D5000 high resolution) of the maleate salt.
FIG. 19 shows the variable temperature X-ray diffraction pattern of the maleate salt.
FIG. 20 shows the results of GVS of the maleate salt.
FIG. 21 shows the post-GVS XRPD data for the maleate salt.
FIG. 22 shows the X-ray diffraction pattern of the maleate salt both before and after being kept for a week in the humidity chamber at 60° C. and 96% RH.
DETAILED DESCRIPTION
As stated above it has now been found that certain salts of 11-(2-pyrrolidin-1-yl-ethoxy)-14,19-dioxa-5,7,26-triaza-tetracyclo[19.3.1.1(2,6).1(8,12)]heptacosa 1(25), 2(26),3,5,8,10,12 (27),16,21,23-decaene exist as single robust polymorphs. In particular the present applicants have found that the maleate salt of this compound exists as a single polymorph.
Whilst it is considered that the structure of maleic acid would be clear to a skilled addressee in the art in order to avoid any uncertainty the structure is shown below.
Initial studies into compound I involved analysis of the hydrochloride salt. It was found as summarised in Table 1 below, that the initially prepared hydrochloride salt produces an inconsistent solid form with significant variability in the DSC, TGA, GVS and XRPD pattern (see FIGS. 1 to 16 ).
TABLE 1
Tabulation of Solid form analysis of various Hydrochloride
salts of Compound 1
Batch #
Batch Size
Solid Form Comment (see text)
HCl 1
0.72 kg
Group 1 + 3 + amorphous
HCl 2
0.6 kg
Predominately Group 1
HCl 3
1.6 kg
Group 1 + 3 + little amorphous
HCl 4
79 mg
Group 1
HCl 5
10 mg
Group 2
HCl 6
30 mg
Group 3
As can be seen from the table notwithstanding the same production conditions (batches 1 to 3) being used there was a wide variety of solid forms identified on analysis of the 6 hydrochloride salt batches indicating that with this salt there is a high degree of polymorphism.
The XRPD for the sample of Batch HCl 1 (see table 1) is shown in FIG. 1 . This diffractogram indicates this batch has relatively low levels of crystallinity and an amorphous halo indicating a mixture of phases. The thermal gravimetric analysis (TGA) and differential scanning calorimetry (DSC) for the sample of Batch HCl 1 is shown in FIG. 2 . The TGA shows a two stage weight loss totalling 4.5% up to 100° C. which equates to 1.4 equivalents of water. This corresponds well to the two endotherms seen in the DSC with onsets of 40° C. and 88° C., respectfully. This is most likely to be a loss of water from the sample since no process solvents were observed in the 1 H NMR. There then follows an exothermic event onset 141° C. which is most likely to be a phase change to a new solid form followed by a final endothermic event, probably a melt, onset 238° C. followed by decomposition. These physical changes can be visually seen in a hot-stage microscopy video.
The GVS results for the sample of Batch HCl 1 are shown in FIG. 3 . The sample shows an initial adsorption of water in the initial adsorption cycle of +5.5% at 90% RH. The sample then loses 5% mass on going to dryness and then regains 2% mass on going to 40% RH with a total gain of 2%. This gain of 2% would bring the water content up to 6.5% which corresponds to a dihydrate. The sample appears to be a partially dehydrated hydrate that, once it has been exposed a high enough level of humidity gains water and then permanently holds on to it during the GVS experiment. To determine if there had been a change in the solid form of the material after the GVS experiment a XRPD diffractogram was obtained and is shown in FIG. 4 . The X-ray diffractogram post GVS is similar to that of the starting material, but with more intense peaks. Also some minor peaks in the original diffractogram (ca. 8.5 and 15.5 2theta) have disappeared. It is likely that the material subjected to the GVS experiment contains more than one crystalline phase (form) and that one of the forms changes on exposure to elevated humidity.
The XRPD spectrum of Batch HCl 2 is shown in FIG. 5 and as can be seen there is a low correlation with the XRPD obtained with the HCl 1 batch. The TGA and DSC spectra of Batch HCl 2 are shown in FIG. 6 and have some similarities, but is not identical, to Batch HCl 1. Batch HCl 2 lost 5.6% water in the first phase of the TGA until decomposition at 260° C. This water loss represents 1.67 equivalents of water. The DSC spectrum shows the same 3 thermal events as seen with Batch HCl 1, however the two data sets are clearly not identical.
The XRPD spectrum of Batch HCl 3 is shown in FIG. 7 and did not agree well with either the HCl 1 or HCl 2 batches. The XRPD of Batch HCl 3 was quite complex with many more reflections that other batches and an additional reflection at 2theta of 6.7 not present in other batches. The TGA and DSC spectra of Batch HCl 3 is shown in FIG. 8 . The sample lost 1.5% water in the first phase of the TGA then another loss of 1.97%, possibly solvent, at 165° C. until decomposition at 260° C. This water loss represents 0.5 equivalents of water, lower than the 1.1 equivalents (3.79%) indicated by Karl-Fischer analysis. One possible reason for this is that a higher temperature is required to liberate the water trapped in the structure by means of dehydration, a small expansion of the lattice which will release water trapped or a change in the crystalline structure. The total weight lost in the TGA is 3.4%. The DSC spectrum shows the same 3 thermal events as seen with Batches HCl 1 and 2 but with an additional endothermic event at 200° C., probably a desolvation.
In order to probe the behaviour observed above the HCl salt was recrystallised from refluxing acetonitrile/water to yield 79 mg of a yellow powder, Batch HCl 4. This was analysed by XRPD, TGA and DSC and the data is shown in FIGS. 9 and 10 . This material was shown to be a single, isolable polymorphic form of the HCl salt (henceforth known as ‘Group 1’). As an alternative to recrystallisation, direct formation of the Group 1 material from the free base and aqueous acid may also be accomplished. FIG. 9 which shows the XRPD spectrum of Batch HCl 4 (Group 1) did not agree well with any of the previously described batches. FIG. 10 shows the TGA and DSC spectra of Batch HCl 4 indicating that the sample loses 6.5% of its mass between ambient and 108° C. Two equivalents of water equates to 6.58%. This correlates well with the broad endotherm observed in the DSC (onset=76° C.). The DSC then shows an exothermic phase change (onset=148° C.) then goes on to show a final endotherm onset 222° C.
GVS analysis was carried out and the data is shown in FIG. 11 . The sample showed very little absorption of water gaining only 1.6% mass on going from 40% RH to 90% RH. The sample lost 2.8% mass on going from 90% RH to dryness. The sample was analysed by XRPD post GVS. The form of the sample was unchanged (data not shown).
A second, different, isolable polymorphic form (Batch HCl 5) may be prepared when the HCl salt is synthesised from amorphous HCl salt via a ‘maturation’ process. In this process a small amount of the amorphous salt (10 mg) was treated with 10 or 20 volumes of methanol or ethanol in a vial. The vials were then capped and placed in a maturation chamber that cycled from ambient to 50° C. with four hours spent under each condition. After approximately 18 hours the samples were filtered and analysed. This material was shown to be a single, polymorphic form of the HCl salt different from that of the Group 1 material (henceforth known as ‘Group 2’). FIG. 12 shows the XRPD diffractograms for samples prepared in ethanol (20 vols, top) and methanol (10 vols, bottom). Although there are small differences between samples it is clear that these data are quite different from other batches described herein. FIG. 13 shows the DSC of the sample prepared in ethanol which is clearly much more complex than other batches.
A third, different, isolable polymorphic form, Batch HCl 6, may be prepared when the HCl salt is synthesised from the free base in acetone or in alcoholic solvents with methanolic or aqueous HCl. FIG. 14 shows the XRPD diffractogram, recorded on low and high resolution instruments, and, again, is different from other batches described herein. Strikingly, the DSC and TGA spectra shown in FIG. 15 are very simple with very little weight loss recorded in the TGA until degradation occurs at around 240° C. and likewise no thermal events in the DSC until melting and decomposition. This material was shown to be a single, polymorphic form of the HCl salt different from that of the Group 1 and 2 materials (henceforth known as ‘Group 3’). In the GVS ( FIG. 16 ) the sample showed very little sorption of water gaining only 1.6% mass on going from 40% RH to 90% RH. The sample lost 2.4% mass on going from 90% RH to dryness. The sample was analysed by XRPD post GVS. The form of the sample was unchanged after the experiment (data not shown). Both the GVS experiments from Batches HCl 4 and 6 (Groups 1 and 3) were somewhat similar to each other but different to that of Batch HCl 1, further highlighting the variable nature of the HCl salt.
The group three material was stressed under conditions which might cause it to convert to group one material or, indeed, another hydrated or polymorphic form. Thus samples were stored at 40° C./75% RH and also at 60° C./96% RH and analysed at regular intervals by XRPD. The results are summarised in Table 2.
TABLE 2
Tabulation of stress tests on group 3 hydrochloride
Experiment
Conditions
Time
Comment
1
40° C./75% RH
0 hrs
Group three.
2
60° C./96% RH
0 hrs
Group three.
3
40° C./75% RH
24 hrs
Group three.
4
60° C./96% RH
24 hrs
Group one.
5
40° C./75% RH
48 hrs
Group three.
6
40° C./75% RH
72 hrs
Group one.
From the XRPD data (not shown) it would appear that the group three material can convert into the group one material at elevated temperature and humidity. This would have implications if the group three material was chosen as the preferred form for production as it would need to be produced in a controlled fashion and any post production manipulations, such as the formulation method, would need to be controlled to ensure that it would not convert into the group one material.
In summary, the processes employed to prepare and purify 11-(2-pyrrolidin-1-yl-ethoxy)-14,19-dioxa-5,7,26-triaza-tetracyclo[19.3.1.1(2,6).1(8,12)]heptacosa-1(25),2(26),3,5,8,10,12(27),16,21,23-decaene HCl salt are not adequately controlling the polymorphic form of the compound as there is significant batch to batch variation observed. Despite careful work to identify 3 different apparently isolable solid forms (Batches HCl 4-6) it is quite clear that the larger scale batches produced (HCl 1-3) do not closely match any of these reference standards. Batches HCl 1 and 3 are both mixtures of Groups 1 and 3 forms with varying quantities of amorphous content. Batch HCl 2 is quite close to Group 1 but unfortunately contains other unexplained peaks in the XRPD pattern. In addition even when a single polymorph is produced (batches 4 to 6) these still exhibit significant water absorption (typically up to 1.6%) which makes their use in pharmaceutical formulations difficult to ensure consistent dosing. In addition the most promising of the hydrochloride salts (batch HCl 6—group 3) from the standpoint of the DSC analysis has been found to convert to other polymorphic forms under stress as discussed above indicating that this is not a stable polymorph.
As a result of the unacceptable variability observed with the hydrochloride salt as discussed above an alternative robust solid form was required. Further discovery endeavours identified the maleate salt as being one such robust solid form.
FIG. 17 shows the results of thermal gravimetric analysis (top) and differential scanning calorimetry (bottom) of the maleate salt. The thermal gravimetric analysis clearly demonstrates that the maleate salt shows no weight loss until the salt melts with decomposition at 200° C. This indicates the general temperature stability and robust nature of the maleate salt and also that it is generally not hygroscopic. In addition inspection of the differential scanning calorimetry plot indicates that no other events (phase changes etc) are evident for this salt up to its melt and decomposition tempature of 200° C.
FIG. 18 shows the high resolution X-ray diffraction pattern (D5000) of the maleate salt. In the X-ray diagram shown the angle of diffraction 2theta is plotted on the horizontal (x) axis and the relative peak intensity on the vertical (y) axis. A complete listing of all peaks observed is shown in table 3. FIG. 19 shows the variable temperature X-ray diffraction pattern of the maleate salt. With reference to the variable temperature X-ray diffraction patterns shown it is notable that there is no change irrespective of the temperature of the experiment once again indicating the robust nature of the salt.
FIG. 20 shows the GVS data for the maleate salt. The maleate has low hygroscopicity, taking up to only less than 0.6% of its weight in water between 0 and 90% RH.
FIG. 21 shows the post-GVS XRPD data. No changes can be observed in the crystalline pattern after the GVS experiment has been carried out, again indicating the robust nature of the maleate salt.
In order to determine the propensity of polymorphism for the maleate salt the material was maturated in 27 different solvents. A small amount of solid was slurried with the corresponding solvent (see Table 4 below) and stored in the incubator and subjected to 4 h-heat/cool cycles at 50° C./r.t. for 24 h. The solvents were then removed under vacuum, and the remaining solids analysed by XRPD. In all cases only one solid form (‘Form A’) was identified.
TABLE 4
Results of solid analysis after maturation studies
Solid
Solid
Solid
Solvent
Form
Solvent
Form
Solvent
Form
Heptane
Form A
3-methyl-1-
Form A
Ethanol
Form A
butanol
Cyclo-
Form A
Methyl
Form A
Isopropyl
Form A
hexane
isobutyl
acetate
ketone
1,4-
Form A
2-butanol
Form A
methanol
Form A
dioxane
Toluene
Form A
2-methoxy
Form A
Acetonitrile
Form A
ethanol
TBME
Form A
1-butanol
Form A
Nitromethane
Form A
Isobutyl
Form A
IPA
Form A
DMSO
Form A
acetate
Propyl
Form A
Methylethyl
Form A
Water
Form A
acetate
ketone
Ethyl
Form A
1-propanol
Form A
Tetrahydro
Form A
acetate
furan
1-pentanol
Form A
acetone
Form A
Dicloromethane
Form A
The stability of the maleate salt form A material was tested in harsher conditions, when the samples were kept for a week in the humidity chamber at 60° C. and 96% RH. FIG. 22 shows that no changes are observed in the crystalline pattern even under these conditions.
TABLE 3
List of significant X-ray diffraction peaks for the maleate salt
Position of Peak (2-theta °, ±0.5°)
Relative intensity
7.0
Weak
8.3
Strong
8.8
Strong
9.2
Weak
10.6
Medium
11.4
Weak
13.0
Medium
14.1
Medium
16.9
Strong
17.5
Strong
18.3
Medium
19.0
Strong
20.7
Medium
21.3
Strong
22.3
Medium
22.7
Medium
23.1
Medium
23.8
Medium
25.3
Strong
25.8
Medium
26.8
Strong
27.5
Weak
28.2
Medium
28.5
Medium
29.1
Medium
30.5
Medium
31.3
Medium
35.0
Medium
36.8
Medium
As can be seen the maleate salt may be characterised by showing on X-ray diffraction a peak on the 2theta scale at 17.5°±0.5°.
The maleate salt may also be characterised by showing on X-ray diffraction a peak on the 2theta scale at 21.3°±0.5°.
In some embodiments the maleate salt may be further characterised as showing on X-ray diffraction at least two peaks on the 2theta scale selected from the group consisting of 8.3°±0.5°, 8.8°±0.5°, 16.9°±0.5°, 17.5°±0.5°, 19.0°±0.5°, 21.3°±0.5°, 23.8°±0.5°, 25.3°±0.5°, 25.8°±0.5° and 26.8°±0.5°.
In some embodiments the maleate salt may be further characterised as showing on X-ray diffraction at least four peaks on the 2theta scale selected from the group consisting of 8.3°±0.5°, 8.8°±0.5°, 16.9°±0.5°, 17.5°±0.5°, 19.0°±0.5°, 21.3°±0.5°, 23.8°±0.5°, 25.3°±0.5°, 25.8°±0.5° and 26.8°±0.5°.
In some embodiments the maleate salt may be further characterised as showing on X-ray diffraction at least six peaks on the 2theta scale selected from the group consisting of 8.3°±0.5°, 8.8°±0.5°, 16.9°±0.5°, 17.5°±0.5°, 19.0°±0.5°, 21.3°±0.5°, 23.8°±0.5°, 25.3°±0.5°, 25.8°±0.5° and 26.8°±0.5°.
In some embodiments the maleate salt may be further characterised as showing on X-ray diffraction peaks on the 2theta scale at 8.3°±0.5°, 8.8°±0.5°, 16.9°±0.5°, 17.5°±0.5°, 19.0°±0.5°, 21.3°±0.5°, 23.8°±0.5°, 25.3°±0.5°, 25.8°±0.5° and 26.8°±0.5°.
In some embodiments the maleate salt may be further characterised as showing on X-ray diffraction peaks on the 2theta scale at 10.6°±0.5°, 13°±0.5°, 14.1°±0.5°, 17.5°±0.5°, 18.3°±0.5°, 20.7°±0.5°, 22.3°±0.5°, 22.7°±0.5°, 23.1°±0.5°, 28.2°±0.5°, 28.5°±0.5°, 29.1°±0.5°, 30.5°±0.5°, 31.3°±0.5°, 35.0°±0.5° and 36.8°±0.5°.
Whilst the peaks discussed above are the characteristic peaks the maleate salt may also show on X-ray diffraction peaks on the 2theta scale at 7.0°±0.5°, 9.2°±0.5°, 11.4°±0.5° and 27.5°±0.5°.
As will be appreciated by a skilled worker in the field the relative intensities of the diffractions can vary depending upon a number of factors such as the method of the sample preparation and the type of instrument used. In addition in certain instances some of the peaks referred to above may not be detectable.
The salts of the present invention may be produced by reaction of the free base of compound I with an appropriate form of maleic acid in an appropriate solvent and recovering from the reaction mixture the resultant salt after crystallisation, precipitation or evaporation.
The reaction to form the salt may be carried out in any non-interfering solvent, or mixture of solvents, in which the free base has appropriate solubility. Examples of suitable solvents of this type include toluene, tetrahydrofuran and water. The process typically involves dissolution of the free base in the appropriate solvent at elevated temperature such as greater than 20° C. In some embodiments, eg tetrahydrofuran, the free base is dissolved in the solvent at a temperature of about 65° C. In some embodiments, eg water, the free base is dissolved in the solvent at a temperature of about 95° C.
Once the free base has been dissolved in the appropriate solvent the process then involves addition of a suitable amount of the acid. The amount of acid may vary although typically the amount of acid used is a stoichiometric equivalent or a slight stoichiometric excess. Following addition of the acid the process then typically involves stirring of the reaction mixture at the addition temperature for a period of 1 hour followed by cooling of the reaction mixture to a temperature below the reaction temperature to facilitate crystallisation. Once the desired level of crystal formation has occurred the crystals may be isolated by filtration and dried using normal means in the art.
In another embodiment the present invention provides the use of the salts of the invention in the treatment of proliferative disorders. The formulations and methodology for the use of compounds of this type and the disorders that may be treated thereby are as disclosed in PCT/SG2006/000352.
The present invention will now be described with reference to the following non-limiting examples. Hydrochloride salts were prepared as discussed above for comparative examples and analysed in an analogous manner.
Example 1
Formation of the Hydrochloride salt of Compound I (Comparative Example)
The free base 11-(2-pyrrolidin-1-yl-ethoxy)-14,19-dioxa-5,7,26-triaza-tetracyclo[19.3.1.1(2,6).1(8,12)]heptacosa-1(25),2(26),3,5,8,10,12(27),16,21,23-decaene was dissolved in dichloromethane, brought to reflux and treated with activated carbon. The mixture was filtered hot through a pad of celite and washed with dichloromethane. To the filtrate was added methanolic HCl and the mixture was stirred at 10-15° C. for 2-3 hours. The slurry was cooled to 5-10° C., filtered, washed with heptane and dried in a vacuum oven at 40-45° C. to afford 11-(2-pyrrolidin-1-yl-ethoxy)-14,19-dioxa-5,7,26-triaza-tetracyclo[19.3.1.1(2,6).1(8,12)]heptacosa-1(25),2(26),3,5,8,10,12(27),16,21,23-decaene hydrochloride.
Example 2
Formation of Maleate Salt
Compound I (50 mg, 0.106 mmol) was suspended in either THF or toluene (2 mL), and gently heated to 65° C. until it became a clear solution. The solution was then treated with 1 equivalent of maleic acid, heated at 65° C. for one hour and slowly cooled down to 5° C. overnight to facilitate crystallisation. The crystals thus formed were then isolated by filtration.
Example 3
Thermal Gravimetric Analysis and Differential Scanning Calorimetry
The samples of both hydrochloride (comparative) and maleate salts were subjected to thermal gravimetric analysis and differential scanning calorimetry under the following conditions. DSC data were collected on a TA Instruments Q2000 equipped with a 50 position auto-sampler. The instrument was calibrated for energy and temperature calibration using certified indium. Typically 0.5-3 mg of each sample, in a pin-holed aluminium pan, was heated at 10° C.·min −1 from 25° C. to 270° C.
A nitrogen purge of 50 ml·min −1 was maintained over the sample. The instrument control software was Thermal Advantage v4.6.6 and the data were analysed using Universal Analysis v4.3A. Alternatively, DSC data were collected on a Mettler DSC 823e equipped with a 50 position auto-sampler. The instrument was calibrated for energy and temperature using certified indium. Typically 0.5-3 mg of each sample, in a pin-holed aluminium pan, was heated at 10° C.·min −1 from 25° C. to 270° C. A nitrogen purge at 50 ml·min −1 was maintained over the sample. The instrument control and data analysis software was STARe v9.01.
TGA data were collected on a TA Instruments Q500 TGA, equipped with a 16 position auto-sampler. The instrument was temperature calibrated using certified Alumel. Typically 5-30 mg of each sample was loaded onto a pre-tared platinum crucible and aluminium DSC pan, and was heated at 10° C.·min −1 from ambient temperature to 300° C. A nitrogen purge at 60 ml·min −1 was maintained over the sample. The instrument control software was Thermal Advantage v4.6.6 and the data were analysed using Universal Analysis v4.3A. Alternatively, TGA data were collected on a Mettler TGA/SDTA 851e equipped with a 34 position auto-sampler. The instrument was temperature calibrated using certified indium. Typically 5-30 mg of each sample was loaded onto a pre-weighed aluminium crucible and was heated at 10° C.·min −1 from ambient temperature to 300° C. A nitrogen purge at 50 ml·min −1 was maintained over the sample. The instrument control and data analysis software was STARe v9.01. The results of the scans are shown in the figures discussed above.
Example 4
X-Ray Diffraction Analysis
The samples of both hydrochloride (comparative) and maleate salts were subjected to X-ray diffraction to determine the characteristic X-ray diffraction pattern. The conditions used were as follows: X-Ray Powder Diffraction patterns were collected on a Siemens D5000 diffractometer using Cu Kα radiation (40 kV, 40 mA), θ-θ goniometer, divergence of V20 and receiving slits, a graphite secondary monochromator and a scintillation counter. The instrument is performance checked using a certified Corundum standard (NIST 1976).
Ambient Conditions
Samples run under ambient conditions were prepared as flat plate specimens using powder as received. Approximately 35 mg of the sample was gently packed into a cavity cut into polished, zero-background (510) silicon wafer. The sample was rotated in its own plane during analysis. The details of the data collection are:
Angular range: 2 to 42 °2θ
Step size: 0.05 °2θ
Collection time: 4 s·step −1 .
Alternatively, X-Ray Powder Diffraction patterns were collected on a Bruker AXS C2 GADDS diffractometer using Cu Kα radiation (40 kV, 40 mA), automated XYZ stage, laser video microscope for auto-sample positioning and a HiStar 2-dimensional area detector. X-ray optics consists of a single Göbel multilayer mirror coupled with a pinhole collimator of 0.3 mm. The beam divergence, i.e. the effective size of the X-ray beam on the sample, was approximately 4 mm. A θ-θ continuous scan mode was employed with a sample-detector distance of 20 cm which gives an effective 2θ range of 3.2°-29.7°. Typically the sample would be exposed to the X-ray beam for 120 seconds.
Samples run under ambient conditions were prepared as flat plate specimens using powder as received without grinding. Approximately 1-2 mg of the sample was lightly pressed on a glass slide to obtain a flat surface.
Non-Ambient Conditions:
Samples run under non-ambient conditions were mounted on a silicon wafer with heat-conducting compound. The sample was then heated to the appropriate temperature at ca. 10° C.·min −1 and subsequently held isothermally for ca 2 minutes before data collection was initiated.
The X-ray diffraction patterns for the maleate salts are shown in the figures discussed above.
Example 5
Variable Temperature X-Ray Diffraction
In order to probe the stability of the samples of the maleate salts variable temperature X-ray diffraction was carried out. Thus, the salts were scanned under X-ray diffraction conditions at a series of temperatures and the characteristic peaks determined. The results of each of the scans are shown in the figures discussed above.
The details of specific embodiments described in this invention are not to be construed as limitations. Various equivalents and modifications may be made without departing from the essence and scope of this invention, and it is understood that such equivalent embodiments are part of this invention. | The present invention relates to certain salts of a 11-(2-pyrrolidin-1-yl-ethoxy)-14,19-dioxa-5,7,26triaza-tetra-cyclo[19.3.1.1(2,6).1(8,12)]heptacosa-1(25),2(26),3,5,8,10,12(27),16,21,23-decaene (Compound I) which have been found to have improved properties. In particular the present invention relates to the maleate salt of this compound. The invention also relates to pharmaceutical compositions containing this salt and methods of use of the salt in the treatment of certain medical conditions. | 2 |
This application claims priority to U.S. provisional application No. 60/950,222, filed Jul. 17, 2007, which is incorporated herein by reference.
BACKGROUND OF THE INVENTION
This invention relates to cotton fiber processing and more particularly to an apparatus and method of separating foreign matter from fibrous cotton that has been ginned from the seed.
Prior methods and apparatus include those such as illustrated in U.S. Pat. No. 6,088,881, incorporated herein by reference, wherein a revolving perforated drum is used to allow air flow through the drum such that a cleaning cylinder may remove cotton fiber from the perforated drum and carry it past a plurality of cleaning grid bars, thereby separating the air flow and removing foreign matter from the fibers, before the fiber is doffed from the cleaning cylinder for subsequent air flow to downstream processing.
However, the perforated revolving cylinder of the '881 apparatus, revolving at velocities to prevent agglomeration of the tufts in the air stream, develops centrifugal forces that cause the fine trash and very short fibers that penetrate the perforations to accumulate on the interior surfaces of the perforated cylinder. These accumulations require the use of compressed air blasts to cause them to move axially out the open ends of the cylinder. While the compressed air blasts provide a solution to this problem of accumulations, the maintenance and cost of the compressed air system detracts from the otherwise excellent performance of the apparatus per the '881 patent.
BRIEF DESCRIPTION OF THE DRAWINGS
An apparatus embodying features of the invention is depicted in the accompanying drawing wherein:
FIG. 1 is a sectional side elevational view of an embodiment of an apparatus of the present invention.
BRIEF SUMMARY OF THE INVENTION
It is an object of the present invention to provide an improved method and apparatus for separating foreign matter from tufts of fibrous cotton. A further object of the invention is to eliminate the need for a compressed air system for cleaning a perforated separator cylinder, while maintaining the other features of the '881 patent by the use of a novel revolving separator in combination with a stationary arcuate perforated section.
DETAILED DESCRIPTION OF THE INVENTION
An improved apparatus and method according to the present invention is illustrated in reference to FIG. 1 , wherein fiber tufts commingled with foreign matter are pneumatically carried by a conveying air stream C into the apparatus via an air duct 11 as is well known in the art. Air duct 11 terminates adjacent an outer surface of a revolving cleaning cylinder 12 and a stationary separator housing. Duct 11 has an arcuate terminal wall portion 14 disposed adjacent to cleaning cylinder 12 to deliver the fiber tufts directly to a plurality of teeth 13 carried by the cleaning cylinder 12 and capable of holding the fiber tufts on said teeth 13 . The cylindrical housing comprises an arcuate non-porous surface 15 , a semi-cylindrical perforated surface or section 16 , and a non porous segment 15 a spaced from terminal portion 14 of duct 11 at the end of a minor chord drawn through revolving cylinder 12 , such that the cylindrical housing is open to duct 11 opposite terminal wall portion 14 . Perforated surface 16 is a stationary separator that is porous to air flow there through but impervious to desirable fiber flow there through. Rotating within the cylindrical housing is an revolving air separator 17 which is pervious to both fiber and foreign matter. As may be seen in FIG. 1 , terminal wall portion 14 of duct 11 converges toward revolving air separator 17 near cleaning cylinder 12 such that fiber tufts carried by the conveying air stream are directed substantially on to the teeth 13 of cleaning cylinder 12 while the direction of the conveying air flow is gradually changed toward the cylindrical housing comprising perforated surface 16 .
Again as may be seen in FIG. 1 , revolving separator 17 includes a plurality of circumferentially spaced outer surfaces 18 such that the spaces between spaced outer surfaces 18 are sufficient to allow the conveying air to pass between the spaced surfaces 18 as air duct 11 converges toward the spaced surfaces 18 without abruptly increasing the conveying air velocity. Outer surfaces 18 pass proximal to the revolving cleaning cylinder 12 and semi-cylindrical stationary surface 16
In one embodiment outer surfaces 18 are defined by circumferentially spaced apart flexible belt-like strips running generally parallel to the axis of rotation of air separator 17 and generally radial to the axis of rotation. The strips are flexible radially and may be made of soft material to resist damage to the cleaning cylinder 12 or semi-cylindrical stationary surface 16 . In another embodiment, spaced outer surfaces 18 are defined by circumferentially spaced apart brush strips running generally parallel to the axis of rotation with the bristles facing outward generally radial to the axis of rotation of the air separator 17 . Suitable hub plates 22 hold the hubs 25 of the strips 18 in place forming an open reel. In either embodiment, the strips are preferably set at a deflection angle of the strips approximately 15 degrees backward from radial to the axis of rotation of the rotating separator 17 relative to its direction of rotation.
The conveying air stream C thus passes through the air separator 17 and is exhausted from the cylindrical housing via perforated surface 16 to become exhaust air stream E. It is worthwhile to note that as outer surfaces 18 rotate across perforated surface 16 the surfaces 18 substantially sweep away any accumulations of matter on the stationary separator surface 16 and return any desirable fiber back to the conveying air stream C, proximal to terminal portion 14 of duct 11 . To effectively accomplish this, revolving outer surfaces 18 move at velocities that develop centrifugal forces sufficient to cause heavier than air matter revolving with the outer surface 18 to move substantially radially outwardly. Further the hubs or inner surface 25 of the strips 18 are configured to resist accumulation of matter heavier than air thereon, such that the rotation of the hub 25 and surfaces 18 moves such matter outwardly where it may be directed towards cleaning cylinder 12 . The rotation of revolving outer surfaces 18 is such that the commingled fiber and foreign matter are exposed to the teeth 13 of the cleaning cylinder 12 while the revolving outer surfaces 18 are rotating toward stationary semi cylindrical surface 16 .
As will be understood from the prior art, the rotation of cleaning cylinder 12 carries the tufts past a stripping bar 27 and plurality of cleaning grid bars 23 disposed to separate a major portion of foreign matter from the cleaning cylinder 12 , which foreign matter may be disposed via a trash conveyor system for subsequent collection and baling. In the embodiment depicted, foreign matter is disposed via a waste airflow W.
As will also appreciated, a rotating doffing cylinder or brush 24 removes the cleaned tufts from the teeth 13 of cleaning cylinder 12 and delivers the cleaned fibers to duct 26 . In the embodiment depicted, the cleaned tufts may be entrained in a doffing air flow D which passes adjacent doffing brush 24 and into duct 26 .
The apparatus may be used to process cotton fiber according to the following description. Spaced apart individual tufts of fiber are conveyed in a high speed conveying air stream C to minimize agglomeration of the tufts, first exposing the air stream to revolving separator 17 which is porous to radially inward and outward air flow and revolving at speeds developing centrifugal forces that cause the fiber tufts and foreign matter rotationally moving with the porous revolving separator 17 to resist radially inward movement such that the fiber tufts and foreign are substantially removed from the conveying air C as it passes through the porous revolving air separator 17 . Thus, the preponderance of the fiber tufts and foreign matter are delivered directly to revolving toothed cleaning cylinder 12 in close proximity to the revolving separator 17 .
A stationary generally cylindrical surface is located downstream of the revolving toothed cylinder 12 relative to the rotation of and proximal to the porous revolving air separator 17 . The stationary arcuate surface includes a porous section 16 being porous to air flow there through, but impervious to desirable fiber flow, and preferably contains one or more non-porous sections 15 . The rotational movement of the outer surfaces 18 carried by revolving porous air separator 17 proximate stationary arcuate surface sweeps any accumulations of desirable fiber from the upstream side of arcuate stationary surface 15 , 16 delivering the fibers back into the conveying air stream C. The periphery of the revolving separator 17 should be porous to radially inward and outward air flow and have means on the radially inward surfaces to prevent the accumulation of matter heavier than air.
Revolving toothed cylinder 12 holds the tufts while revolving past stripping bar 27 and cleaning bars 23 that strip foreign matter from the fiber tufts. A doffing brush or roller 24 revolving proximate and counter to toothed cleaning cylinder 12 removes the cleaned fibers from teeth 13 and delivers the cleaned fiber tufts from the process.
While the forgoing specification describes only a few embodiments of the present invention, the invention is not so limited and is intended to encompass the full scope of the claims appended hereto. | An apparatus for cleaning foreign matter from separated tufts of fiber uses a revolving open reel type structure mounted within a porous housing to separate a conveying air stream from tufts of fiber conveyed thereby and deliver the tufts to a toothed cleaning cylinder which passes beneath a plurality of cleaning bars. The open reel utilizes brush like outer surfaces to sweep tufts of fiber from the housing back into the air stream adjacent the cleaning cylinder. | 3 |
FIELD OF THE INVENTION
[0001] This invention relates to ion-binding ligands covalently bonded to membranes and to a process for removing and concentrating certain selected ions from solutions using the ligand-membrane compositions, wherein such ions may be admixed with other ions present in much higher concentrations. More particularly, the invention relates to ligand-membrane compositions and to a process for removing such ions from an admixture with other ions in a source solution by forming a complex of the selected ions with the ligand-membrane compositions by flowing such solutions through a contacting device containing the ligand-membrane compositions and then breaking the complex of the selected ion from the composition to which such ion has become attached by flowing a receiving liquid in much smaller volume than the volume of solution passed through the contacting device to remove and concentrate the selected ions in solution in the receiving liquid. The concentrated ions thus removed may then be recovered by known methods.
BACKGROUND OF THE INVENTION
[0002] Composite membranes of the type utilized in one embodiment of the present invention have been previously described in U.S. Pat. No. 4,618,533 to Steuck. Some of the ion-binding ligands of the types disclosed herein are also known. For example, U.S. Pat. No. 4,952,321 to Bradshaw et al. discloses amine-containing hydrocarbons attached to a solid inorganic support such as silica or silica gel wherein the ligand is bound to the solid inorganic support through a hydrocarbon spacer containing a trialkoxysilane group. U.S. Pat. Nos. 5,071,819 and 5,084,430 to Tarbet et al. disclose sulfur and nitrogen-containing hydrocarbons as ion-binding ligands. U.S. Pat. Nos. 4,959,153 and 5,039,419 to Bradshaw et al. disclose sulfur-containing hydrocarbon ligands. U.S. Pat. Nos. 4,943,275 and 5,179,213 to Bradshaw et al. disclose ion-binding crowns and cryptands as ligands. U.S. Pat. No. 5,182,251 to Bruening et al. discloses aminoalkylphosphonic acid-containing hydrocarbons ligands. U.S. Pat. No. 4,960,882 to Bradshaw discloses proton-ionizable macrocyclic ligands. U.S. Pat. No. 5,078,978 to Tarbet et al. discloses pyridine-containing hydrocarbon ligands U.S. Pat. No. 5,244,856 to Bruening et al. discloses polytetraalkylammonium and polytrialkylamine-containing hydrocarbon ligands. U.S. Pat. No. 5,173,470 to Bruening et al. discloses thiol and/or thioether-aralkyl nitrogen-containing hydrocarbon ligands. U.S. Pat. No. 5,190,661 to Bruening et al. discloses sulfur-containing hydrocarbon ligands also containing electron withdrawing groups. Copending application Ser. No. 08/058,437 filed May 7, 1993, discloses oxygen donor macrocycles, for example, ligands containing macrocyclic polyether cryptands, calixarenes, and spherands, multiarmed ethers and mixtures of these. All of these previous reports have involved binding of the ligands to solid inorganic supports via a silane-containing spacer grouping. However, researchers have not previously reported incorporating complex, strongly interacting and highly selective ion-binding ligands into membranes which would be highly desirable because of the high surface-to-area ratios, convenient physical formats, ease of production, ease of use, and inexpensive cost of such membranes. The present invention successfully accomplishes this feat.
SUMMARY OF THE INVENTION
[0003] The compositions of the present invention comprise ion-binding ligands that are covalently bonded to a membrane through an amide, ester, thioester, carbonyl or other suitable bond. Membranes that are inherently hydrophilic, or partially hydrophilic, and contain moieties appropriate for making these bonds are preferred. Such membranes include polyamides, such as nylon, and cellulosic materials, such as cellulose, regenerated cellulose, cellulose acetate, and nitrocellulose. If the membrane used does not contain reactive groups it may be modified or derivatized appropriately. Composite membranes are also useful. A composite membrane comprises a porous polymer membrane substrate and an insoluble, cross-linked coating deposited thereon. Representative suitable polymers forming the membrane substrate include fluorinated polymers including poly(tetrafluoroethylene) (“TEFLON”), polyvinylidene fluoride (PVDF), and the like; polyolefins such as polyethylene, ultra-high molecular weight polyethylene (UPE), polypropylene, polymethylpentene, and the like; polystyrene or substituted polystyrenes; polysulfones such as polysulfone, polyethersulfone, and the like; polyesters including polyethylene terephthalate, polybutylene terephthalate, and the like; polyacrylates and polycarbonates; and vinyl polymers such as polyvinyl chloride and polyacrylonitriles. Copolymers can also be used for forming the polymer membrane substrate, such as copolymers of butadiene and styrene, fluorinated ethylene-propylene copolymer, ethylene-chlorotrifluoroethylene copolymer, and the like.
[0004] With composite membranes, the substrate membrane material is not thought to affect the performance of the derivatized membrane and is limited in composition only by its ability to be coated, or have deposited on its surface, an insoluble polymer layer that contains the appropriate reactive group. This provides a hydrophilic layer which interacts well with water or other aqueous solutions. The end result is that when an organic ligand is attached to the surface of either a hydrophilic membrane or a composite membrane having a hydrophilic surface, the basic characteristics of any given ligand molecule are not changed by the process of attaching it to the surface or by the nature of the surface itself.
[0005] The coating of composite membranes comprises a polymerized cross-linked monomer. Representative suitable polymerizable monomers include hydroxyalkyl acrylates or methacrylates including 1-hydroxyprop-2-yl acrylate and 2-hydroxyprop-1-yl acrylate, hydroxypropylmethacrylate, 2,3-dihydroxypropyl acrylate, hydroxyethylacrylate, hydroxyethyl methacrylate, and the like, and mixtures thereof. Other polymerizable monomers that can be utilized include acrylic acid, 2-N,N-dimethylaminoethyl methacrylate, sulfoethylmethacrylate and the like, acrylamides, methacrylamides, ethacrylamides, and the like. Other types of hydrophilic coatings that can be used within the scope of the invention include epoxy functional groups such as glycidyl acrylate and methacrylate, primary amines such as aminoethyl methacrylates, and benzyl derivatives such as vinyl benzyl chloride, vinyl benzyl amine, and p-hydroxyvinyl benzene.
[0006] The coating of composite membranes also comprises a precipitated crystal system, such as that involving the material known under the trademark “NAFION.” “NAFION” is a sulfonic acid or sodium sulfonate of a perfluorinated polyether.
[0007] The basic consideration in selecting a composite membrane is that the coating placed on the membrane substrate is the determining factor in defining the chemistry used to covalently attach the ligand. For example, a composite membrane displaying a carboxylic acid functional group can form an amide bond with a pendant amine group from the ligand, one of the most stable methods of ligand immobilization. The composite polymers referenced above can be prepared with carboxylic acid active groups that can be readily converted to amides upon reaction with an amine group on a ligand. However, any of the other organic species which are reactive toward an acid chloride could be used to attach an organic ligand to the surface. Additional examples of such groups would be esters, thioesters, Grignard reagents, and the like.
[0008] If the reactive group on the surface is a sulfonic acid, then an analogous procedure using a sulfonyl chloride would yield results similar to those obtained with carboxylic acid functionalities. One such polymer containing sulfonic acid reactive groups is available under the tradename “NAFION” from DuPont as described above.
[0009] The ligand is selected from the group consisting of amine-containing hydrocarbons, sulfur and nitrogen-containing hydrocarbons, sulfur-containing hydrocarbons, crowns and cryptands, aminoalkylphosphonic acid-containing hydrocarbons, polyalkylene-polyamine-polycarboxylic acid-containing hydrocarbons, proton-ionizable macrocycles, pyridine-containing hydrocarbons, polytetraalkylammonium and polytrialklylamine-containing hydrocarbons, thiol and/or thioether-aralkyl nitrogen-containing hydrocarbons, sulfur-containing hydrocarbons also containing electron withdrawing groups, and macrocyclic polyether cryptands, wherein the ligands are capable of selectively complexing ions such as either certain alkali, alkaline earth, noble metal, other transition metal, and post transition metal ions when contacted with solutions thereof when admixed with other ions.
[0010] The process for removing and concentrating certain selected ions using the ligand-membrane compositions is carried out in any manner that provides for bringing the ion to be removed into contact with the ligand affixed to the membrane. Overall the process comprises selectively removing and concentrating one or more selected species of ion from a plurality of other ions in a multiple ion solution in which the other ions may be present at much higher concentrations. The multiple ion solution or source solution is brought into contact with a composition of the present invention. The preferred embodiment disclosed herein involves carrying out the process by bringing a large volume of the multiple ion solution into contact with a composition of matter of the invention. Contact is preferably made in a contacting device comprising a cartridge containing the composition of matter of the invention by causing the multiple ion solution to flow through the cartridge and thus come in contact with the composition of the invention. However, various contact apparatus may be used instead of a cartridge. The selected ion or ions complex with the composition. Following the complexing step, a small volume of a receiving liquid or eluant is brought into contact with the loaded composition to break the complex by chemical or thermal means and to dissolve the selected ions and carry them away from the composition. The selected ions can then be recovered from the receiving liquid by well known procedures.
[0011] More particularly, the process comprises forming a complexing agent by covalent bonding of a ligand of the type mentioned previously to a composite membrane, such as one of those previously mentioned. The complexing agent is then introduced into a contacting device such as a cartridge. The solution containing the multiple ion species flows through the cartridge in contact with the complexing agent, whereby the selected ions complex with the complexing agent. The selected ions are thus separated from the rest of the ion mixture that flows out of the cartridge. A small volume of the receiving liquid or eluant is then passed through the cartridge to break the complex and dissolve and carry out of the cartridge the selected ion or ions. The selected ions are then recovered from the receiving phase by well known procedures.
DETAILED DESCRIPTION OF THE INVENTION
[0012] Preparation of the Ligand-Membrane Compositions
[0013] The compositions of the present invention may be prepared by any suitable method wherein the ligands can be covalently bonded to a membrane containing reactive functional groups.
[0014] The membrane is selected to yield both selected bulk properties and selected surface properties. For naturally hydrophilic membranes, the selected bulk and surface properties will be provided by whatever polymer that comprises the membrane. For composite membranes, the selected bulk properties will be provided by the membrane substrate and the selected surface properties will be provided by the coating. A composite membrane is formed by depositing a monomer directly on the surface of the substrate, including the inner surfaces of the pores, by in situ deposition of the cross-linked monomer. The desired deposition of the cross-linked monomer onto the porous substrate is effected as a direct coating and does not require or utilize an intermediate binding chemical moiety. Any monomer for the coating polymer can be used so long as it is capable of being polymerized by free radical polymerization and can be cross-linked. The only requirements of the polymerized monomer is that it is capable of coating the entire surface of the porous membrane, that it provide the surface with ligand-reactive functional groups, and that it be sufficiently hydrophilic to allow for efficient use of the ligand to be attached. Generally, the porous substrate has an average pore size between about 0.001 and 10 μm, and more usually, between about 0.1 and 5.0 μm. The composite membrane is formed by any suitable method, such as is disclosed in U.S. Pat. No. 4,618,533, which is hereby incorporated by reference. Briefly, this procedure involves washing the porous membrane substrate with a suitable solvent for wetting the entire surface of the substrate. The substrate is then bathed in a mixture of the free radical polymerizable monomer, a polymerization initiator, and a cross-linking agent in a solvent under conditions to effect free radical polymerization of the monomer and coating of the porous substrate with the cross-linked polymer. The surface of the coated polymer membrane contains hydrophilic or polar-substituents that can be activated to react with and covalently bond the ligands to the membrane surface.
[0015] The composite membranes prepared according to U.S. Pat. No. 4,618,533 can contain carboxylic acid moieties on the surface. Other suitable moieties could include hydroxyl, sulfonic acid, epoxy, primary amine, and derivatized benzyl groups such as polymers referenced above.
[0016] Preparation of a composite membrane by a precipitated crystal technique involves, briefly, washing the porous membrane substrate with a suitable solvent for wetting the entire surface of the substrate. The substrate is then bathed in a solution containing the crystals that are to be precipitated. This solution is then removed and the membrane substrate is treated with a compound that precipitates and fixes the crystals to the substrate. The membrane is washed and dried before use.
[0017] In the present invention, the activation of the carboxylic acid groups is exemplified by the reaction of the carboxylic acid groups with thionyl chloride to form acid chloride groups according to the formula:
membrane-COOH+S(O)Cl 2 →membrane-C(O)Cl+SO 2 +HCl
[0018] Carboxylic acid groups also can be converted to acid chloride groups by reaction with phosphorus pentachloride or phosphorus trichloride.
[0019] Ligands (L) containing reactive amines, alcohols, thiols, Grignard reagents and the like may be covalently bonded to the membrane through the —C(O)Cl group as follows:
membrane-C(O)Cl+H 2 NL→membrane-C(O)NHL+HCl (amide) (1)
membrane-C(O)Cl+HOL→membrane-C(O)OL+HCl (ester) (2)
membrane-C(O)Cl+HSL→membrane-C(O)SL+HCl (thioester) (3)
membrane-C(O)Cl+XMgL→membrane-C(O)L+MgXCl (ketone) (4)
[0020] In a similar manner, the activation of the sulfonic acid groups is exemplified by the reaction of the sulfonic acid groups with thionyl chloride to form sulfonyl chloride groups according to the formula:
membrane-S(O) 2 OH+S(O)Cl 2 →membrane-S(O) 2 Cl+SO 2 +HCl
[0021] Sulfonyl chloride groups also can be obtained by reaction of sulfonic acid groups with phosphorus pentachloride or phosphorus trichloride.
[0022] Ligands containing reactive amines, alcohols and the like may be covalently bonded to the membrane through the —S(O) 2 Cl group as follows:
membrane-S(O) 2 Cl+H 2 NL→membrane-S(O) 2 NHL+HCl (sulfonamide) (1)
membrane-S(O) 2 Cl+HOL→membrane-S(O) 2 OL+HCl (sulfonate ester) (2)
[0023] This reaction does not proceed as readily as the reactions with acid chlorides formed from carboxylic acids. However, any reaction may be used provided it is functional to form a stable covalent bond between the ligand and the membrane. For the present, it has been found that the amide linkage is most stable and readily formed.
[0024] Ligands, which may be adapted to contain —NH, —OH, —SH, —MgX moieties which are reactive so as to form a covalent bond with membrane attached functionalities are illustrated in the patents indicated below, which are hereby incorporated by reference: amine-containing hydrocarbons (U.S. Pat. No. 4,952,321), sulfur and nitrogen-containing hydrocarbon ligands (U.S. Pat. Nos. 5,071,819 and 5,084,430), sulfur-containing hydrocarbon ligands (U.S. Pat. Nos. 4,959,153 and 5,039,419), crowns and cryptand ligands (U.S. Pat. Nos. 4,943,375 and 5,179,213), aminoalkylphosphonic acid-containing hydrocarbon ligands (U.S. Pat. No. 5,182,251), proton-ionizable macrocycle ligands (U.S. Pat. No. 4,960,882), pyridine-containing hydrocarbon ligands (U.S. Pat. No. 5,078,978), polytetraalkylammonium and polytrialkylamine-containing hydrocarbon ligands (U.S. Pat. No. 5,244,856), thiol and/or thioether-aralkyl nitrogen-containing hydrocarbon ligands (U.S. Pat. No. 5,173,470), and sulfur and electron withdrawing group-containing hydrocarbon ligands (U.S. Pat. No. 5,190,661).
[0025] An oxygen donor macrocycle ligand, such as disclosed in copending application Ser. No. 08/058,437 filed May 7, 1993, having a reactive grouping attached, may be prepared by various reaction schemes. Two are illustrated. The first involves the reaction of a cis dihydroxy crown ether with a polyether diol wherein the diol groups have been activated by reaction with a “leaving” group such as tosyl chloride. The following reaction sequence (Reaction A) shows the formation of an oxygen donor macrocycle ligand (Formula 2) by means of reacting a cis dihydroxy crown ether (Formula 3) with a tosylated polyether diol (Formula 4) as follows wherein Ts stand for the tosyl group, R 3 , R 4 , R 5 , and R 6 is each a member independently selected from the group consisting of H, allyloxymethyl, alkylthio, alkylamino, carboxy, carboxyalkyl, and epoxyalkyl. R 7 is a member selected from the group consisting of H and alkyl, Z is a member selected from the group consisting of o-phenylene and o-naphthalene or alkyl, R 1 and R 2 are each a member selected from the group consisting of H, allyl, alkenyl, carboxy, carboxyalkyl, allyloxy, aminoalkyl, hydroxy, thio, and alkylthio. The functional groups that are not directly reactive with the corresponding groups on the surface of the membrane must be further reacted so as to allow a covalent bond. As an example, a carboxy alkyl functional group could be converted to an acid chloride and further reacted with ethylene diamine (in large excess) to provide a mono amide with a free amine. This could then be reacted with the membrane. Further, n is an integer of 2 to 4, a is an integer of 0 or 1, b is an integer of 0 to 3 with the proviso that b must be at least 1 when a is 0, and m is an integer of 0 to 5. To provide a reactive grouping to react with a reactive membrane, it is mandatory that one or two, and preferably only one, of the R 1 through R 5 groups must be other than H. The remaining R 1 through R 5 groups are H.
[0026] While the Ts or tosyl group is illustrated above, other leaving groups such as mesylates, chlorides, bromides and the like can also be utilized. The tosyl group is preferred because it is crystalline and has better reaction properties.
[0027] The second reaction scheme involves the reaction of a cis dibromomethyl crown ether with a polyether diol. The following reaction sequence (Reaction B) shows the formation of an oxygen donor macrocycle ligand (Formula 2) by means of reacting a cis dibromomethyl crown ether (Formula 5) with a polyether diol (Formula 6) as follows wherein symbols have the same meaning as given for Formula 2 above:
[0028] The compound corresponding to Formula 2, having a reactive-grouping may then be reacted with a membrane derivatized with hydrophilic functionalities.
[0029] Polyalkylene-polyamine-polycarboxylic acid-containing hydrocarbon ligands may be prepared by various methods. For example, in one method the polyalkylene-polyamine-polycarboxylic acid ligand is bound to the membrane. In a second method, a polyalkylenepolyamine is reacted with a membrane followed by reacting with a polycarboxylic acid.
[0030] The above described ligands have heretofore been attached to solid supports such as silica gel, silica, glass, glass fibers, nickel oxide, zirconia, alumina, titania and the like. The attachment of the ligand to the solid support has been by means of a silane spacer grouping. There are certain drawbacks to the use of such solid support. For example, they most often have to be contained in a column or similar structure and do not have the adaptability for other configurations that a membrane possesses. Further, silane chemistry is complicated and limits certain reactions or applications. Finally, the instability or even partial dissolution of the inorganic supports in some solution matrices makes their use in some separation applications poor or unacceptable. However, such ligands, that have been attached to the above mentioned inorganic solid supports, have not previously been affixed to membranes.
[0031] The novelty of the invention is in the membrane ligand combination and in the method of using such combinations in removing desired ions. Any of the ligands previously used may be modified for use in the present invention. Because the ligands are not in and of themselves novel, they will be referred to as ligands (“L”) and may be further designated by classes, i.e. amine-containing hydrocarbon ligands; sulfur and nitrogen-containing hydrocarbon ligands; sulfur-containing hydrocarbon ligands; crown and cryptand ligands; aminoalkylphosphonic acid-containing hydrocarbon ligands; proton-ionizable macrocycle ligands; pyridine-containing hydrocarbon ligands; polytetraalkylammonium and polytrialkylamine-containing hydrocarbon ligands; thiol and/or thioether-aralkyl nitrogen-containing hydrocarbon ligands; sulfur and electron withdrawing group-containing hydrocarbon ligand; and oxygen donor macrocycle ligands. This listing of ligands is exemplary only and is not intended to be all encompassing. Other ligands, known or yet to be developed, may also be utilized with the only limitation being that they can be covalently attached to the membrane and are functional in the selective attracting and binding of the selected ions being removed from the solutions being treated.
[0032] The membrane ligand combination of the invention can therefore be defined by the formula:
M—B—L
[0033] wherein M is any membrane or composite membrane derivatized to have a hydrophilic surface and contain polar functional groups, L is any ligand as defined above containing a functional grouping reactive with an activated polar group from the membrane and B is the covalent linkage formed by the reaction between the activated polar group and the functional group of the ligand. Representative of 3 linkages are members selected from the group consisting of amide (NHCO), ester (COO), thioester (COS), carbonyl (CO), ether (O), thioether (S), and sulfonamide (SO 2 NH).
[0034] The membrane/ligand compositions of the present invention that are useful for separating selected ions will be apparent to those skilled in the art by the following examples each of which utilizes a composite membrane prepared according to U.S. Pat. No. 4,618,533 and containing carboxylic acid groups or sulfonic acid groups.
EXAMPLE 1
[0035] In this example, a nitrogen-containing ligand derivatized membrane was prepared according to the following procedure. A 3×3 inch piece of polytetrafluoroethylene (PTFE) (“TEFLON”) membrane coated by the method of U.S. Pat. No. 4,618,533 with crosslinked acrylic acid containing carboxylic acid functional groups immobilized on the surface was immersed in enough thionyl chloride to completely cover the surface of the membrane. The membrane remained covered by this solution for 3-14 hours to enable the thionyl chloride to react with and convert the carboxylic acid groups to acid chlorides. The activated membrane was then removed and washed thoroughly with hexane. Other organic solvents, such as toluene, would work equally well. The activated membrane was then placed in a flask containing a solution composed of 3 g of pentaethylenehexamine ligand and enough toluene to be sure the membrane was completely covered by the mixture. This mixture was allowed to react for 8-14 hours to form an amide bond between one of the amine groups of the ligand and the acid chloride group of the membrane. The membrane was again washed with organic solvent to remove unbound ligand and permitted to air dry in a well-ventilated hood. After the membrane was dried it was tested to determine its ion binding properties. Testing results are shown in Example 14.
EXAMPLE 2
[0036] In this example, a 3×3 inch piece of polyvinylidene fluoride (PVDF) membrane coated by the method of U.S. Pat. No. 4,618,533 with crosslinked acrylic acid containing carboxylic acid functional groups was converted to the acid chloride form and then derivatized with pentaethylenehexamine as in Example 1.
[0037] In Examples 3-12 which follow the carboxylic acid derivatized PTFE composite membrane of Example 1 was utilized for ligand attachment. However, the PVDF composite membrane of Example 2 could have been used with similar results. When testing the separation properties of ligands affixed to composite membranes of both Examples 1 and 2, the results were substantially the same.
EXAMPLE 3
[0038] In this example, a nitrogen and sulfur-containing ligand derivatized membrane was prepared according to the following procedure. A 3×3 inch square of carboxylic acid group containing PTFE composite membrane was prepared and treated with thionyl chloride as in Example 1. This material was then reacted with pentaethylenehexamine as a first step to attach the amine via an amide bond to the membrane. This intermediate product was then washed, and immersed in a second solution containing toluene and 1 g of ethylene sulfide to provide the ligand with a —NHCH 2 CH 2 SH grouping. Again, it was necessary to ensure that the solution covered the membrane at all times. The reaction times for each step are from 8-14 hours. After the membrane was dried, it was tested for ion complexation properties as shown in Example 15.
EXAMPLE 4
[0039] In this example, a nitrogen and sulfur-containing ligand derivatized membrane was prepared according to the following procedure. A 3×3 inch square of carboxylic acid group containing PTFE composite membrane was treated with thionyl chloride as in Example 1. This material was then reacted with ethylene diamine instead of pentaethylenehexamine as in Example 3. The result of this reaction is a material that is bonded to the membrane via an amide linkage and contains one free amino group that is then further reacted with a solution containing toluene and ethylene sulfide as in Example 3. After the membrane was dried, it was tested for ion complexation properties as shown in Example 16.
EXAMPLE 5
[0040] In this example, a sulfur-containing ligand derivatized membrane was prepared according to the following procedure. The carboxylic acid group containing PTFE composite membrane was prepared as in Example 4 so that the carboxylic acid groups were converted to the acid chloride form. The membrane was then immersed in a solution containing toluene and the reaction product of ethanedithiol and one equivalent of 2-methyl aziridine to immobilize a —CONHCH 2 CH(CH 3 )SCH 2 CH 2 SH ligand on the membrane. The free SH group was then blocked with a methanol solution containing methyl iodide and sodium carbonate. After the membrane was dried, it was tested for ion complexation properties as shown in Example 17.
EXAMPLE 6
[0041] In this example, a crown ether containing ligand was prepared and attached to a membrane according to the following procedure. The acid chloride form of the carboxylic acid group containing PTFE composite membrane was prepared as in Example 1. The crown was prepared for attachment by taking 2 g of allyloxymethyl-8-crown-6 and dissolving it in either dichloromethane or benzene. The double bond of the allyl group was then converted into the epoxide by adding hydrogen peroxide (1 to 2 small drops of a 30% solution) to the stirring mixture. Ammonium hydroxide (0.2 g) was then added to the epoxidized crown and the temperature was raised to between 30° C. and 60° C. The reaction was allowed to proceed for 6-14 hours to form a ligand comprising 18-crown-6 containing a —CH 2 OCH 2 CH(OH)CH 2 NH 2 grouping. This ligand-containing reaction mixture was added to a toluene solution containing the membrane. This procedure resulted in the 18-crown-6 being attached via an amide linkage and can also be used to attach a wide variety of other macrocyclic compounds, or starting materials containing double bonds. After the membrane was dried, it was tested for ion complexation properties as shown in Example 18.
EXAMPLE 7
[0042] In this example, an aminophosphonic acid-containing ligand derivatized membrane was prepared according to the following procedure. A 3×3 inch square of carboxylic acid group containing PTFE composite membrane was treated with thionyl chloride and ethylene diamine as in Example 4. The resulting amino-amide was further reacted by placing the membrane into a 3-necked round bottom flask containing 83 ml concentrated HCl, 83 ml water, and 70 g of phosphorous acid. The mixture was heated to reflux, and 270 ml of formaldehyde was slowly added over a period of 1 hour. The mixture was refluxed for 1 to 4 additional hours resulting in a ligand attached via an amide linkage comprising the grouping CONHCH 2 CH 2 N (CH 2 PO (OH 2 ) 2 . This product was washed with water, and dried. This product was then tested for its ion complexation properties as shown in Example 19.
EXAMPLE 8
[0043] In this example, the procedure of Example 7 was followed with the exception that pentaethylenehexamine was substituted for ethylene diamine, with the volumes of reagents being adjusted in accordance with this substitution. This results in a ligand comprising the grouping —CONH(CH 2 CH 2 NH) 5 CH 2 PO(OH) 2 . This product was then tested for its ion complexation properties as shown in Example 20.
EXAMPLE 9
[0044] In this example, a nitrogen-containing ligand derivatized membrane was prepared according to the following procedure. A 3×3 inch piece of PTFE composite membrane with carboxylic acid groups on the surface according to Example 1 was converted to the acid chloride form and reacted with tetraaza-12-crown-4 in toluene with the resultant formation of an amide bond between one of the ring nitrogen atoms and the acid chloride. The resulting membrane was washed 4 times with toluene and then treated with concentrated HCl, phosphorous acid, and formaldehyde as in Example 7 to produce a membrane with a macrocyclic aminoalkylphosphonic pendent group. This material was then tested for ion complexing properties as shown in Example 21.
EXAMPLE 10
[0045] In this example, an aminocarboxylic acid-containing membrane was prepared according to the following procedure. The material was prepared as in Example 7 up to the point of having ethylene diamine attached to the surface via an amide linkage. This material was further reacted by placing the membrane into a flask containing 200 ml dimethylformamide (DMF), 0.1 g dimethylaminopyridine (DMAP), 25 ml pyridine, and 1 g or diethylenetriaminepentaacetic acid (DTPA) dianhydride. The mixture was allowed to react at 80° C. for 24-72 hours. The final product was washed with water, dried, and tested for ion binding properties as shown in Example 22.
EXAMPLE 11
[0046] In this example, a nitrogen-containing cryptand was attached to a carboxylic acid group containing PTFE composite membrane according to the following procedure. The procedure for producing a membrane with cryptand 2.2.2 attached thereto was identical to the procedure used in Example 6 except that allyloxymethyl-cryptand-2.2.2 was used in place of 18-crown-6. After the membrane was dried, it was tested for ion complexation properties as shown in Example 23.
EXAMPLE 12
[0047] In this example, a nitrogen-containing crown was attached to a membrane according to the following procedure. An acid chloride form of the carboxylic acid group containing PTFE composite membrane was prepared as in Example 1. Hexaza-18-crown-6 dissolved in toluene was then allowed to react with the membrane for 8-14 hours as in Example 9. The membrane was washed with toluene and dried before testing the ion removal properties as shown in Example 24.
EXAMPLE 13
[0048] In this example, an ultra-high molecular weight polyethylene (UPE) membrane was coated with “NAFION” by a precipitated crystal technique to yield a membrane having sulfonic acid reactive groups on the surface, and then a nitrogen-containing ligand-derivatized membrane was prepared.
[0049] Pieces (2×12 inches, 3×3 inches, or 2.75 cm diameter discs) of UPE membrane were rinsed three times each with 150 ml of HPLC grade isopropanol and then three time each with 150 ml of HPLC grade methanol. The membranes were then air dried until they reach a constant weight. The membranes were then pre-wet in methanol and soaked in 50 ml of “NAFION” Solution (sulfonic acid or sodium sulfonate of perfluorinated polyether ion exchange powder in lower aliphatic alcohols and 10% water, 5 wt. % solution, Aldrich Chemical Co.) for about 5 minutes. The “NAFION” Solution was then decanted and the membranes were bathed in methylene chloride. The membranes were then rinsed three times each in 150 ml of methylene chloride, air dried for 2 hours, and dried under vacuum overnight (15 hours).
[0050] The sulfonic acid groups on the membrane were converted to the sulfonyl chloride form by reaction with phosphorus pentachloride, analogous to forming an acid chloride from a carboxylic acid as in Example 1, to result in an activated membrane. Thus, a 2×12 inch, 3×3 inch, or 2.75 cm diameter piece of “NAFION”-coated UPE membrane was immersed in enough phosphorus pentachloride solution to completely cover the surface of the membrane. The membrane remained immersed for 8-14 hours to enable the phosphorus pentachloride to convert the sulfonic acid groups to sulfonyl chloride groups. This activated membrane containing sulfonyl chloride groups was then removed from the phosphorus pentachloride solution and washed thoroughly in hexane or toluene. The activated membrane was then placed in a flask containing a solution of 3 g of pentaethylenehexamine ligand and enough toluene to ensure complete coverage of the membrane. This mixture was allowed to react for 8-14 hours to form a sulfonamide bond between one of the amine groups of the ligand and a sulfonyl chloride group of the activated membrane. The membrane was again washed with organic solvent to remove unbound ligand and permitted to air dry.
[0051] Other ligand derivatized membranes can also be prepared by following the above guidelines. Also ligands may be attached to sulfonic acid derivatized membranes in the manner described above through the formation of sulfonamide or sulfonate ester bonds.
[0052] Metal Ion Recovery and Concentration
[0053] The metal ion recovery and concentration process of the invention relates to the selective recovery of selected metal ions from mixtures thereof with other metal ions using the compositions of the invention as defined above. Effective methods of recovery and/or separation of metal ions from culinary water supplies, high purity fluids, waste solutions, deposits and industrial solutions and metal recovery from waste solutions, e.g., from emulsions on photographic and X-ray films, represent a real need in modern technology. These ions are typically present at low concentrations in solutions containing other ions at such greater concentrations. Hence, there is a real need for a process to selectively recover and concentrate these undesirable hazardous and/or desirable ions. The present invention accomplishes this separation effectively and efficiently by the use of ligands bonded to membranes in accordance with the present invention.
[0054] The general method for selectively recovering and concentrating metal ions from solutions of mixed ions involves complexing selected ions in a source solution with a composition of the present invention and then breaking the complex to liberate the complexed ions and dissolving the liberated ions in a receiving liquid in a much smaller volume than the volume of the source solution. As used herein, “source solution,” “loading solution,” and the like means a solution containing a mixture of an ion or ions that are selected to be concentrated, separated, and/or recovered together with other ions and complexing or chemical agents that are not selected to be removed but which are present in much greater concentrations in the solution. As used herein, “receiving solution,” “stripping solution,” “elution solution,” “eluant,” and the like means an aqueous solution that has greater affinity for the ions that are to be concentrated, separated, and/or recovered, or in which such ions are soluble. In either event, the selected ions are quantitatively stripped from the ligand in concentrated form in the receiving solution, because the receiving solution will ordinarily have a much smaller volume than the source solution.
[0055] The method of using the membrane/ligand compositions of the present invention for separating selected ions from solutions will be apparent to those skilled in the art upon examination of the following illustrative examples.
EXAMPLE 14
[0056] A 0.2 g sheet of the membrane of Example 1 was placed in a beaker containing 25 ml of 5×10 −4 M CuCl 2 in 1 M sodium acetate and 0.1 M acetic acid (pH=5.5). The membrane was contacted with this source solution for 120 minutes. The membrane was then removed from the source solution, rinsed with water, and placed in 5 ml of receiving solution consisting of 1 M HCl.
[0057] The source and receiving solutions were analyzed before and after contact with the membrane for copper and sodium using flame atomic absorption (AA) spectroscopy. Initially, the source solution contained 23 g/l sodium and 31 ppm copper, but after contact with the membrane it contained 23 g/l sodium and about 1 ppm copper.
[0058] The receiving solution initially contained copper and sodium levels below the level of detection, but after contact with the membrane contained an undetectable amount of sodium and 154 ppm copper. This example shows that the membrane-ligand separation was highly selective for copper over sodium, that copper was readily removed from the source solution by contact with the membrane, and that the copper ions could be recovered in a small volume of receiving solution. It is expected that concentration of copper ions in the receiving solution would be even greater when larger volumes of source solution and larger membranes are used.
EXAMPLE 15
[0059] A 0.2 g sheet of the membrane of Example 3 was placed in a beaker containing 25 ml of 5×10 −4 M Hg(NO 3 ) 2 , 1.0 M Ca(NO 3 ) 2 , and 0.5 M NaNO 3 . The membrane was contacted with this source solution for 120 minutes. The membrane was then removed from the source solution, rinsed with water, and placed in 5 ml of a receiving solution consisting of 0.5 M thiourea, 0.1 M HNO 3 .
[0060] The source and receiving solutions were analyzed before and after contact with the membrane for the presence of mercury using inductively coupled plasma (ICP) spectroscopy and for the presence of calcium and sodium using flame atomic absorption (AA) spectroscopy. Initially, the source solution contained 4 g/l calcium, 12.5 g/l sodium, and 101 ppm mercury. After contact with the membrane, the source solution contained 4 g/l calcium, 12.5 g/l sodium, and <1 ppm mercury.
[0061] The receiving solution initially contained calcium, sodium, and mercury levels below the level of detection. After contact with the membrane, this solution contained calcium and sodium at levels below the level of detection and mercury at 505 ppm. Thus, mercury was separated from the source solution also containing sodium and calcium with a high degree of selectivity. The mercury was readily removed from the source solution containing a mixture of ions, and the mercury was recovered and concentrated by elution in a simple receiving solution. As with Example 14, it is expected that the concentration factor can be improved with a system operating on a larger scale, particularly with the membrane engineered in cartridge form.
EXAMPLE 16
[0062] A 0.2 g sheet of the membrane of Example 4 was placed in a beaker containing 25 ml of 5×10 −4 M AgNO 3 , 1.0 M Fe(NO 3 ) 3 , and 0.1 M NaNO 3 . The membrane was contacted with this source solution for 120 minutes. The membrane was then removed from the source solution, rinsed with water, and placed in 5 ml of a receiving solution consisting of 6 M HCl.
[0063] The source and receiving solutions were analyzed before and after contact with the membrane for the presence of silver, iron, and sodium using flame AA spectroscopy. Initially, the source solution contained 5.6 g/l iron, 12.5 g/l sodium, and 54 ppm silver. After contact with the membrane, the source solution contained 5.6 g/l iron, 12.5 g/l sodium, and <1 ppm silver.
[0064] The receiving solution initially contained iron, sodium, and silver levels below the level of detection. After contact with the membrane, however, the receiving solution contained undetectable levels of iron and sodium and 265 ppm silver. The membrane-ligand combination was highly selective for removing silver ions from a source solution of mixed ions. The silver ions thus could be recovered and concentrated in purified form.
EXAMPLE 17
[0065] A 0.2 g sheet of the membrane of Example 5 was placed in a beaker containing 25 ml of 5×10 −4 M PdCl 2 in 6 M HCl, 0.1 M NiCl 2 , 0.1 M FeCl 3 , and 0.1 M ZnCl 2 . The membrane was contacted with this source solution for 120 minutes. The membrane was then removed from the source solution, rinsed in water, and placed in 5 ml of a receiving solution consisting of 2 M NH 3 and 1 M HCl.
[0066] The source and receiving solutions were analyzed before and after contact with the membrane for palladium, nickel, and zinc using ICP spectroscopy. Initially, the source solution contained 5.9 g/l nickel, 5.6 g/l iron, 6.5 g/l zinc, and 52 ppm palladium. After contact with the membrane, the source solution contained 5.9 g/l nickel, 5.6 g/l iron, 6.5 g/l zinc, and <1 ppm palladium.
[0067] The receiving solution initially contained nickel, iron, zinc, and palladium at levels below the level of detection. After contact with the membrane, however, the receiving solution contained undetectable levels of nickel, iron, and zinc, but contained 262 ppm palladium. Thus, the membrane-ligand combination was highly selective for binding palladium ions from a source solution containing a mixture of ions, and permitted removal, purification, and recovery of the palladium ions.
EXAMPLE 18
[0068] A 0.2 g sheet of the membrane of Example 6 was placed in a beaker containing 25 ml of 5×10 −4 M Pb(NO 3 ) 2 in 1 mM HNO 3 , 0.1 M Mg(NO 3 ) 2 , and 0.1 M Ca(NO 3 ) 2 . The membrane was contacted with this source solution for 120 minutes. The membrane was then removed from the source solution, rinsed with water, and placed in 5 ml of a receiving solution consisting of 0.03 M tetrasodium EDTA.
[0069] The source and receiving solutions were analyzed before and after contact with the membrane for the presence of lead, magnesium, and calcium using flame AA spectroscopy. Initially, the source solution contained 2.4 g/l magnesium, 4.0 g/l calcium, and 102 ppm lead. After contact with the membrane, the source solution contained 2.4 g/l magnesium, 4.0 g/l calcium, and about 2 ppm lead.
[0070] The receiving solution initially contained magnesium, calcium, and lead at levels below the level of detection. After contact with the membrane, the receiving solution contained undetectable levels of magnesium and calcium and 495 ppm lead. Thus, the membrane-ligand combination was highly selective in removing lead ions from a source solution containing a mixture or ions and permitted recovery and concentration of relatively pure lead.
EXAMPLE 19
[0071] A 0.2 g sheet of the membrane of Example 7 was placed in a beaker containing 25 ml of 5×10 −4 M Sb in 2 M H 2 SO 4 , 0.3 M CuSO 4 , and 0.1 M NiSO 4 . The membrane was contacted with this source solution for 120 minutes. The membrane was then removed from the source solution, rinsed in water, and placed in 5 ml of a receiving solution consisting of 6 M HCl.
[0072] The source and receiving solutions were analyzed before and after contact with the membrane for copper, nickel, and antimony using flame AA spectroscopy. Initially, the source solution contained 5.9 g/l nickel, 19 g/l copper, and 56 ppm antimony. After contact with the membrane, the source solution contained 5.9 g/l nickel, 19 g/l copper, and <5 ppm antimony.
[0073] The receiving solution initially contained nickel, copper, and antimony at levels below the level of detection. After contact with the membrane, however, the receiving solution contained undetectable levels of nickel and copper, but contained 285 ppm antimony. Thus, the membrane-ligand combination was selective for binding antimony from a source solution containing a mixture of ions, and permitted removal, purification, and recovery of the antimony.
EXAMPLE 20
[0074] A 0.2 g sheet of the membrane of Example 8 was placed in a beaker containing 25 ml of 5 ppm iron, 5 ppm lead, 5 ppm copper, 5 ppm nickel, and 5 ppm zinc in tap water. Tap water contains relatively high concentrations of sodium, potassium, calcium, and magnesium ions. The membrane was contacted with this source solution for 240 minutes. The membrane was then removed from the source solution, rinsed in water, and placed in 5 ml of a receiving solution consisting of 6 M HCl.
[0075] The source and receiving solutions were analyzed before and after contact with the membrane for iron, nickel, and zinc using ICP spectroscopy and for copper and lead using flame AA spectroscopy. Initially, the source solution contained the levels of each metal as mentioned above. After contact with the membrane, the source solution contained <1 ppm of each of the metals.
[0076] The receiving solution initially contained iron, lead, nickel, copper, and zinc at levels below the level of detection. After contact with the membrane, however, the receiving solution contained 25 ppm nickel, 25 ppm copper, 24 ppm iron, 26 ppm lead, and 26 ppm zinc. Thus, the membrane-ligand combination readily removed iron, lead, copper, nickel, and zinc from a source solution containing a mixture of ions despite the presence of sodium, potassium, calcium, and magnesium ions in the source solution.
EXAMPLE 21
[0077] A 0.2 g sheet of the membrane of Example 9 was placed in a beaker containing 25 ml of 200 ppb iron in 1% HF. The membrane was contacted with this source solution for 480 minutes. The membrane was than removed from the source solution, rinsed in water, and placed in 5 ml of a receiving solution consisting of 37% HCl.
[0078] The source and receiving solutions were analyzed before and after contact with the membrane for iron using graphite furnace AA spectroscopy. Initially, the source solution contained 200 ppb iron. After contact with the membrane, the source solution contained 10 ppb iron.
[0079] The receiving solution initially contained iron at a level below the level of detection. After contact with the membrane, however, the receiving solution contained 910 ppb iron. Thus, the membrane-ligand combination readily removed iron from the source solution despite the very low level of iron in the source solution and the presence of both acid and the strongly iron-chelating fluoride.
EXAMPLE 22
[0080] A 0.2 g sheet of the membrane of Example 10 was placed in a beaker containing 25 ml of 10 ppm iron, 10 ppm copper, and 10 ppm nickel in 0.5 M HP and 0.5 M NaF. The membrane was contacted with this source solution for 240 minutes. The membrane was then removed from the source solution, rinsed in water, and placed in 5 ml of a receiving solution consisting of 3 M HCl.
[0081] The source and receiving solutions were analyzed before and after contact with the membrane for iron and nickel using ICP spectroscopy and for copper using flame AA spectroscopy. Initially, the source solution contained 10 ppm each of iron, copper, and nickel. After contact with the membrane, the source solution contained <1 ppm of each of the three metals.
[0082] The receiving solution initially contained iron, copper, nickel, and sodium at levels below the level of detection. After contact with the membrane, however, the receiving solution contained sodium at a level below the level of detection and 50 ppm each of iron, copper, and nickel. Thus, the membrane-ligand combination readily removed iron, copper, and nickel from the source solution, and these three metals could be separated from the source solution and recovered.
EXAMPLE 23
[0083] A 0.2 a sheet of the membrane of example 11 was placed in a beaker containing 25 ml of 5 ppm potassium in deionized distilled water at pH 8. The membrane was contacted with this source solution for 120 minutes. The membrane was then removed from the source solution, rinsed in water, and placed in 5 ml of a receiving solution consisting of 0.1 M HCl.
[0084] The source and receiving solutions were analyzed before and after contact with the membrane for potassium using flame AA spectroscopy. Initially, the source solution contained 15 ppm potassium, but after contact with the membrane it contained <1 ppm of potassium.
[0085] The receiving solution contained potassium at a level below the level of detection, but after contact with the membrane contained 75 ppm potassium. Thus, potassium could be readily removed from the source solution by binding to the membrane and recovered by elution in a receiving solution.
EXAMPLE 24
[0086] A 0.2 g sheet of the membrane of example 12 was placed in a beaker containing 25 ml of 5 ppm of each of lead, cadmium, mercury, copper, and nickel in tap water. The membrane was contacted with this source solution for 480 minutes. The membrane was then removed from the source solution, rinsed with water, and placed in 5 ml of a receiving solution consisting of 6 M HCl.
[0087] The source and receiving solutions were analyzed before and after contact with the membrane for mercury, cadmium, and nickel using ICP spectroscopy, and for lead, copper and mercury using flame AA spectroscopy. Initially, the source solution contained 5 ppm of each of lead, cadmium, mercury, copper, and nickel, but after contact with the membrane it contained <1 ppm of each of these elements.
[0088] The receiving solution initially contained lead, cadmium, mercury, copper, and nickel at levels below the level of detection. After contact with the membrane, however, the receiving solution contained 25 ppm of each of the elements. Hence, lead, cadmium, mercury, copper, and nickel were all readily removed from a source solution also containing sodium, potassium, calcium, and magnesium. Further, all of the elements removed from the solution by adsorption to the membrane were recovered and concentrated in the receiving solution.
EXAMPLE 25
[0089] A 0.04 g sheet (2.75 cm diameter disc) of the membrane of Example 13 was placed in a membrane holder (O-ring and clams). This arrangement allowed for a 1.83 cm diameter portion of the disc to be in contact with a solution flowing through the membrane. A 5 ml source solution containing 6 ppm Cu in 1 M Zn(NO 3 ) 2 , 0.1 M sodium acetate, and 0.01 M acetic acid was passed through the membrane using vacuum suction from a vacuum pump at a flow rate of 1 ml/min. The membrane was then washed by flowing 2 ml of 1 M NH 4 Cl through the membrane at 1 ml/min. Next, 3 ml of a receiving solution comprising 0.5 M HCl was passed through the membrane at a flow rate of 2 ml/min.
[0090] The source and receiving solutions were analyzed before and after they were passed through the membrane for copper, zinc, and sodium using flame atomic absorption spectroscopy. Initially, the source solution contained 6 ppm Cu, 65 g/l Zn, and 2.3 g/l Na. After contact with the membrane, the Zn and Na levels in the source solution were unchanged, and the Cu level was 2 ppm.
[0091] The receiving solution initially contained Cu, Zn, and Na at levels below the level of detection. After passing through the membrane, however, the receiving solution contained undetectable levels of Zn and Na, but contained 10 ppm Cu. Thus, the membrane-ligand combination was highly selective for the Cu at low levels in a source solution containing concentrated Zn and Na.
[0092] From the foregoing, it will be appreciated that the ligand-membrane compositions of the present invention provide a material useful for separation, recovery, and concentration of selected metal ions from mixtures of those ions with other ions, even when those other ions are in far greater concentrations. The recovered metals can then be analyzed or further concentrated from the receiving solution by standard techniques known in the technology of these materials.
[0093] Although the process of separating and concentrating certain metal ions in this invention has been described and illustrated by reference to certain specific membrane-bound ligands, processes using analogs of these ligands are within the scope of the processes of the invention as defined in the following claims. | A method for removing, separating, and concentrating certain selected ions from a source solution that may contain larger concentrations of other ions comprises bringing the source solution in contact with a composition comprising an ion-binding ligand covalently bonded to a membrane having hydrophilic surface properties. The ligand portion of the composition has affinity for and forms a complex with the selected ions, thereby removing them from the source solution. The selected ions are then removed from the composition through contact with a much smaller volume of a receiving solution in which the selected ions are either soluble or which has greater affinity for the selected ions than does the ligand portion of the composition, thereby quantitatively stripping the complexed ions from the ligand and recovering them in concentrated form in the receiving solution. The concentrated ions thus removed may be further separated and recovered by known methods. The process if useful in the removal of selected ions, including noble metals and other transition metals from a variety of source solutions such as are encountered in semiconductor, nuclear waste cleanup, metals refining, environmental cleanup, providing ultra high purity fluids, electric power, and other industrial enterprises. The invention is also drawn to the ligand-membrane compositions. | 8 |
FIELD OF THE INVENTION
The invention describes improvements in the commercial-scale processing of nickel and cobalt containing laterite ores for the recovery of these metals, by reacting such ores with sulphuric acid at elevated temperatures and pressures
BACKGROUND OF THE INVENTION
For over a century, nickel laterite ores high in magnesia, relatively low in iron, and enriched in nickel, commonly referred to as garnierite ores or saprolite ores, have been processed by pyrometallurgical means to produce either a ferronickel, a Class II nickel product that could go directly to market for the production of stainless steels, or to produce an intermediate sulphide “matte” product that could go to refineries for conversion to either Class I or Class II nickel products. A good portion of the cobalt would be lost, some in the slag during the smelting stage, and in the case of ferronickel most of the cobalt would be present as a product impurity of no value. Such pyrometallurgical processes involve drying the humid ores, preheating them with or without effecting a partial reduction, and subsequent reduction smelting at high temperatures in electric furnaces. It is axiomatic that such pyrometallurgical processes consume high amounts of energy per unit of nickel production, and in most cases result in complete loss of value of the cobalt that accompanied the nickel in the ore.
About half a century ago, an ammoniacal leaching process was developed and commercialized which could treat laterite ore relatively high in iron and of lower nickel content than the garnierites and saprolites. It employed a combination of pyrometallurgical and hydrometallurgical technologies. The laterite ore is first dried and then subjected to partial reduction in Herreschoff furnaces or rotary kilns, at elevated temperatures but well below smelting temperatures, to selectively reduce the nickel and cobalt but only partially reduce the iron. This partially reduced calcine is then quenched and leached in ammoniacal carbonate solutions to dissolve nickel and cobalt; and the nickel is subsequently recovered from the ammoniacal leach solution as a nickel hydroxide/carbonate which would then be converted to a Class II nickel oxide or to utility-grade nickel. In some cases the nickel solutions would proceed to electrolytic refining for the production of refined nickel. Nickel extractions seldom exceed 80% and cobalt extractions seldom exceed 45%. While this hybrid pyrometallurgical-hydrometallurgical process could treat the high-iron, low-magnesia and low-nickel laterite ores, often referred to as limonite ores, and is less demanding of energy than the smelting process, in actual continuous practice, the nickel recoveries often fall below 75% and cobalt recoveries below 40%.
Research in the early 1950's demonstrated that by subjecting the high-iron, low-magnesium and low-nickel laterite ores, that is the limonites, also containing significant quantities of cobalt, directly in their humid state to sulphuric acid at elevated temperatures and pressures, that nickel and cobalt extractions of over 90% could be achieved with the energy requirement only a fraction of that required by the smelting or ammoniacal leaching processes. While this technology heralded a new era for the production of nickel and cobalt, only one commercial plant was built at Moa Bay in Cuba. This plant confined itself to the processing of limonites very low in magnesia content, i.e., with less than 1% magnesium oxide, and operated at around 240° C. and 475 psig. The plant which is in operation today, employs pachuca-type autoclaves which rely on the process steam to provide both the heat requirement and the agitation which is inadequate and promotes build-up inside these autoclaves which in turn necessitates frequent shutdowns for cleanouts. The product of the Moa Bay plant is an intermediate nickel-cobalt sulphide, which is sent overseas for refining to marketable nickel and cobalt end products.
The value of this new hydrometallurgical technology that could treat humid ores directly without drying and which yields impressively high extractions of nickel and cobalt, became more and more appreciated as a result of the energy crises of the 1970's and 1980's and as a need grew for new sources for cobalt outside of Zaire and Zambia whose production had dropped off drastically. At the same time, the development and demonstrated success of large-scale mechanically-agitated compartmentalized autoclaves in other industries such as the gold industry, gave added interest for application of such reactors to the processing of nickel-cobalt laterites. In such reactors, the requirement for process steam and for agitation are managed and adjusted independently one of the other. Furthermore, extensive research developmental work carried out by P. C. Duyvesteyn, G. R, Wicker, R. E. Doane of Amax Extractive & Development Inc. “An Omnivorous Process for Laterite Deposits”, International Laterite Symposium, Evans, Shoemaker, Veltman Eds., TMS-AIME, Kingsport Press, Kingsport Tenn., 1979, demonstrated that enhanced results could be realized at somewhat higher temperatures of around 270° C. and corresponding pressures of around 800 psia; and that this new technology employing mechanically-agitated reactors need not limit itself to the very low-magnesia laterite ores, but could be applied to ores containing several percent of magnesia. Of course, acid requirements increase significantly as the magnesia increases as does the requirements for neutralizing agents. The greatest impetus to proceed with this new technology comes from engineering and economic analyses which indicate that hydrometallurgical process plants could be constructed at a capital cost per unit of annual nickel and cobalt production substantially below that of the established conventional processes and would yield a unit cost of production which permits economic treatment of limonites with as little as 1% of nickel, material that up until now had been considered as overburden and uneconomical to process, i.e., material that previously could not be classified as ore. This has led to the construction of three separate acid pressure leaching plants in Australia, with commissioning in 1999/2000.
U.S. Pat. No. 4,541,994, 1985, assigned to Lowenhaupt et al. speaks of reacting “coarse, magnesium rich fractions” with partially neutralized pregnant liquors produced by high pressure leaching, at lower pressures, and claims carrying out of such reactions “at a pressure of from atmospheric to about 300 psig”, also “wherein said pressure is atmospheric and said temperature is below 80° C.”, also “wherein said temperature is about 60° C.”, and also “wherein said temperature is ambient”. Their atmospheric leach tests Nos. 7, 8, 9 and 10 at 80° C., for example, demonstrated that nickel and cobalt tend to be upgraded in the fine fractions and magnesium in the coarse fractions. In these tests, the Mg:Ni ratio in the +200 mesh size in relation to the Mg:Ni ratio in the −200 mesh averaged 2:1; and the Mg:Co ratio in the +200 mesh size in relation to the Mg:Co ratio in the −200 mesh size averaged 2.1:1. Only the −200 mesh size would proceed to acid pressure leaching. While less acid would thus be required per unit of nickel and cobalt to yield high extractions in the pressure leach, overall nickel and cobalt recoveries would be greatly decreased.
Currently, in preparation for the pressure leaching, the humid predominantly limonitic laterite ores are pulped with substantial quantities of calcium-free water either from a “fresh” water source or with de-ionized saline water, to a pulp density usually under about 40% solids; and excess acid is added to the autoclaves to effect the desired leaching in 60 minutes or less, when employing reaction temperatures of up to 270° C.
It is well understood and appreciated by those familiar with acid pressure leaching of laterite ores, that the pH of acidic leaching solutions is different at elevated temperatures than at temperatures below 100° C.; and that the solubility of metals such as nickel, cobalt, manganese, and magnesium drops off drastically at temperatures above about 150° C. Accordingly, sulphuric acid well in excess of that theoretically required to sulphate the desired metals must be employed to maintain an adequate level of acidity at the elevated reaction temperatures, as well as to enhance the kinetics of the sulphating reactions. The net result is that the leachate emanating from the autoclaves after being cooled and de-pressurized, can contain as much as 30 grams per liter to as much as 50 grams per liter of free sulphuric acid.
Typically, with low-magnesia limonite ores the sulphuric acid addition to the feed is about 30% by weight of the ore (on a dry weight basis); and the free acid in the leachate could represent at least 25% and as much as 40% of the initial acid addition under certain operating conditions. Before proceeding to recovery of the nickel and cobalt from the leachate by any of the conventional means of precipitation with hydrogen sulphide or by more-recently developed solvent-extraction or ion-exchange technologies, or by precipitation by more common basic neutralization agents such as magnesia or sodium oxides or carbonates, it is usual to carry out a preliminary partial neutralization with limestone to a pH of 3.5 to 4.5 in order to neutralize the bulk, that is over 95%, of the free acid and to precipitate most of the ferric iron. At this stage the partially neutralized leachate would be virtually saturated with calcium sulphate. The overall impact of this partial neutralization technique is that a significant tonnage of excess acid is wasted, a significant tonnage of extra limestone is required to neutralize the excess acid, the partially-neutralized pregnant solution is saturated with calcium sulphate, following metal recovery the barren solution cannot be recycled to preparation of new feed for the autoclaves, and substantial quantities of process effluent needs to be discharged to the external environment after final neutralization to lower the concentrations of base metal contaminants.
As already stated, one of the basic tonnage materials required to carry out acid pressure leaching, besides the ore and sulphuric acid, is water. It is necessary to pulp and dilute the ore feed to about 40% solids or lower. It is highly desirable, and in most cases essential, that this make-up water be free of calcium so as to avoid problems that could arise from calcium sulphate precipitation particularly in the preheating system at the feed end of the pressure system autoclaves. Thus, commercial installations rely on fresh water sources if such are available, or arrange for de-ionization of saline waters. The tonnage of calcium-free water required is very large, usually in the order of a tonne of water for every tonne of raw humid laterite ore. While adequate quantities of fresh water may be available for initial demonstration plants, it is unlikely that there would be enough available for any large-scale operations and expansions. Furthermore, there is a serious environmental consideration in that every tonne of fresh water taken into the process usually results in a comparable tonnage of process water that must be discarded eventually to the sea, and which could carry certain quantities, albeit minute quantities, of base metals and other contaminating elements.
SUMMARY OF THE INVENTION
It is an object of the present invention to provide a process of hydrometallurgical treatment of laterite ores of the limonitic type for the recovery of nickel and cobalt which reduces the amount of fresh water needed for pulping the feedstock and the amount of sulphuric acid used in the chemical leaching step.
In the improved method of the present invention, a significant portion of the “mother liquor” emanating from the autoclaves is recycled to the feed preparation stage thereby substituting for all or at least a major proportion of the fresh water or de-ionized water that must be added and also supplying a portion of the amount of sulphuric acid that is required for leaching. Concomitantly with the major savings in fresh water or de-ionized water requirements, a significant reduction in new sulphuric acid requirements is effected along with a corresponding saving in limestone and lime required for subsequent neutralizations. A further benefit results from the fact that less process waters need to be expelled to the external environment Thus, several significant processing advantages and benefits are simultaneously realized.
The present invention provides a process of leaching a nickel and cobalt containing predominantly limonitic portion of a laterite ore profile, comprising the steps of:
a) preparing a feedstock of a predominantly limonitic portion of a laterite ore containing nickel and cobalt;
b) pulping said feedstock with a liquid to produce a pulped ore;
c) adding an effective amount of sulphuric acid to the pulped ore to produce a sulphuric acid solution, agitating and leaching said feedstock in said sulphuric acid solution at an elevated temperature under pressure for a selected period of time whereby metal oxides are leached from said ore to produce a leach pulp;
d) separating said leach pulp into a mother liquor solution and a first thickened leach pulp, wherein said liquid used to pulp said feedstock in step b) includes a selected amount of said mother liquor solution; and
e) recovering nickel and cobalt products from said first thickened leach pulp.
In a variation of the present invention, acid efficiency may be further increased by reacting the first thickened leach pulp with highly-serpentinized, high-magnesia nickel saprolite ore, at atmospheric pressure and preferably above 90° C. and below 100° C., to achieve partial neutralization of the excess acid before it passes on to further neutralization with limestone and subsequently passing on to a decantation step (preferably using counter-current decantation) for solids-liquid separation and recovery of a clarified pregnant solution containing the nickel and cobalt values originating from both the limonitic ores treated at high temperatures and pressures and the highly-serpentinized saprolitic ores treated subsequently by atmospheric leaching.
In a further variation of the present invention, additional advantages are realized by completely eliminating the requirement for limestone and lime by carrying out preliminary partial neutralizations firstly with a highly-serpentinized high-magnesia saprolite ore and subsequently by the use of magnesite, MgCO 3 or magnesia, MgO before passing onto solid-liquid separation and recovery of the clarified pregnant solution. The saprolite ore contributes nickel and a lesser amount of cobalt units and reduces substantially the quantity of the other neutralizing agents that would otherwise be required. When producing an intermediate nickel-cobalt product, final neutralization could be effected by any non-calcium basic oxides such as magnesia, or sodium-based oxides, carbonates or hydroxides. The metal values could alternatively be precipitated with H 2 S or sodium sulphide compounds; or could be recovered by either solvent extraction means or with chelating resins.
BRIEF DESCRIPTION OF THE DRAWINGS
The process for acid leaching of nickel and cobalt containing laterite ores in accordance with the present invention will now be described, by way of example only, reference being had to the accompanying drawings, in which:
FIG. 1 is a flowchart showing the steps common to most of the prior art pressure acid leaching processes for extracting nickel and cobalt from laterite ores;
FIG. 2 shows a flowchart showing the steps of the process of acid leaching nickel and cobalt containing laterite ores according to the present invention;
FIG. 3 shows a flowchart illustrating an alternative embodiment of the process of the present invention; and
FIG. 4 is a plot of pH versus time showing the atmospheric partial neutralization of leach pulp from pressure leaching of limonite ore using highly-serpentinized saprolitic ore.
DETAILED DESCRIPTION OF THE INVENTION
Sulphuric acid is being used in the hydrometallurgical treatment of laterite ores of the limonitic type for the recovery of nickel and cobalt. More particularly, the prior art process of acid pressure leaching of high-iron limonitic-type laterites, as shown schematically in FIG. 1, is very efficient in extracting both the nickel and the cobalt at levels above 90%; but requires large quantities of sulphuric acid including a significant proportion of excess acid plus large quantities of limestone for subsequent neutralization. The raw limonitic ore can contain 40% or more of free moisture in its natural state. However additional water needs to be added for pulping the ore to a pulp density usually under about 40% solids and preferably in the range of 30% to 40% solids, depending on whether the preheating of the feed pulp is by indirect or by direct heat exchange with the steam produced in the pressure letdown system, in preparation for pressure leaching. Accordingly, there is a large demand for water to make up the liquid phase. In normal practice the water added in feed preparation is fresh water, roughly in the proportion of one tonne of fresh water to one tonne of ore in its natural state. This represents a heavy demand on fresh water supplies. Furthermore, this quantum of water must eventually be treated with lime or some other neutralizing agent to insure removal of base metals prior to discharge to the external environment. In this single pass system, acid efficiency when effecting 95% extraction of the nickel and cobalt is, at best, about 75%, and could be as low as 60%.
The present improved process re-cycles “mother liquor” emanating from the autoclaves back to feed preparation and thereby virtually eliminates the need for fresh water addition at this stage, as depicted in FIG. 2 . The net result is a series of important improvements including: the requirement for fresh water for feed preparation is virtually eliminated; acid efficiency is increased significantly, and acid requirements reduced significantly; limestone requirements are correspondently reduced, significantly; the quantity of process water to be disposed to the external environment is reduced, very substantially; the downstream metal recovery system is reduced in size as the re-cycling yields a pregnant solution of higher nickel and cobalt concentrations; and overall, the unit cash operating costs are favourably impacted, i.e. reduced.
The “leach pulp” is produced by pressure leaching the pulped ore at elevated temperatures in the sulphuric acid solution and therefore, as used herein, the term “leach pulp” refers to the leached ore and solution containing the dissolved metals so that the “leach pulp” comprises both solids and liquids. This solution produced by the pressure leaching is referred to as the “mother liquor” as mentioned above. The liquid used to pulp the feedstock ore is made up of a significant portion of the mother liquor solution produced by the pressure leaching of the pulped ore.
As can be seen by comparing the prior art process shown in the flowchart of FIG. 1 and the process according to the present invention shown in the flowchart of FIG. 2, the main additional equipment required to practice the present invention is a thickener to receive the hot leach pulp emanating from the autoclave(s) in order to separate solids from liquid thereby permitting re-circulation of a portion of the liquid—mother liquor—to the feed preparation step in quantities as determined by process requirements. It should be recognized that the materials of construction accommodating the hot acidic mother liquor must be corrosion resistant metals or alloys. With regard to the disposal of the iron-gypsum precipitate, there are two options: one is to return it to the counter-current-decantation system; and the other is to de-water and wash it in a separate filtration plant.
Referring to FIG. 2, the process of leaching a nickel and cobalt containing predominantly limonitic portion of a laterite ore profile, comprises preparing a feedstock of a predominantly limonitic portion of a laterite ore containing nickel and cobalt by conventional crushing, screening and fine grinding the starting material. The ground ore of which the prepared feedstock is comprised should preferably be essentially all of minus 100 mesh size. The next step in the process is to pulp the prepared feedstock with the liquid to give a pulped ore with a density preferably between about 30% and 40% solids depending on certain other process design parameters. This pulping step may be carried out in a rotating type of vessel similar to a grinding mill but without any grinding medium. Sulphuric acid is then added to the pulped ore in a pressure vessel to produce a sulphuric acid solution, and the solution is agitated at an elevated temperature whereupon leaching of the feedstock in the sulphuric acid solution occurs. The leaching takes place in autoclaves where a certain pressure is established corresponding to the selected elevated temperature which is maintained by the addition of superheated steam. This process is referred to as pressure leaching. After leaching for a selected period of time metal oxides are leached from the ore to produce the leach pulp. The leach pulp is then removed from the pressure vessel and separated into a mother liquor solution and a first thickened leach pulp. A selected amount of the mother liquor solution is then recirculated back to be used for pulping freshly prepared feedstock. Nickel and cobalt are then recovered from the first thickened leach pulp. As can be seen from FIG. 2, the amount of sulphuric acid added to the pulped ore includes sulphuric acid added directly to the pulped ore in addition to unreacted sulphuric acid present in the mother liquor.
The final composition of the liquid used for pulping the prepared feedstock typically includes the water that accompanied the humid ore feed, the mother liquor solution added, as well as any fresh make-water. The degree of re-circulation of mother liquor and the composition of the pulping liquid will be determined in part by the magnesia and nickel contents of the ore feed. Since the solubility of magnesium and nickel are much lower at the high leaching temperatures than at room temperature, the amount of magnesium and nickel in the liquid comprising mother liquor/water must be kept preferably below those which are soluble at the high leaching temperature employed, otherwise there could be significant precipitation of magnesium and nickel salts in the last feed preheating heat exchanger and in the autoclave itself. The undesirability of introducing too much magnesium and nickel into the system is demonstrated in Example 2 discussed hereinafter. The amount of mother liquor present in the pulping liquid is selected so that the dissolved magnesium does not exceed about 12 grams per liter. The conclusion regarding magnesium is supported by research as disclosed in William L. Marshal and Ruth Slusher of the Reactor Chemistry Division, Oak Ridge National Labratory, Tenn. “Solubility and Hydrolytic Instability of Magnesium Sulfate in Sulfuric Acid-Water and Deuterosulfuric Acid-Deuterium Oxides Solutions, 200° to 350° C.”, Journal of Chemical and Engineering Data, Vol. 10, No. Oct. 4, 1965. Regarding nickel, concentrations should be kept below about 15 grams per liter. It can be deduced from research disclosed by William L. Marshall, James S. Gill and Ruth Slusher of the Reactor Chemistry Division, Oak Ridge National Laboratory, Oak Ridge, Tenn., “Aqueous Systems at High Temperature-V 1 , Investigations on the System NiO—SO 3 —H 2 O and its D 2 O Analogue from 10 −4 to 3 m SO 3 , 150-450° C.”, Journal of Inorganic Chemistry, 1962, Vol. 24, pp 889 to 897, Pergamon Press Ltd., that nickel concentrations in the pressure leaching system should be kept below about 18 grams per liter and preferably below about 15 grams per liter.
Once the reacted pulp exits the pressure system and operating temperatures drop below 100° C. the leachate can dissolve appreciable additional quantities of magnesium as well as other metal salts. To take advantage of this fact, a variation of the present invention contemplates reacting the settled first thickened pulp fraction, after solids-liquid separation of the leach pulp to produce the mother liquor, with highly-serpentinized high-magnesia saprolite ore, to effect the first partial neutralization of the excess acid. FIG. 3 illustrates a flowchart showing the steps in this different embodiment of the process. In addition to the extra equipment requirement of the process of FIG. 2, a separate feed preparation facility is required for crushing and comminuting the highly-serpentinized saprolite ore, as well as a separate installation of leaching tanks to carry out atmospheric leaching/partial neutralization. In this flowchart the iron precipitate, the gypsum, the leached tailings produced by pressure leaching the limonite ore and the tailings produced by atmospheric leaching of the saprolite ore all proceed together to the counter-current-decantation system.
In commercial practice, it may be advantageous to add some pregnant solution or some barren solution, to lower the pulp density at this stage. By bringing the pH up to about 2, over 90% of the excess acid will have been neutralized. The next stage of partial neutralization would be effected by the addition of limestone, lime, magnesite or magnesia to bring the pH up to about 4 in order to precipitate and remove the ferric iron. Following the two stages of partial neutralization the leached and partially neutralized pulp passes on to the counter-current-decantation system, as shown in FIG. 3, for the production of a clarified pregnant solution that goes to metals recovery. Final recovery of the nickel into an impure intermediate product can be carried out in a number of different ways as described in FIGS. 2 and 3 and in the Examples.
In selecting the highly-serpentinized variety of saprolite ore, the present invention achieves neutralization of excess acid with the simultaneous high extractions of the nickel and cobalt contents of the saprolite ore in reaction times of less than one hour.
EXAMPLE 1
To demonstrate the main feature of the present invention, two samples of high-iron low-magnesium relatively low-nickel limonitic laterite ores obtained from the southern region of New Caledonia, but relatively rich in cobalt as shown by the ore analyses in Table 1 were pressure leached with sulphuric acid in a two-liter autoclave, in a series of three tests in which the mother liquor from the first leach test obtained after settling and solid-liquid separation, “ML1”, was used to prepare the feed pulp for the second leach test; and the mother liquor from the second leach test obtained after settling and solid-liquid separation, “ML2”, was used to prepare the feed pulp for the third leach test. The leaching conditions are summarized in Table 2. The liquid phase, “ML3”, of the third leached pulp was very much enriched in nickel and cobalt, and the nickel and cobalt extractions were 95% or higher in all cases, as can be seen in Table 3. Nickel extraction was 96.2% and cobalt extraction 97.0% while recycling of mother liquors increased the metal concentrations to 12.3 gpl Ni and 1.9 gpl Co in the final liquor emanating from the autoclave. The third pulp then proceeded to metal recovery. The first treatment was to react it with fine limestone as in conventional commercial practice, as depicted in FIG. 2, to achieve a pH of 4.7, thereby neutralizing over 98% of its residual free acid and precipitating out gypsum and ferric iron as hydroxide. After settling, filtering and washing of the filter cake with dilute sulphuric acid the resulting diluted liquor, which is now to be referred to as the clarified pregnant solution, was ready to move forward to nickel and cobalt recovery.
Several different processes are currently being employed in commercial practice to recover and separate the nickel and cobalt into refined or semi-refined products. In the present example, intermediate nickel-cobalt products were produced by two different precipitation techniques. The pregnant solution was split into two fractions. One fraction was further reacted with lime, CaO, to a pH of 11, thereby precipitating essentially all of the nickel, cobalt and manganese as hydroxides concomitant with the production of a substantial quantity of gypsum. The other fraction was reacted with soda ash, Na 2 CO 3 , to a pH of 9, thereby precipitating essentially all of the nickel, cobalt and manganese. The analyses of the final products are shown in Table 1. An excess of lime was added in the first case, accounting for the lower-than-expected grade in the final product.
Those skilled in the art will appreciate that in the flowscharts depicting the present process in FIGS. 2 and 3, the basic neutralizing agents could be added as finely ground dry products, or as finely ground and pulped products where the pulping liquor could be fresh water, barren solution or pregnant solution, as deemed appropriate.
In continuous commercial operation wherein the feed is preheated by direct heat exchange with live steam from the pressure letdown system, with a limonitic ore feed of about 1.5% Ni, the circulation of mother liquor to the extent that it would supplant 100% of the fresh water required for feed preparation would yield liquor emanating from the autoclaves containing between 14 and 15 gpl of Ni as compared to liquor of between 8 and 9 gpl Ni by conventional use of fresh water alone. Since the free acid contents of these two liquors would be essentially the same, it is calculated that the acid efficiency will have been increased to about 86% % from about 75% % by the re-circulation of mother liquor. Thus, besides drastically reducing fresh water requirements in the overall processing, there is a substantial gain from reducing acid requirement per unit of nickel recovered. Further advantages stem from the fact that lesser quantities of neutralizing agents would be required, the downstream equipment could be downsized with the higher-grade clarified pregnant solution, and the amount of liquid effluent released to the external environment would be drastically reduced.
TABLE 1
Acid pressure leaching of limonite ores
Chemical Composition Wt %
Ni
Co
Mn
Fe
Mg
SiO 2
Al 2 O 3
Cr z O 3
Ores
NC-1
1.45
0.23
1.63
49
0.25
2.3
5.0
2.4
NC-2
1.17
0.21
1.45
49
0.25
2.2
5.1
2.2
Residues
1 st Leach
0.013
0.003
0.24
54
0.14
2.9
3.3
0.1
2 nd Leach
0.047
0.012
0.46
54
0.14
2.7
2.9
0.1
3 rd Leach
0.055
0.007
0.52
56
0.12
2.5
2.9
0.1
Products
CaO ppt
6.5
1.1
5.9
0.0
1.2
0.0
0.0
16
Na 2 CO 3
18.2
2.9
15.7
0.0
2.6
0.0
0.0
3.8
ppt
TABLE 2
Weights of Reactants
Leach Conditions
Ore
Leach
Ore
H 2 O*
H 2 O
“ML”
H 2 SO 4
H 2 SO 4
Pulp
Temp
Press
Time
Sample
No.
g
g
g
g
g
% of Ore
% Solids
° C.
psia
min
NC-2
1 st
360
240
500
—
102
28
30
270
800
30
NC-1
2 nd
360
240
18
500
82
28
30
270
800
30
NC-1
3 rd
360
240
50
490
81
28
30
270
800
30
*This H 2 O represents the H 2 O that would be contained by the raw limonitic feed ore, averaging about 40% H 2 O.
TABLE 3
Acid pressure leaching of limonite ores; Re-circulation of mother liquor;
Nickel and cobalt extractions
% Extractions
Ore
Leach
Rxn Time
Pulping
Solution (gpl)
Sol'n Assay
Residue Assay
Sample
No
min
Medium
Ni
Co
H 2 SO 4
Ni
Co
Ni
Co
NC-2
1 st
00
H 2 O
12
5.01
0.91
97.7
96.7
20
5.05
0.94
98.1
99.2
25
5.06
0.93
98.0
98.2
30
5.11
0.94
50
98.9
98.8
98.9
98.8
NC-1
2nd
00
ML1
4.92
0.91
43
10
8.64
1.43
88.8
82.2
20
8.89
1.51
93.4
91.8
25
9.08
1.55
93.9
91.8
30
9.07
1.55
52
96.8
95.0
96.8
95.0
NC-1
3rd
00
ML2
8.41
1.44
49
10
10.80
1.75
77.0
82.8
20
11.21
1.83
82.7
90.6
25
11.54
1.86
86.9
92.7
30
12.29
1.91
58
96.2
97.0
96.2
97.0
EXAMPLE 2
To further demonstrate the main features of the present invention, as well as to demonstrate additional advantageous variations and improvements, a third sample of limonitic laterite ore, of the composition given in Table 4, was obtained from the East Coast region of New Caledonia for acid pressure leaching; while a highly-serpentinized saprolite ore from the same region was obtained for partial neutralization of leach pulp emanating from the autoclave. Two acid pressure leaching tests were carried out where in the first test dry ore sample was pulped with fresh water while in the second test ore was pulped in its natural state, i.e. containing 40% by weight of H 2 O, with addition of recycle mother liquor, ML1, from the first leach after the pulp from the first pressure leach was first partially neutralized by atmospheric leaching with highly-serpentinized saprolite ore to a pH of about 1.7. The reacted pulp emanating from the second pressure leach was also firstly partially neutralized by atmospheric leaching of highly-serpentinized saprolite ore to a pH of about 1.7, before being settled and filtered to yield a pregnant solution containing the nickel, cobalt and significant quantities of iron and magnesium leached from the highly-serpentinized saprolite ore. Results are summarized in Tables 5 and 6. The final pregnant solution with 10.3 gpl of Ni, 1.7 gpl of Co and 51.1 gpl of magnesium was then partially neutralized to a pH of 3.0 to precipitate some 87% of its contained iron, by the addition of magnesia. After removal of the iron precipitate by filtration, one portion of the clarified pregnant solution of pH 3.0 was reacted with additional quantities of magnesia to a pH of 7.6 thereby precipitating out most of the nickel, cobalt, manganese and remaining iron. Another portion of the same clarified pregnant solution was reacted with Na 2 S to precipitate out virtually all of the nickel, cobalt and remaining iron but only 30% of the manganese, yielding a final solid product analyzing 15.5% Ni, 2.4% Co, 0.4% Mn and 0.5% Fe.
TABLE 4
Laterite ores from the East Coast of New Caledonia
Chemical Composition Wt %
Ore Sample
Ni
Co
Mn
Fe
MgO
SiO 2
Al 2 O 3
Cr 2 O 3
LOI
M4-Limonite
1.57
0.28
1.20
46.5
1.5
4.6
4.2
3.0
14.2
M1-Saprolite
1.92
0.02
0.11
7.3
32.0
39.2
0.6
0.5
14.3
TABLE 5
Acid pressure leaching of limonitic ores; Re-circulation of mother liquor;
Atmospheric neutralization/leaching with highly-serpentinized saprolite ores;
Leaching conditions
Weights of Reactants
Leach Conditions
Ore
Leach
Ore
H 2 O*
H 2 O
“ML”
H 2 SO 4
H 2 SO 4
Pulp
Temp
Press
Time
Sample
No.
g
g
g
g
g
% of Ore
% Solids
° C.
psia
min
M4
1 st
360
240
495
0
105
29
30
270
800
30
M1
27
Partial neutralization to pH 1.7
98
Atm.
40
M4
2 nd
360
240
76
425
99
28
30
270
800
30
M1
36
Partial neutralization to pH 1.7
97
Atm.
40
*This H 2 O represents the H 2 O that would be contained by the raw limonitic feed ore, averaging about 40% H 2 O.
TABLE 6
Acid pressure leaching of limonite ores; Re-circulation of mother liquor;
Atmospheric neutralization/leaching with highly-serpentinized saprolite ore;
Nickel, cobalt and magnesium extractions
Ore
Leach
Rxn Time
Pulping
Solution (gpl)
% Extractions
Sample
No
min
Medium
Ni
Co
Mg
H 2 SO 4
Ni
Co
Mg
M4
1 st
00
H 2 O
10
6.6
1.2
5.5
48
87.7
87.7
100
20
6.8
1.3
5.6
49
90.7
96.1
100
30
7.1
1.3
6.0
50
93.0
99.0
100
M1
40
7.4
1.3
14.5
8
M4 +
Overall extraction based on residue analyses
96.8
96.8
77.8
M1
M4
2 nd
00
ML1
7.4
1.3
14.5
8
10
9.3
1.4
24.3
57
83.3
65.7
71.7
20
10.4
1.7
27.9
58
95.7
91.2
100
30
8.7
1.5
23.3
50
75.0
76.0
62.2
M1
40
10.3
1.7
51.1
21
M4 +
Overall extraction based on residue analyses
86.0
85.7
67.3
M1
As can be seen from the 2 nd Leach, Tables 5 and 6, there is evidence from the solution samples taken during the course of the pressure leaching, that nickel, cobalt and magnesium were precipitating and re-dissolving in the sampling apparatus yielding the anomalous pattern of extractions. More significantly, extractions based on final leached residue analyses indicate, strongly, that a reaction time of 30 minutes is inadequate in a system that has been supercharged with nickel, cobalt and magnesium, by re-circulation of mother liquor.
EXAMPLE 3
Additional tests were carried out with limonite ore M4, circulating mother liquor ML as in Example 1, i.e., without any prior partial neutralization as had been done in Example 2, and following the flowsheet of FIG. 3 . Furthermore, the reaction time with re-circulated ML, the 2 nd Leach, was lengthened to 60 minutes. As seen from Tables 7 and 8, high nickel and cobalt extractions were achieved, and a final leach solution containing 12.1 gpl Ni, 2.1 gpl Co, and also containing 4.4 gpl Fe was produced. The leach pulp emanating from the autoclave after the 2 nd leach, was partially neutralized with highly-serpentinized saprolite ore, M1, at a temperature of 96° C., to a pH of 1.65, in 30 minutes. This partially neutralized leach pulp was further neutralized to a pH of 3.2, at an average temperature of 91° C., by the addition of fine CaCO 3 . The leach pulp was then settled, filtered and washed to yield a clarified pregnant solution analyzing 12.9 gpl Ni, 2.1 gpl Co and only 0.05 gpl Fe, ready to pass on to nickel and cobalt recovery.
TABLE 7
Acid pressure leaching of limonite ores; Re-circulation of mother liquor;
Leaching conditions
Weights of Reactants
Leach Conditions
Ore
Leach
Ore
H 2 O*
H 2 O
“ML”
H 2 SO 4
H 2 SO 4
Pulp
Temp
Press
Time
Sample
No.
g
g
g
g
g
% of Ore
% Solids
° C.
psia
min
M4
1 st
360
240
488
0
112
31
30
270
800
30
M4
2 nd
360
240
142
360
97.6
27
30
270
800
60
*This H 2 O represents the H 2 O that would be contained by the raw limonitic feed ore, averaging about 40% H 2 O.
TABLE 8
Acid pressure leaching of limonite ores; Re-circulation of mother liquor;
Nickel, cobalt and magnesium extractions
Ore
Leach
Rxn Time
Pulping
Solution (gpl)
% Extractions
Sample
No
min
Medium
Ni
Co
Mg
H 2 SO 4
Ni
Co
Mg
M4
1 st
30
H 2 O
8.6
1.5
7.1
44
93
96
100
Based on residue analyses
95.0
89
48
M4
2 nd
00
ML1
8.6
1.5
7.1
44
30
9.6
1.7
8.2
43
73
76
110
45
8.2
1.4
6.8
40
56
46
80
60
14.3
2.3
12.3
73
132
130
200
Final
12.1
2.1
10.6
72
104
105
160
Based on residue analyses
96.5
85+
35+
As can be seen from the 2 nd leach, Tables 7 and 8, there is the same evidence from solution samples taken during the course of the pressure leaching, as was already seen in the 2 nd leach of Example 2, that nickel, cobalt and magnesium were precipitating and re-dissolving in the sampling apparatus, yielding the anomalous pattern of extractions. Also seen from Table 8, based on final leached residue analyses, is that a reaction time of 60 minutes was more than adequate to yield a good extraction level of nickel. The anomalous magnesium results suggest that a significant proportion of the magnesium was precipitating out and reporting in the leached residue.
The process of the present invention is very advantageous over current processes for several reasons. For example, either all or a very large proportion of the fresh water requirement in the pulping step can be replaced by re-circulation of mother liquor emanating from the pressure vessels. Since this mother liquor contains unreacted acid, up to 40% of that initially added to the prepared feedstock ore, overall acid consumption can be significantly reduced. Also, the amount of basic reagents required for subsequent neutralization are reduced by a corresponding amount and the quantity of process liquid effluent discharged is significantly reduced.
The foregoing description of the preferred embodiments of the invention has been presented to illustrate the principles of the invention and not to limit the invention to the particular embodiment illustrated. It is intended that the scope of the invention be defined by all of the embodiments encompassed within the following claims and their equivalents. | An improved process of hydrometallurgical treatment of laterite ores predominantly of the limonitic type for the recovery of nickel and cobalt using sulphuric acid. In order to obtain high extractions of these metals while treating these ores in their humid state, in reaction times of up to 60 minutes, temperatures of up to 270° C. and corresponding pressures of up to 800 psia are used. In the present invention, a significant portion of the “mother liquor” emanating from the pressure leaching reaction is recycled to the feed preparation stage thereby substituting for all or a major proportion of the water that must be added. Concomitantly with the major savings in water requirements, a significant reduction in new sulphuric acid requirements is effected along with a corresponding saving in limestone and lime required for subsequent neutralizations. The amount of process water released to the environment is significantly reduced or eliminated. | 8 |
[0001] This application claims priority in Provisional Patent Application Ser. No. 61/112,859 filed on Nov. 10, 2008 which is incorporated by reference herein in its entirety.
[0002] The invention of this application relates to vises and, more particularly, to multiple jaw vises.
INCORPORATION BY REFERENCE
[0003] The invention of this application relates to vises and, more particularly, to multiple jaw vises wherein multiple jaw vises are known in the art. In particular, Buck U.S. Pat. No. 5,649,694 discloses a multiple jaw vise and is incorporated by reference herein for showing the same. Similarly, Buck U.S. Pat. No. 6,079,704 discloses a multiple jaw vise and is incorporated by reference herein for showing the same. Buck U.S. Pat. No. 6,139,001 discloses a multiple jaw vise and is incorporated by reference herein for showing the same. Cousins et al. U.S. Pat. No. 5,893,551 discloses a multiple jaw vise with machinable jaws and is incorporated by reference herein for showing the same. Lenz U.S. Pat. No. 5,098,073 discloses a multiple jaw vise with a double threaded screw and is incorporated by reference herein for showing the same. Also incorporated by reference herein in its entirety is JERGENS Production Vise Catalog which is attached and forms part of this specification as does the above incorporation by reference documents.
BACKGROUND OF THE INVENTION
[0004] Vises are well known in the art and have evolved over the years. Further, multiple jaw vises are also known in the art and have been well received. In particular, the vises shown in the Buck patents listed above and incorporated by reference in this application as background material have been well received. These patents disclose two jaw vises that are effective and which have been used in industry for many years. However, the vises shown in the Buck patents are costly to manufacture and are costly and difficult to maintain in the field. One such difficulty in the field is that the chips produced by an associated machining operation can become lodged in the vise's actuation mechanism and can be difficult to remove from portions of the vise. This can cause considerable down time for a machining operation which can be costly. This is especially true in view of the costs associated with operating the machines in which these kinds of vises are used. Further, these costs include both machine cost for the machine being idle during this cleaning work and the labor cost associated with the operator working on non-productive work during this cleaning operation. As is known in the art, both the machining time and operator time for these kinds of machining operations are costly. Further, having one of these operations down to allow for the chip removal or cleaning of the vise also impacts the operation's production numbers.
[0005] With special reference to FIG. 3 of Buck U.S. Pat. No. 6,139,001, shown is an end sectional view of Buck's vise or work holding device 11 with a base member 12. Also shown is right movable jaw assembly 16. Jaw assembly 16 is one of the two jaws disclosed in Buck. Particular reference is taken to base member 12 which is a solid block of material wherein a central guide passage or channel 26 must be machined to form this base. More particularly, base member 12, after machining, has upwardly projecting side legs 20, 22 extending on either side of central passage 26. This longitudinally extending guide passage 26 has a generally inverted T-shaped cross-sectional configuration wherein it has an upward opening between the parallel side legs 20, 22 that is smaller than the bottom region of this passage. This guide passage is defined in part by opposed guide surfaces 28, 30 which define opposite sides of the upper portion of guide passage 26. The bottom portion of guide passage 26 is partially defined by a bottom guide surface 32 that is wider than the spacing between surfaces 28 & 30 which forms this “T” shape. As can be appreciated, passage 26 requires one or more expensive machining operations to transform a solid block of material into the disclosed T-shaped block. While other manufacturing methods could be used, each would require expensive tooling and/or machinery to produce the base. Yet even further, this method of machining block 12 makes producing multiple sizes of these vises difficult and expensive.
SUMMARY OF THE INVENTION
[0006] The invention of this application relates to vises and more particularly to multiple jaw vises that are more cost effective to produce and which are less costly to operate. More particularly, the vise according to the present invention includes a multi-piece base section that reduces the number of machining operations necessary to produce the vise.
[0007] According to one aspect of the invention of this application, the base member is formed by a lower member and an upper member joined by vertically extending supports.
[0008] According to another aspect of the invention of this application, the vertical members are a plurality of spaced cylindrical members extending along the side edge of the upper and lower base members.
[0009] According to yet a further embodiment of the invention of this application, the base is formed by a bottom block having a generally rectangular cross-sectional configuration with two ends and opposing sides extending between these ends. This base further includes vertically extending support columns positioned along both of these opposing sides in a spaced relationship joining the bottom block to a pair of parallel top blocks extending with the bottom block with are spaced from one another thereby forming a central slot for guiding the jaws of the vise.
BRIEF DESCRIPTION OF THE DRAWINGS
[0010] The foregoing, and more, will in part be obvious and in part be pointed out more fully hereinafter in conjunction with a written description of preferred embodiments of the present invention illustrated in the accompanying drawings in which:
[0011] FIG. 1 is a bottom perspective view of a vise according to certain aspects of the present invention;
[0012] FIG. 2 is a top view of the vise shown in FIG. 1 ;
[0013] FIG. 3 is a side view of the vise shown in FIG. 1 ;
[0014] FIG. 4 is a sectional view taken along lines 4 - 4 in FIG. 3 ;
[0015] FIG. 5 is a sectional view taken along lines 5 - 5 in FIG. 2 ; and,
[0016] FIG. 6 is a side view of yet another embodiment according to certain aspects of the present invention;
[0017] FIG. 7 is a sectional view taken along lines 7 - 7 in FIG. 6 ;
[0018] FIG. 8 is a side view of yet a further embodiment according to certain aspects of the present invention; and
[0019] FIG. 9 is a sectional view taken along lines 9 - 9 in FIG. 8
DETAILED DESCRIPTION OF EMBODIMENTS
[0020] Referring now to the drawings, in view of the background material of this application, and with special reference to FIGS. 1-5 , shown is a two jaw vise 10 which generally includes a base 12 , a central jaw block 14 and a pair of opposing vise jaws 16 and 18 . As is known in the art, jaws 16 and 18 move relative to base 12 toward and away from one another and function to clamp one or two work pieces (not shown) between the respective vise jaws and central block 14 . The movement of these jaws is in a working portion WP of the vise. Details on this vise and jaw arrangement are not described herein in the interest of brevity in that it is well known in the art and is shown and described in the Buck patents incorporated by reference in this application and which form a part of this description.
[0021] Base 12 has an overall length OL extending in a longitudinal direction 13 and is a multi-component base as opposed to the machined solid block found in the prior art. In this respect, base 12 includes a bottom or base block 20 that can be a single solid block, multiple components joined together, a non-solid block and variations thereof. In that it has been found that a single unified component block works particularly well, this single block arrangement is shown while this application is not to be limited to a single component bottom block. Bottom block 20 further includes a top surface 20 T and an oppositely facing bottom surface 20 B with ends 20 E 1 and 20 E 2 , and sides 20 S 1 and 20 S 2 . Further, block 20 can be substantially rectangular across a major portion of length OL or at least along portions WP.
[0022] Base 12 further includes upper rails 22 and 24 that extend parallel to one another in a longitudinal direction 13 . As with bottom block 20 , rails 22 and 24 can be formed by any method known in the art including, but not limited to, a machined rail and an extruded rail. Further, these rails can be a single component as is shown or formed by multiple components, such as multiple rail sections, to form the needed profiles to allow controlled motion of the jaws as is needed to produce a vise that can effectively hold a work piece. In one embodiment, rails 22 and 24 are rectangular rails such that rail 22 includes a top 22 T, a bottom 22 B, an inner edge 221 and an outer side edge 22 S; similarly, rail 24 can include a top 24 T, a bottom 24 B, an inner edge 241 and an outer side edge 24 S. Rails 22 and 24 further include ends 22 E 1 and 22 E 2 ; and 24 E 1 and 24 E 2 , respectively. As with bottom 20 , rails can be substantially rectangular across a major portion of length OL or at least along portions WP. Rail 22 and 24 can produce the controlled motion of the jaws by including inwardly facing portions 26 and 28 . In other embodiments, the controlled motion of jaws 16 and 18 can be by both portions 26 and 28 and top 20 T of block 20 .
[0023] Further, the rails and/or blocks can also include any known feature in the art to help the vise mount onto and maintain its position relative to a machining operation. This can include, but is not limited to keyways 30 and 32 in block 20 and fastener openings 34 for alignment pins and/or securing bolts 36 .
[0024] Base 12 further includes vertically extending columns 40 that extend between bottom block 20 and rail 22 and vertical extending columns 42 that extend between block 20 and rail 24 . In this embodiment, columns 40 and 42 are mounted columns in that they are separate components mounted between the rails and the bottom block. Columns 40 and/or 42 can be any form of column like structure without detracting from the invention of this application. Further, all of columns 40 do not need to be identical and, similarly, all of columns 42 do not need to be identical. Further, some or all of columns 40 can be different than some or all of columns 42 and visa versa. In one embodiment, columns 40 and 42 are cylindrical columns which can be formed by a column bolt 46 and a sleeve 48 wherein sleeve 48 has a length 48 L and a central passage which allows bolt 46 to pass therethrough. In this respect, sleeves 48 and/or columns 40 / 42 can extend between a top extent 50 and a bottom 52 extent wherein top 50 engages rail bottoms 22 B and 24 B and bottom 52 engage base top 20 T, and define length 48 L.
[0025] Sleeve 48 can be a wide range of configurations including the cylindrical configuration shown and length 48 L can be used to maintain a desired spacing between the rails and the bottom block. Further, these columns could be a unified component or could include multiple fasteners. In yet even other embodiments, one or more columns could be spacers wherein dowels or other components hold them in place. But, these columns can be configured such that they do not include locking fasteners such as a bolt which will be discussed in greater detail below.
[0026] A plurality of columns 40 and/or 42 can be spaced longitudinally along the rails to produce side gaps 54 between adjacent columns which also will be discussed in greater detail below. In this particular embodiment, ten columns are used on each rail wherein there are a total of twenty columns. In other embodiments, some of which will be discussed in greater detail below, more or less columns could be used without detracting from the invention of this application.
[0027] Base 12 further includes end caps or plates 56 and 58 positioned on the longitudinal ends 20 E 1 and 20 E 2 of bottom 20 , respectively. End cap 56 extends between rail ends 22 E 1 and 24 E 1 and bottom block end 20 E 1 wherein cap 56 also joins block 20 to rails 22 and 24 and maintains spacing 48 L similar to that of columns 40 and 42 . Similarly, end cap 58 extends between rail ends 22 E 2 and 24 E 2 and bottom block end 20 E 2 wherein cap 58 also joins block 20 to rails 22 and 24 . End caps 56 and 58 can be joined to the rails and the bottom in any way known in the art including, but not limited to removable fasteners. In one embodiment, caps 56 and 58 are joined to the rails and the bottom by way of fasteners 64 which threadingly engage with the rails and the bottom. By using threaded fasteners, vise 10 can be disassembled to allow for cleaning and the repair of internal components. However, in other embodiments, and for certain industries, the vise may be designed to be tamperproof. As with all fasteners referenced in this application, any fastener known in the art can be used for fastener 64 and others.
[0028] End plates 56 and 58 can include any feature or configuration known in the art to allow the vise to operate in the field including opening 70 which can allow for access to a driving or actuation mechanism 71 of vise 10 and opening 72 which allows crank 74 to actuate the driving mechanism which will not be discussed in greater detail herein in the interest of brevity in that vise driving mechanisms are known in the art. Crank 74 can be any crank known in the art including a crank which includes a transverse handle 76 joined to a shaft 78 . In addition, mechanism 71 can include an adjustable length shaft portion 79 to allow mechanism 71 to be used for more than one size vise which will be discussed in greater detail below.
[0029] Rails 22 and 24 can at least partially control the movement of jaws 16 and 18 to allow for their longitudinal movement. Further, this control can be supplemented by portions of the base block. As is shown, this control is assisted by base top 20 T.
[0030] In the embodiments discussed below, like reference numbers are used to describe like or similar components of the vises described above and further discussions of these components is not being repeated in the interest of brevity.
[0031] With reference to FIGS. 6 and 7 , shown is vise 100 having an overall length OL and which includes yet other column arrangements. In these embodiments, vise 100 includes both a different number of columns and more than one configuration of column. More particularly, vise 100 includes columns 110 having an inner pin 112 and a sleeve 114 . However, while shown as two component columns, these columns and other columns can be formed by a single component without detracting from the invention of this application.
[0032] In one embodiment, vise 100 includes two columns 110 and four columns 40 extending between rail 22 and bottom 20 . While, in this embodiment, columns 40 can be used to secure or fasten the rail to the bottom and columns 110 can be used to merely maintain a desired spacing 48 L, columns 110 could be press fitted into the rail and the bottom to also fasten the two components together at least in part. As is discussed above, this could be used to help make the vise tamperproof. Further, other joining methods could be used, such as welding, to join the columns to the bottom and rails. Similarly, the same column arrangement can be used to secure rail 24 to bottom 20 . However, as is mentioned above, while it may be preferred to make both sides the same, this is not necessary and this application should not be limited in that way. Further, this particular column arrangement, including the specific location and columns 110 relative to columns 40 , is not required and this application should not be limited to this specific spacing and/or locations.
[0033] As with the other embodiments of this application, spacings or gaps are produced in these side portions of the vise. In the embodiments shown in FIGS. 6 and 7 , gaps of different sizes are produced. In this respect, vise 100 includes gaps 120 - 124 which have differing sizes. Gaps 121 and 123 are in working portions WP, which are closer to the machining locations of the vise. These gaps can be larger to allow for the chips to be cleaned more easily from these working regions. While not shown in the interest of brevity, the opposite side of vise 100 can include the same column configuration; however, this is not a requirement.
[0034] With reference to FIGS. 8 and 9 , shown is vise 200 that includes yet other embodiments. In this respect, vise 200 includes side rails wherein at least a portion of the rails extending to bottom 20 thereby having an integral column arrangement. In this respect, vise 200 , which has an overall length OL, includes a rail 210 having downwardly extending columns 212 - 214 which extend downwardly from a top rail portion 220 . Rail 210 has a length OL and extends between ends 220 E 1 and 220 E 2 . In this embodiment, the columns are an integral component of the rail portion or could be fabricated to the rail portion by any joining method known in the art including, but not limited to, welding. In that columns 212 - 214 are spaced from one another, rail 210 includes spacings or gaps 230 and 232 in working portions WP. Further, while vise 200 is shown to include columns having different widths in the longitudinal direction, this is not required and rail 210 could be formed by columns having uniform widths and/or equal spacings or gaps therebetween. The same is true with the size of the gaps. These do not need to be identical and there could be any number of these spacings depending on the size of the vise. Further, in yet other embodiments, the vise can include a combination of integral columns and mounted columns. Rail 210 can be joined to base 20 by fasteners 240 that pass through bottom 20 and thread into one of columns 212 - 214 .
[0035] As a result of this construction, base 12 can be formed without the need to perform multiple and deep grinding operations to a solid metal block. Further, these grinding operations can be dimensionally critical wherein precision grinding equipment along with special grinding wheels can be necessary. As can be appreciated, these grinding wheel operations can also require costly wheel dressing operations to achieve the necessary internal dimensions and/or profiles of this machined block. While this can be simplified by using computer control grinding and/or milling operations (CNC), the amount of material that needs to be removed can use a considerable amount of machining time which is also costly.
[0036] As can also be appreciated, not only is it expensive to perform multiple machining operations to the base block, a considerable amount of waste is also produced by these machining operations. In this respect, the machining necessary to produce prior art bases can result in a significant amount of scrap metal in that much of the block is machined away. While metal chips can be salvaged, this is wasteful especially in view of the costly metal that is often used to produce these bases and the energy costs associated with this amount of machining. In the embodiments of the invention of this application, significant amounts of scrap and energy can be eliminated in that the bottom, rails and end caps can be purchased such that they are configured similar to their final dimensions and relatively simple machining operations can produce parts within the desired dimensional tolerances.
[0037] Furthermore, this base configuration also advantageously produces the openings, spacings or gaps 54 , 120 - 124 , 130 and/or 132 spaced about the sides of the base that allow the chips, produced during an associated machining operation using vise 10 , 100 and 200 , to be easily blown out of these bases. As can be appreciated, when these vises are in use a considerable amount of chips can often be produced as the component part, that is being held by the vises are being machined. These chips need to be cleaned from the vise or the vise could eventually jam which can cause down time for the particular machining operation.
[0038] Again, as is discussed above, the vises of this application can have any actuation mechanism known in the art including, but not limited to, manually cranked vises and hydraulic vises.
[0039] In even yet other embodiments, combinations and equivalences thereof of the components including, but not limited to, the column arrangements can be used to produce even more vises according to the invention of this application.
[0040] Yet another benefit of the vise of this application is the ability to quickly and easily produce a wide range of sizes of these vises. As is known in the art, virtually any item can be machined to produce a finished part or component. In that virtually any component can be machined, there is a need for vises in a wide range of sizes. This situation is difficult for the vise manufacturing of prior art vises in that each component must be machined differently for each size. As a result, it is difficult and costly to stock multiple sizes of vise bases and it is then difficult to fill vise orders quickly in that unique components must be manufactured or inventoried to produce each vise.
[0041] However, a vise according to the present invention can be quickly made to order in view of the ability to stock common components to produce a much wider range of vise sizes. In this respect, the primary components of the vises of this application can be quickly formed into a vise of a desired size without the need for high cost inventory. For example, the rails and the bottom blocks discussed above are much less costly to produce than the prior art machined base in that they can be extruded and/or require much less costly machining operations. This alone greatly reduces inventory costs. In addition to this benefit, these less costly parts can be made in lengths much longer than overall length OL of each vise. Then, once an order arrives, these components can be quickly cut or trimmed to the desired overall length of the particular vise. This can be a relatively simple trimming operation in that the overall length dimension does not require the tight tolerances of the internal machining operation of the prior art vises. Further, multiple lengths of the actuating shafts and/or adjustable shaft sections 79 of the vise can also be utilized to allow for these differing lengths. As a result, different size vises can be quickly made with common components and these common components can be inventoried at much lower costs than was possible with prior art vises. This can further include stocking a single base for different widths of vises wherein a relatively simple trimming operation could also be used to transform a universal base block into more than one size vise.
[0042] While not shown, the vise according to the present invention can be used for any known application, and even newly found applications, for these styles of vises. This includes powered versions of these vises wherein hand crank 74 is replaced with a powered crank (not shown). Further, the vise according to the present invention could be incorporated as a component of a clamping system without detracting from the invention of this application.
[0043] While considerable emphasis has been placed on the preferred embodiments of the invention illustrated and described herein, it will be appreciated that other embodiments and/or equivalents thereof 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. | A two jaw vise having a base extending in a longitudinal direction between two ends, a central fixed block and opposing jaws on either side of the central block. The opposing jaws being movable longitudinally and joined to the base for controlled movement longitudinally. The base including a base block extending longitudinally between the first and second ends and including first and second longitudinally extending rails. The first and second rails extending parallel to the base block and being spaced from the base block. The first and second rails at least partially forming the controlled movement of the jaws. The base further including first and second pluralities of vertically extending columns extending between the base block and the first and second rails, respectively. The base including at least one gap between adjacent columns. | 1 |
The present invention relates to ventilation devices in general and in particular to such a device that can be used with vertical or horizontal sliding windows, and is especially effective with combination storm and screen windows or doors.
BACKGROUND OF THE INVENTION
Most original and replacement windows for modern residential buildings are of either the casement or the sliding variety, with either vertical or horizontal movement for opening and closing the window. Casement type windows provide for automatic deflection of incoming air due to the pivoting nature of their actuation. Slider type windows on the other hand do not provide for any deflection of incoming air. Similarly, if the window is open during a rain storm there is a strong likelihood that rainwater will enter the room and puddle on the floor.
Older homes, such as those built before 1950, contained mostly double hung windows. Older styles of storm windows and screen frames were usually hung or attached to the exterior frame and were changed from season to season. These were gradually replaced with relatively inexpensive extruded aluminum "combination storm and screen" windows, custom fitted to the exterior frames. These still exist on the majority of older homes in the upper half of North America. Although many environmentally superior replacement windows are available today, they are very expensive and are limited in application to those people that can afford to have them installed. The combination storm and screen windows mentioned above are still manufactured and find a ready market in the older homes in inner cities and rural towns and villages.
Over approximately the same period, older style separate storm doors and screen doors have been replaced with the same general design of "combination storm and screen" doors, manufactured from aluminum extrusions.
Combination storm and screen windows and doors permit an almost infinite adjustment of opening up to the limit of screening and are usually controlled by spring friction or by using spring loaded adjustable stops. While this type of window or door satisfies an important need, they lack the ability to permit a small opening of, say, 2 to 3 inches during a rain storm, thereby necessitating closure of the windows or doors, at least on the windward side of the residence. When at home, this closing function can be done by the occupants. However, in the occupant's absence, or while sleeping (and particularly in babies' or small children's bedrooms) a sudden rain storm can cause entry of water and the consequent damage to floors, not to mention the general disturbance to the household.
Upstairs windows, in particular, may not be left open during the day to relieve the usually higher temperature found in the upper floors of older homes. For this reason, one must remember to close such windows before all occupants depart the residence. Senior citizens and those with physical impediments may have great difficulty in acting promptly to close such windows in the event of sudden rain storm and may tend to leave such windows closed during times of inclement weather or threatening forecasts.
Aside from the consequences described above the need exists to allow indirect ventilation of rooms, especially bedrooms, to avoid draughts, particularly in early spring or late fall when fresh air is needed, but that same air is cooler than normal summer air. Occasional ventilation is needed sometimes in the winter or in more temperate zones and a means of deflecting such incoming air is useful and convenient.
There have been attempts in the past to produce ventilators for sliding window but they have all been deficient in one way or another. Prior art ventilators are found for example in Canadian Patents Nos. 148,861 (Fisher) of Jun. 2, 1913; 449,739 (Eichenberger) of Jul. 13, 1948; 465,612 (Allen) of Jun. 6, 1950; and 492,545 (Shelley) of May 5, 1953.
SUMMARY OF THE INVENTION
The present invention meets the above criteria with a simple, inexpensive ventilator that any person can install in a slider type window. The ventilator of this invention uses a pair of generally triangular end members and a bridging member that extends between the end members. The bridging member is thin and can be extruded from a plastics material. the bridging member has a pair of longitudinally extending spaced apart rib members parallel to a long edge thereof on one side, with each rib member containing a partially enclosed slot which enters the rib member from the opposite side of the bridging member. Each end member has a slot adjacent one of the long edges thereof, which slot has a profile corresponding to the outer profile of the bridging member. Each end member slot thus includes an enlarged area for reception of the end of each rib member and there is an opening through the end member at each enlarged area for reception of a threaded fastener, such as a self-tapping machine screw. When the bridging member is assembled to an end member a screw is passed through each opening in the end member and is threaded into the respective slot of the bridging member to secure the bridging member to the end member. In this way the components can be packaged in an unassembled, flat condition, and they can be stored in the same condition during the winter months. The threaded fastener technique allows for quick assembly and disassembly a multitude of times and permits wider tolerances during manufacture.
The above describes the most basic embodiment of the invention. The bridging member could be supplied in a standard length of, say, one meter, and the homeowner could easily cut the member to the desired length with a hacksaw or any good wood saw. Another embodiment has the bridging member provided with a pair of ribs on the same side as the slot openings with the ribs of one bridging member being receivable in the slots of another bridging member so as to achieve adjustability of length. Although it would be preferable to only use a pair of telescoping bridging members for the average installation there would be nothing preventing the telescoping assembly of three or more bridging members to attain a ventilator of almost any desired length. Of course, as the length increases the stability of the ventilator will decrease due to the increased unsupported length.
Broadly speaking therefore the present invention provides a ventilator device for a slider type window comprising a pair of generally right-triangular end members and a bridging member extendable between the end members, the bridging member having rib portions extending along one side parallel to one long edge thereof, with a partially enclosed slot extending into each rib portion from the opposite side of the bridging member, and each end member having a slot adjacent one of the long edges thereof, the end member slot conforming in shape to the end profile of the bridging member and having an enlarged area corresponding to the end face of each rib portion, with an opening through the end member at each enlarged area aligned with the corresponding partially enclosed slot for reception of a threaded fastener threadable into the partially enclosed slot to secure the end member to the bridging member.
The present invention also provides a ventilator device for positioning within a slider type window between fixed and movable frame portions thereof, the device comprising: a pair of generally right-triangular end members and a pair of bridging members telescopically extendable between the end members; each of the bridging members having a pair of rib portions extending along one side parallel to one long edge thereof, a generally diamond-shaped slot extending into each rib portion from the opposite side of the bridging member, and a pair of generally triangular rib members extending along the opposite side of the bridging member parallel to the one long edge: and each end member having a slot adjacent one of the long edges thereof, each end member slot conforming in shape to the end profile of the bridging member to be received therein and having pairs of first and second enlarged areas to accommodate the end faces of the rib portions and rib members respectively, with an opening through the end member at each first enlarged area aligned with the corresponding diamond-shaped slot of a bridging member for reception of a threaded fastener threadable into the diamond-shaped slot to secure the end member to one of the bridging members.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 shows a typical vertical slider type window with a ventilator of the present invention in place.
FIG. 2 is an exploded perspective view showing the components of the invention.
FIG. 3 is an exploded perspective view of another embodiment of the present invention.
DESCRIPTION OF THE PREFERRED EMBODIMENT
FIG. 1 illustrates a typical vertical slider type window such as a storm window and screen combination as might be found in a storm door, for example. The combination includes a peripheral frame 10, a slider frame 12 containing window glass 14, a fixed screen 11 and a fixed or slidable frame 16 containing window glass 18. The window does not form part of the invention and, in fact, the invention is operable with a horizontal slider type window as well.
The ventilator 20 of the present invention is shown in position between the sill 22 and the bottom frame or sash member 24 of the slider frame 12. The ventilator 20 includes a pair of end members 26 and a pair of relatively slidable or telescopic bridging members 28',28" between the end members 26. As seen in FIG. 1 the bridging members 28',28" telescope together so that the end members 26 can be positioned against the vertical frame members 30,30.
FIG. 2 shows an exploded view of the components use in the FIG. 1 configuration. It is seen for example that each end member 26 has a shape that is generally fight-triangular, there being two long edges 32,34 and a short edge 36 that meets the edge 32 at substantially a right angle. Two of the vertices are provided with cut out sections 38,40 for reception of the window frame member 24 and for reception in or against the sill 22 respectively. A strengthening rib or flange 42 extends along the edge 32 and projects laterally outwardly therefrom. On the opposite side of the end member is a slot 44 defined by raised ribs or flanges 46,48, the slot 44 being adapted to receive the end of a respective bridging member 28',28". The flange 48 includes two semicircular portions 50,50 which define enlarged areas 52,52 within the slot 44. Other semicircular portions 54,54 define enlarged areas 56,56 within the slot 44. Each enlarged area 56 includes an opening 58 that extends through the end member 26 and is adapted to receive a fastener such as a self-tapping machine screw 60. The opening or hole 58 can have a countersunk area 62 on the outside of the end member so that the head of the screw 60 will not be exposed above the surface of the end member. Preferably the end members 26 will be injection molded from a thermoplastic material.
The bridging members 28',28" are also shown in FIG. 2. The members are identical to each other but, when they are assembled together one is turned upside down and back to front relative to the other so that they can be telescoped together. Therefore only the member 28' will be described in full.
The bridging member 28' is elongate, with parallel long edges 64,64 and end edges 66,66. The member is extruded from a plastics material and has on one side 68 thereof a pair of longitudinally extending rib portions 70,70 parallel to the long edges 64,64 with one of the rib portions 70 being closer to a long edge 64 than the other rib portion 70. A partially enclosed slot 72 extends into each rib portion 70 from the opposite side 74 of the bridging member. Each slot 72 extends for the full length of the bridging member and in the embodiment as illustrated it has a square or diamond-shaped transverse profile, opening to the opposite side 74 of the bridging member along one vertex of that profile. A pair of rib members 76,76 is provided on the side 74 of the bridging member, the rib members being parallel to the rib portions 70,70 and having the same spacing therebetween and orientation on the bridging member so that when the bridging members are brought together in a telescoping relationship the rib members 76,76 of one bridging member will be received within corresponding slots 72,72 of the other bridging member, with their long edges 64,64 being coplanar. As seen in FIG. 2 the rib member 76 has an inverted triangular profile which fits snugly within the diamond-shaped profile of the slot 72, the angled sides of the rib member sliding on the angled sides of the slot and the widest part of the rib member extending between the laterally opposed vertices of the slot. These profiles are convenient to extrude, but it is understood that other mating profiles would work equally well without departing from the intent of the invention. Circular profiles for example would be acceptable.
One important feature of the present invention is seen in FIG. 2 wherein the each of the openings or holes 60 is shown to be in alignment with a corresponding slot 72 of the bridging member to be received in the end member slot 44. For assembly of an end member to a bridging member one need only insert the bridging member into the slot 44 and then to drive a screw 62 through the opening 60 into the slot 72 so that the self-threading property of the screw will securely fasten the end member to the bridging member. With two screws in place the components are tightly fastened together with no chance of separation. Furthermore the end member and the bridging member can be disconnected for winter storage. Of course the maximum size of the slot 72 is smaller than the diameter of the screw 62 so that the threads of the screw will bite into the material of the bridging member to hold the components together. A diamond-shaped (or square) slot is preferred because the plastic material is displaced into the corners as the screw is threaded into the slot. This allows repeated assembly and disassembly, something that might not be as available with circular slots, which tend to gall after repeated use.
When the end members have been assembled, one to each bridging member, the bridging members 28',28" are telescoped together with the rib members 76,76 of the bridging member 28' received in the slots 72,72 of the bridging member 28" and the fib members 76,76 of the bridging member 28" received in the slots 72,72 of the bridging member 28'. The assembled ventilator 20 may then be positioned in any convenient window as illustrated in FIG. 1. As indicated earlier, one significant application for this invention is in association with the vertically slidable window sections of aluminum combination storm and screen windows or doors. The ventilator can be locked in place between the slidable window and the surrounding frame or track so that any incoming breeze is directed upwardly to prevent draughts and so that any rain entering through the screen is prevented from entering the dwelling and falling to the floor. This allows the homeowner to use the combination storm and screen window or door even in inclement weather so as to obtain the ventilating advantages thereof.
While the invention has been described and illustrated with respect to vertically slidable windows, it is also useful with horizontal sliding type window. In such an application the ventilator of the invention would be oriented vertically with the cut out 40 positioned in a vertical portion of the peripheral window frame and the cut out 38 receiving the vertical edge of the sliding window frame of the window.
FIG. 3 shows another variation of the present invention although the principles thereof are unchanged. In this embodiment each bridging member 80'80" has a reentrant J-shaped flange 82 extending along one long edge thereof with the flange defining an opening 84 for receiving the other long edge of the other bridging member. That other long edge may optionally have a small locking ridge 86 receivable within the flange 82 to further prevent unwanted separation of the bridging members. Each bridging member has a pair of parallel spaced apart rib portions 88 extending the length thereof, with each rib portion having a partially enclosed, generally circular slot 90 therein, which slot serves the same purpose as the slots 72,72 of the first embodiment.
The generally right triangular end members 92 have opposed slots 92,94 which are mirror images of each other and which are separated by a relatively thin web 96 of end member material, the slots each being dimensioned to receive an end face of a bridging member therein. Each slot 92,94 has enlarged areas 98 therein corresponding to the rib portions 88 and through holes 100, 102 alignable with the slots 90,90. Since the end members 92 are interchangeable end for end it is necessary to provide two holes at each enlarged area 98 to compensate for the offset of one bridging member and its slots 90 relative to the other. A self-tapping machine screw 104 passes through the appropriate holes 100,102 to secure the end member to the corresponding bridging member.
It is not necessary to telescope two or more bridging members together to achieve a useful ventilator. A single bridging member could extend between a pair of end members, the bridging member being provided in a relatively long section of, say, a meter or so. It could be cut to length with a hacksaw and then attached to the end members to create a non-adjustable ventilator. With the first embodiment it would be desirable to have end members in which the is no offset between the slots 44 of the left and right hand end members as there is but a singe bridging member being used. When an even number of bridging members are telescoped together the offset between the slots 72,72 of the righthandmost and the lefthandmost bridging members will have to be compensated for by slightly offsetting the slots 44 of the right and left end members. This would not be a problem with the second embodiment as there is automatic compensation through the use of two holes 100,102 at each enlarged area 98. Of course, slots formed in the manner of the slots 44 of the first embodiment could be used with the second embodiment and vice versa.
The present invention provides window ventilators which are effective, usable with practically any style of slider type window, inexpensive to produce and package, and easy to install. The foregoing has described the preferred embodiments of the invention but it is understood that variations therein may occur to a skilled person, which variations would not depart from the spirit of the inventions. Accordingly the protection to be afforded this invention is to be determined from the claims appended hereto. | A ventilator for slider type windows is provided, the ventilator having triangular end members and one or more bridging members extending therebetween. The ventilator is positionable between fixed and movable portions of the window and deflects incoming air upwardly or to the side. Each bridging member is provided with a pair of rib portions, each having a partially enclosed slot running the length thereof. Each end member has a slot adapted to receive the end face of a bridging member and has a pair of holes extending therethrough in alignment with the corresponding slots of the bridging member received therein. A screw extends through each hole and is threaded into the adjacent bridging member slot to secure the bridging member to the end member. The ventilator is particularly useful with combination storm and screen windows or doors. The ventilator can be packaged with all components flat and can be assembled and disassembled with ease. | 4 |
BACKGROUND OF THE INVENTION
[0001] 1. Field of the Invention
[0002] The present invention relates to a polarization measuring apparatus for detecting the polarization of input signal light by measurement of the Stokes parameter or the like.
[0003] 2. Description of the Related Art
[0004] In optical communication systems, as one means for increasing the transmission capacity, it is considered that a communication speed per one channel is increased. However, if the bit rate of a signal light reaches a range exceeding 10 Gbps (giga bit/second) or 40 Gbps, the pulse width of the signal light becomes several tens of ps (picosecond). Therefore, it becomes difficult to distinguish between a ‘ 0 ’ level and a ‘ 1 ’ level of the respective bits due to the waveform distortion caused by various factors. Since such waveform distortion becomes a factor in determining the main specifications such as system length, then when designing a system, various measures, such as arranging parts for compensating for the waveform distortion, are taken.
[0005] As a factor causing the waveform distortion of the signal light, there is polarization mode dispersion (PMD). This PMD is the dispersion which arises as a result of an occurrence of differential group delay (DGD) between two orthogonal polarization modes, due to, for example, the deformation of a core of an optical fiber to be used as an optical transmission path into an elliptic shape, a lateral pressure, a partial temperature change and the like. For example, in the case where an optical fiber is laid in a place, which is subjected to vibration or the like, along the side of a railroad, a change in the PMD is extremely fast, and a speed of the change is said to be approximately several KHz.
[0006] PMD compensators (to be referred to as PMDC hereunder) for compensating for the abovementioned PMD have been recently developed by various companies. A well-known PMDC configuration is basically a loop back system where the waveform distortion of a signal light is monitored and a compensation amount of the PMD is controlled corresponding to the monitoring result. However, according to such a loop back system, it is difficult to directly and quantitatively monitor a state of the waveform distortion and a generated dispersion amount. As substitute means, typically, there is a method for monitoring a degree of polarization (DOP). Moreover, examples of measuring the bit error rate (BER), or measuring the electrical spectrum hole burning are also known.
[0007] The DOP can be measured using a polarization measuring apparatus (polarimeter). As a conventional polarizabon measuring apparatus, there is known, for example, an apparatus for measuring four Stokes parameters representing polarization (for example, Japanese Unexamined Patent Publication No. 618332, Japanese Unexamined Patent Publication No. 9-72827, Japanese National Publication No. 2001-520754, and Japanese National Publication No. .2003-508772).
[0008] FIG. 7 shows a configuration of a basic optical system of the conventional polarization measuring apparatus as mentioned above. In this optical system, firstly an input signal light is branched into four at 25% each, by an optical coupler (CPL) 1 . Then, a first branched light passes through a quarter wave plate (QWP) 2 and a polarizer (POL) 3 1 letting through only a polarization component which is inclined by 45° with respect to a preset reference plane, and is input to a light receiving element (PD) 4 1 . A second branched light passes through a polarizer (POL) 3 2 letting through only a polarization component which is inclined by 45° with respect to the above reference plane, and is input to a light receiving element (PD) 4 2 . A third branched light passes through a polarizer (POL) 3 3 letting through only a polarization component which is parallel (or perpendicular) with respect to the above reference plane, and is input to a light receiving element (PD) 4 3 . A fourth branched light is directly input to a light receiving element (PD) 4 4 .
[0009] If the electric signals which are photoelectrically converted by the respective light receiving elements 4 1 , 4 2 , 4 3 and 4 4 , to be output, are D Q , D 45 , D 0 , and D T , then the four Stokes parameters S 0 , S 1 , S 2 and S 3 are represented by the relationship shown in the following equation (1).
S 0 =D T
S 1 =2· D 0 −D T
S 2 =2· D 45 −D T
S 3 =2· D Q −D T (1)
[0010] Here, S 0 represents the intensity of the input signal light, S 1 represents a horizontal linear polarization component (0°, S 2 represents a linear polarization component which is inclined by 45°, and S 3 represents a right-handed rotatory circular polarizabon component. By using the abovementioned Stokes parameters S 0 to S 3 , the DOP to be measured is represented in accordance with the relationship of the following equation (2).
DOP = S 1 2 + S 2 2 + S 3 2 S 0 ( 2 )
[0011] However, in the abovementioned conventional polarization measuring apparatus, there are following problems.
[0000] (a) Enlargement of the Apparatus Size
[0012] In the conventional polarization measuring apparatus, as shown in the optical system in FIG. 7 , a large number of optical elements, such as, the optical coupler 1 , the quarter wave plate 2 , the polarizers 3 1 to 3 3 , and the light receiving elements 4 1 to 4 4 must be arranged in required positions, and hence there is a tendency for the size of the whole apparatus to become large.
[0000] (b) Deterioration of Measurement Accuracy Due to Reflected Lights Generated in the Optical Elements
[0013] Generally, a part of an incident light is reflected at a light incident plane and the like of an optical element, a refractive index of which is changed. In order to suppress the generation of this reflected light, an anti-reflection film is normally formed on the light incident plane of the optical element. However, it is difficult to completely prevent the generation of the reflected light by the ant-reflection film. In the optical system shown in FIG. 7 , there is a possibility that reflected lights are generated at the respective light incident planes of the optical coupler 1 , the quarter wave plate 2 , the polarizers 3 1 to 3 3 , and the light receiving elements 4 1 to 4 4 , and also, there are many places which can be reflection surfaces. In the case where some of these reflection surfaces are in a parallel or nearly parallel state with respect to a light emission plane of a former stage optical element, then for example as shown in FIG. 8 , the multi-reflection of light occurs and an interference system is formed. Therefore, the power of the signal light detected by the light receiving element is varied with time, and a transmission characteristic has the wavelength dependence, resulting in the deterioration of measurement accuracy. Moreover, there is also a possibility that a part of the light reflected at the light incident and emission planes of the respective optical elements becomes a stray light. In an optical system where parts such as light receiving elements are arranged adjacent to each other in order to miniaturize the apparatus, the above stray light is input to a light receiving element different to a light receiving element to which the stray light is to be input primarily, to cause light leakage (cross-talk), resulting in the deterioration of measurement accuracy.
[0000] (c) Deterioration of Measurement Accuracy Due to the Phase Shift between p/s Waves
[0014] In the conventional polarization measuring apparatus, the input signal light is branched into four by the optical coupler 1 , in order to obtain the four Stokes parameters S 0 to S 3 . In the case where one utilizing for example a dielectric multi-layer film is used as the optical coupler 1 , it is known that the phase shift occurs between the p wave (p polarized light) and the s wave (s polarized light) of the branched light (specifically, the transmitted light) due to the optical coupler 1 . Such phase shift between the p/s waves does not cause a problem in a function of branching the optical power, but does change the polarization of the signal light after passing through the optical coupler 1 . Therefore, in the case where there is an optical element such as a polarizer on the latter stage of the optical coupler 1 , the phase shift affects the power of the signal light passing through the polarizer or the like, which becomes a factor in the deterioration of measurement accuracy.
[0000] (d) Deterioration of Measurement Accuracy Due to Temperature Fluctuation
[0015] Since the conventional polarization measuring apparatus comprises a large number of optical elements as shown in FIG. 7 , characteristics of the respective optical elements are changed with the temperature fluctuation, which causes the deterioration of measurement accuracy. Moreover, since the input signal light is branched into four, and then transmitted over the respective optical elements, a mounted area becomes large and there is thus the likelihood of influence of optical axis shift due to the temperature fluctuation.
SUMMARY OF THE INVENTION
[0016] The present invention has been accomplished in view of the problems as shown in the abovementioned (a) to (d), with an object of providing a miniaturized polarization measuring apparatus which can measure the polarizabon of input signal light with high accuracy, even in an optical system where a plurality of light receiving elements are arranged adjacent to each other.
[0017] In order to achieve the abovementioned object, a polarizaton measuring apparatus of the present invention comprises: an optical branching section that branches an input signal light into a plurality of signal lights; a plurality of optical elements arranged on a plurality of branched optical paths through which the signal lights branched by the optical branching section are propagated, respectively, for providing the signal lights with polarizations and phase shifts, which are different for each signal light; and a plurality of light receiving elements receiving the signal lights respectively propagated through the branched optical paths, to detect the powers of the signal lights, wherein, the elements adjacent to each other of the optical elements and the light receiving element arranged on the same branched optical path, are arranged to be inclined to each other so that a light emission plane of the element positioned on a former stage and a light incident plane of the element located on a latter stage are not substantially in parallel, and there is provided a shielding section that prevents a stray light generated by the reflection of the signal light between the elements where the light incident and emission planes are arranged to be inclined to each other, from reaching the light receiving element located on another branched optical paths which is different from the branched optical path concerned.
[0018] According to such a configuration, the opposing incident and emission planes of the adjacent elements which exist on the same branched optical path are arranged to be inclined to each other, so as to avoid that an interference system is formed due to the multi-reflection of the reflected light. Also, the stray light generated between the elements arranged with their incident and emission planes inclined to each other, is blocked by the shielding section, to be prevented from being incident on the light receiving element on another branched optical path to be received. Therefore, it becomes possible to stably measure the polarization of the input signal light with extremely high accuracy.
[0019] Moreover, as one aspect of the above polarization measuring apparatus, the configuration may be such that the optical branching section branches an input signal light into first to fourth signal lights, and the plurality of optical elements include: a quarter wave plate and a first polarizer letting through only a polarization component which is inclined by 45° with respect to a preset reference plane, which are sequentially arranged on a first branched optical path through which the first signal light is propagated; a second polarizer letting through only a polarization component which is inclined by 45° with respect to the reference plane, which is arranged on a second branched optical path through which the second signal light is propagated; and a third polarizer letting through only a polarization component which is parallel or perpendicular with respect to the reference plane, which is arranged on a third branched optical path through which the third signal light is propagated, and the plurality of light receiving elements include: a first light receiving element receiving the first signal light passed through the quarter wave plate and the first polarizer; a second light receiving element receiving the second signal light passed through the second polarizer; a third light receiving element receiving the third signal light passed through the third polarizer; and a fourth light receiving element receiving the fourth signal light branched by the optical branching section to be propagated through a fourth branched optical path, and a light emission plane of the quarter wave plate and a light incident plane of the first polarizer, a light emission plane of the first polarizer and a light incident plane of the first light receiving element, a light emission plane of the second polarizer and a light incident plane of the second light receiving element, and a light emission plane of the third polarizer and a light incident plane of the third light receiving element, are each arranged to be inclined to each other so as not to be substantially in parallel.
[0020] Furthermore, the configuration may be such that the optical branching section includes: a first stage optical coupler branching an input signal light into a reflected light and a transmitted light at a branching ratio of 1:3; a second stage optical coupler branching the transmitted light from the first stage optical coupler into a reflected light and a transmitted light at a branching ratio of 1:2; and a third stage optical coupler branching the transmitted light from the second stage optical coupler into a reflected light and a transmitted light at a branching ratio of 1:1, and an incident angle of each of the signal lights given to the first to third stage optical couplers is set to be a predetermined angle away from the Brewster angle.
[0021] According to such a configuration, by using optical couplers in a three stage configuration as the optical branching section, and setting the incident angle of each of the signal lights given to the optical couplers, to the predetermined angle away from the Brewster angle, it becomes possible to reduce the phase shift which occurs between p/s waves of the branched light in each optical coupler, so that the higher measurement accuracy can be realized.
[0022] In addition, the above polarization measuring apparatus is preferably configured such that the reflected light of the first stage optical coupler is propagated through the fourth branched optical path, the reflected light of the second stage optical coupler is propagated through one of the second branched optical path and the third branched optical path, the reflected light of the third stage optical coupler is propagated through the first branched optical path, and the transmitted light of the third stage optical coupler is propagated through the other of the second branched optical path and the third branched optical path.
[0023] In this way, by appropriately setting the branched optical paths for propagating therethrough the signal lights branched by the optical couplers in the three stage configuration, taking into consideration differences in the respective optical path lengths, it becomes possible to minimize a mounted area of the optical parts.
[0024] Moreover, as a specific configuration of the above described polarization measuring apparatus, the optical branching section, the plurality of optical elements, and the plurality of light receiving elements may be mounted on the same substrate, and also there may be provided a temperature control section that controls the temperature of the substrate to be constant.
[0025] According to such a configuration, by mounting the optical parts on the same substrate and controlling the temperature of the substrate, the temperatures of the respective optical parts on the substrate become constant. Therefore, a change in optical characteristic, optical axis shift and the like due to the temperature fluctuation, can be suppressed. Thus, it becomes possible to measure the polarization of input signal light with even higher accuracy.
[0026] Other objects, features and advantages of the present invention will become apparent from the following description of embodiments, in conjunction with the appended drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
[0027] FIG. 1 is a plan view showing a configuration of an optical system of a polarization measuring apparatus according to one embodiment of the present invention.
[0028] FIG. 2 is a cross-sectional view along an optical axis of input signal light in the optical system in FIG. 1 .
[0029] FIG. 3 is a diagram for explaining an arrangement of optical couplers in the above embodiment.
[0030] FIG. 4 is a diagram showing an arrangement of optical elements adjacent to each other on the same branched optical path in the above embodiment.
[0031] FIG. 5 is a plan view showing a specific arrangement example of optical elements in the above embodiment.
[0032] FIG. 6 is a diagram exemplarily showing an appearance of the polarization measuring apparatus in the above embodiment.
[0033] FIG. 7 is a diagram showing a configuration of a basic optical system of a conventional polarization measuring apparatus.
[0034] FIG. 8 is a diagram for explaining a situation where an interference system is formed between optical elements adjacent to each other in the conventional polarization measuring apparatus.
DETAILED DESCRIPTION OF THE INVENTION
[0035] Hereunder is a description of the best mode for realizing a polarization measuring apparatus of the present invention, with reference to appended drawings. Throughout the drawings, the same reference numerals denote the same or corresponding parts.
[0036] FIG. 1 is a plan view showing a configuration of an optical system of a polarizabon measuring apparatus according to one embodiment of the present invention.
[0037] In FIG. 1 , the present polarization measuring apparatus is provided with three optical couplers 1 A, 1 B and 1 C each obtained by forming, for example, a dielectric multi-layer film on a plate, as a specific configuration corresponding to the optical coupler 1 in the above described conventional basic optical system shown in FIG. 7 . The optical couplers 1 A to 1 C are in a three stage configuration where an input signal light L IN is incident on the optical coupler 1 A of a first stage, a transmitted light of the optical coupler 1 A is incident on the optical coupler 1 B of a second stage, and a transmitted light of the optical coupler 1 B is incident on the optical coupler 1 C of a third stage. Branching ratios of the incident lights at the respective optical couplers 1 A to 1 C (reflected light power transmitted light power) are set to be 1:3 for the first stage, 1:2 for the second stage, and 1:1 for the third stage. As a result, the input signal light L IN is branched into a reflected light of the optical coupler 1 A, a reflected light of the optical coupler 1 B, and a reflected light and a transmitted light of the optical coupler 1 C, at the same power respectively. Moreover, a light incident plane of each of the optical couplers 1 A to 1 C is inclined with respect to a propagation direction of the input signal light L IN so that an incident angle of signal light is away from the Brewster angle. Here, the incident angles of the respective optical couplers 1 A to 1 C are respectively set to be 22.5°, taking into consideration the most effective arrangement in order to miniaturize the whole apparatus as described later. However, this does not mean that the incident angles of the respective optical couplers 1 A to 1 C are limited to the above value.
[0038] The branched light reflected by the optical coupler 1 A, is here incident directly on a light receiving element 4 4 . Moreover, the branched light reflected by the optical coupler 1 B passes through a polarizer 3 2 letting through only a polarization component inclined by 45° with respect to a preset reference plane, to be incident on a light receiving element 4 2 . As the above reference plane, for example, it is possible to set an arbitrary plane such as a bottom face of a package of the present apparatus as described later. The polarizer 3 2 is arranged to be inclined by a predetermined angle with respect to the light receiving surface of the light receiving element 4 2 so as not to form an interference system by its light emission plane and the light receiving surface of the light receiving element 4 2 .
[0039] The branched light reflected by the optical coupler 1 C passes through a quarter wave plate 2 and a polarizer 3 1 letting through only a polarization component inclined at 45° with respect to the abovementioned reference plane, to be incident on a light receiving element 4 1 . Moreover, the branched light which has passed through the optical coupler 1 C, passes through a polarizer 3 3 letting through only a polarization component parallel (or perpendicular) with respect to the abovementioned reference plane, to be incident on a light receiving element 4 3 . Similarly to the abovementioned polarizer 3 2 , the polarizers 3 1 and 3 3 are each arranged to be inclined by a predetermined angle with respect to the light receiving surfaces of the light receiving elements 4 1 and 4 3 so as not to form interference systems by their respective light emission planes and the respective light receiving surfaces of the light receiving elements 4 1 and 4 3 . Moreover, the quarter wave plate 2 is also arranged to be inclined by a predetermined angle with respect to the light incident plane of the polarizer 3 1 so as not to form an interference system by its light emission plane and the light incident plane of the polarizer 3 1 .
[0040] Furthermore, the present polarization measuring apparatus is provided with a shielding wall 5 blocking a stray light generated between optical elements adjacent to each other arranged on each of branched optical paths P 4 , P 2 and P 1 through which the branched lights reflected by the respective optical couplers 1 A, 1 B and 1 C are propagated, from being propagated toward the light receiving element on another branched optical path, which is different from the branched optical path concemed. Here, for example, a member having an approximately C-shaped cross-section which is laid along both sides of the branched optical path P 2 corresponding to the reflected light of the optical coupler 1 B, is used for this shielding wall 5 . However, the shape of the shielding wall 5 is not limited to the above example, and this can be suitably designed taking into consideration a propagation direction of the stray light as described later.
[0041] Electric signals D Q , D 45 , D 0 and D T indicating the powers of the signal lights received by the respective light receiving elements 4 1 to 4 4 , are sent to a calculating section (not shown here) connected to the outside via a lead wire or the like of the package which accommodates an optical system as described later, and the Stokes parameters S 0 to S 3 and DOP are calculated in accordance with the abovementioned relationships of equation (1) and equation (2) in the calculating section.
[0042] In addition, for example as shown in the cross-sectional view along an optical axis of the input signal light L IN in FIG. 2 , the present polarization measuring apparatus comprises; a single substrate 6 on an upper surface of which are arranged the abovementioned respective optical elements (the optical couplers 1 A to 1 C, the quarter wave plate 2 , the polarizers 3 1 to 3 3 , light receiving elements 4 1 to 4 4 , and the shielding wall 5 ); and a Peltier 7 which is provided in contact with a bottom surface of the substrate 6 . A material such as metal having a coefficient of linear expansion as close as possible to a coefficient of linear expansion of each of the arranged optical elements, is used for the substrate 6 . The Peltier 7 controls the temperature of the substrate 6 so that the temperature of each optical element arranged on the same substrate 6 is not changed. The temperature of the substrate 6 controlled by the Peltier 7 may have differences depending on the location, and the temperature control is performed by the Peltier 7 so that the temperature distribution is not changed.
[0043] Next is a description of an operation of the polarization measuring apparatus having the above configuration.
[0044] In the present polarization measuring apparatus, the input signal light L IN the polarization of which is to be measured, is sequentially incident on the optical couplers 1 A to 1 C in the three stage configuration, and is thus branched into four signal lights having mutually equal powers. At this time, the signal light is given at the incident angle of 22.5° with respect to the light incident plane of each of the optical couplers 1 A to 1 C, so that the phase shift occurred between the p/s waves of each of the transmitted light and the reflected light, is reduced. To be specific, generally, in the case where the signal light is branched using an optical coupler which utilizes a dielectric multi-layer film, then in many cases, from the point of ease of arrangement, the arrangement of the optical coupler is designed so that the reflected light is emitted in a direction of 90° with respect to the incident light as shown in (A) of FIG. 4 . Compared to this arrangement of the optical coupler where the signal light is given at the incident angle of 45°, by adopting the arrangement of the optical coupler where the signal light is given at the incident angle of 22.5° away from the Brewster angle as shown in (B) of FIG. 4 , the phase shift occurred between the p/s waves of the signal light branched by the optical coupler can be reduced to about {fraction (1/3 )} times.
[0045] The three signal lights reflected in a direction at 45° with respect to an incident direction of the input signal light L IN by the optical couplers 1 A to 1 C in the three stage configuration, and the signal light passed through the optical coupler 1 C, are respectively propagated through any one of the first branched optical path P 1 where the quarter wave plate 2 , the polarizer 3 1 and the light receiving element 4 1 are arranged, the second branched optical path P 2 where the polarizer 3 2 and the light receiving element 4 2 are arranged, the third branched optical path P 3 where the polarizer 3 3 and the light receiving element 4 3 are arranged, and the fourth branched optical path P 4 where the polarizer 4 4 is arranged, in order to obtain the four Stokes parameters S 0 to S 3 represented by the relationship of the abovementioned equation (1). For the first to fourth branched optical paths P 1 to P 4 , the number of optical elements through which the signal light passes from when it is branched by the optical coupler until it is received by the light receiving element is two in the first branched optical path P 1 , one in the second and third branched optical paths P 2 and P 3 , and zero in the fourth branched optical path P 4 . Therefore, there occur differences in the necessary optical path lengths for the respective branched optical paths. Consequently, the mounting area of the present apparatus differs depending on which of the first to fourth branched optical paths P 1 to P 4 , the four signal lights branched by the optical couplers 1 A to 1 C are sent to. Therefore, in the present embodiment, in order to realize the minimum mounting area, taking into consideration the above differences in the optical path lengths, the reflected light of the first stage optical coupler 1 A is sent to the fourth branched optical path P 4 , the reflected light of the second stage optical coupler 1 B is sent to the second branched optical path P 2 , the reflected light of the third stage optical coupler 1 C is sent to the first branched optical path P 1 , and the transmitted light of the third stage optical coupler 1 C is sent to the third branched optical path P 3 . Since the optical path length of the second branched optical path P 2 and the optical path length of the third branched optical path P 3 become equivalent, the reflected light of the second stage optical coupler 1 B may be sent to the third branched optical path P 3 , and the transmitted light of the third stage optical coupler 1 C may be sent to the second branched optical path P 2 . The abovementioned arrangement of the optical system is here described as a ‘0121’ type in which the number of optical elements passing through is sequentially represented from the input side. As another arrangement of the optical system capable of realizing a small mounting area, a ‘0112’ type is also useful, although here omitted from the drawing.
[0046] Since a part of the signal light propagated through each of the first to fourth branched optical paths P 1 to P 4 , is reflected when it is incident on the optical element arranged on each of the optical paths, then if a reflecting plane thereof is in parallel or close to parallel with respect to the light emission plane of the optical element on a former stage, an interference system is formed to cause the multi-reflection as shown in FIG. 8 described above. Specifically, locations where the interference system is possibly formed in the arrangement of the optical system shown in FIG. 1 , are between the quarter wave plate 2 and the polarizer 3 1 , and between the polarizer 3 1 and the light receiving element 4 1 on the first branched optical path P 1 , between the polarizer 3 2 and the light receiving element 4 2 on the second branched optical path P 2 , and between the polarizer 3 3 and the light receiving element 4 3 on the third branched optical path P 3 . Therefore, in the present embodiment, for the abovementioned respective locations, as shown in FIG. 3 , the respective optical elements are arranged so that the light emission plane of the optical element on the former stage becomes a state inclined with respect to the light incident plane of the optical element on a latter stage (an approximately inverted V-shape). It is desirable to design inclination angles of the opposing light incident and emission planes so as not to generate the substantial multi-reflection, taking into consideration characteristics of the respective optical elements and beam diameters of the signal lights passing therethrough. By having such an approximate inverted V-shape arrangement, it becomes possible to avoid the formation of interference system. However, as shown in FIG. 3 , there is a possibility that the reflected light becomes a stray light to be incident on the light receiving element on another branched optical path. Therefore, here the shielding wall 5 is provided in order to prevent the propagation of stray light as mentioned above.
[0047] FIG. 5 is a plan view showing a specific arrangement example of the respective optical elements taking into consideration the formation of interference system and the propagation of stray light as mentioned above. However, the arrangement of the optical system in the present invention is not limited to this example.
[0048] In the arrangement example of FIG. 5 , assuming that one side face (the top side plane in FIG. 5 ) of the package in which the respective optical elements of the present apparatus are accommodated, is a reference plane of arrangement angle, the input signal light L IN is incident in parallel on the reference plane. The light receiving surfaces of the respective light receiving elements 4 1 , 4 2 , and 4 4 which receive the branched lights reflected in a direction of 45° by the respective optical couplers 1 A to 1 C, are inclined by 41° with respect to the reference plane, and the light receiving surface of the light receiving element 4 3 which receives the branched light transmitted over the optical coupler 1 C, is inclined by 94° with respect to the reference plane.
[0049] Moreover, the light incident and emission planes of the quarter wave plate 2 located on the first branched optical path P 1 are inclined by 42° with respect to the reference plane, and the light incident and emission planes of the polarizer 3 1 are inclined by 43° with respect to the reference plane. Therefore, the light incident and emission planes between the quarter wave plate 2 , and the polarizer 3 1 and the light incident and emission planes between the polarizer 3 1 and the light receiving element 4 1 , become nonparallel and attain the state as shown in FIG. 3 . The stray light generated between the polarizer 3 1 and the light receiving element 4 1 , is propagated to the second branched optical path P 2 side. However, the stray light is blocked by the shielding wall 5 located between the first and second branched optical paths P 1 and P 2 and is not received by the light receiving element 4 2 . The stray light generated between the quarter wave plate 2 and the polarizer 3 1 is propagated to the opposite side to second branched optical path P 2 side. However, since a light receiving element of another branched optical path does not exist in this direction, a shielding wall for blocking the stray light is not specially provided. However, in the case where it is necessary to consider the reflection of stray light at the package side face, a shielding wall may be provided in the vicinity of the quarter wave plate 2 and the polarizer 3 1 in order to block the propagation of stray light.
[0050] Furthermore, the light incident and emission planes of the polarizer 3 2 located on the second branched optical path P 2 are also inclined by 43° with respect to the reference plane. Therefore, the respective light incident and emission planes between the polarizer 3 2 and the light receiving element 4 2 become nonparallel and attain the state as shown in FIG. 3 . The stray light generated between the polarizer 3 2 and the light receiving element 4 2 is propagated to the fourth branched optical path P 4 side. However, the stray light is blocked by the shielding wall 5 located between the second and fourth branched optical paths P 2 and P 4 and is not received by the light receiving element 4 4 . In addition, the light incident and emission planes of the polarizer 3 3 located on the third branched optical path P 3 are inclined by 92° with respect to the reference plane. Therefore, the respective light incident and emission planes between the polarizer 3 3 and the light receiving element 4 3 become nonparallel and attain the state as shown in FIG. 3 .
[0051] When the respective optical elements are actually arranged on the above locations, it is preferable to verify the location accuracy utilizing a technique such as image processing. By performing such verification, it becomes possible to reduce the deterioration of measurement accuracy due to manufacturing errors.
[0052] The numerical values in brackets shown in the abovementioned FIG. 5 denote the dimensions of the respective optical elements. The dimensions of the respective optical elements used in the present embodiment are exemplified as width×height×depth (mm), in which each of the optical couplers 1 A to 1 C is 2×2×1, the quarter wave plate 2 is 2×2×1.5, each of the polarizers 3 1 to 3 3 is 2×2×0.5, and each of the light receiving elements 4 1 to 4 3 is 1.6×2.55×1. By applying the respective optical elements of the abovementioned dimensions and the ‘ 0121 ’ type optical system as above described, it becomes possible to accommodate the optical system inside a package with internal dimensions of width×height of 9.5×20 (mm) for example.
[0053] FIG. 6 is a diagram showing an external appearance of the polarization measuring apparatus accommodated in the package as mentioned above. Here, a cap on the package top face is omitted in order to show the appearance inside the package. In this manner, it is possible to use a greatly miniaturized butterfly-type general-purpose package for the present polarization measuring apparatus. Moreover, here it becomes difficult for noise to enter into the monitor signals D Q , D 45 , D 0 , and D T , by taking out the signals D Q , D 45 , D 0 , and D T output from the respective light receiving elements 4 1 to 4 4 , from lead terminals located on one side of the package, and by collecting together control system terminals which carry a large current, such as temperature control terminals of the Peltier 7 , at lead terminals located on the other side of the package,. By performing such mounting, the Stokes parameters S 0 to S 3 and the DOP can be measured with higher accuracy. In addition to this, although not specifically shown in the figure here, if circuits connected up to the respective light receiving elements 41 to 44 inside the package are arranged as far apart from the other circuits as possible, it becomes possible to reduce an influence of noise more effectively.
[0054] According to the polarizaton measuring apparatus of the present embodiment as described above, the optical elements adjacent to each other on the same branched optical path are arranged to be inclined to each other, to avoid the formation of interference system, and the stray light generated between the optical elements arranged to be inclined is blocked by the shielding wall 5 to be prevented from reaching the optical elements on another branched optical path, so that the signal light powers can be accurately and stably detected in the respective optical elements 4 1 to 4 4 . Therefore, it becomes possible to measure the Stokes parameters and the DOP with extremely high accuracy. Moreover, the incident angle of the signal light to each of the optical couplers 1 A to 1 C in the three stage configuration is away from the Brewster angle, so that the phase shift occurred between the p/s waves of the branched light is reduced. Therefore, it becomes possible to measure the polarizaton of the input signal light with higher accuracy. Furthermore, by making the arrangement of the optical system as the ‘0121’ type or the ‘0112’ type, the entire apparatus can be miniaturized. In addition, the respective optical elements constituting the above optical system are arranged on the same substrate 6 , and the temperature of the substrate 6 is controlled by the Peltier 7 . Therefore, it becomes possible to reduce the deterioration of measurement accuracy due to the temperature fluctuation. Moreover, the signal system terminals and the control system terminals are arranged separately with lead terminals on opposite sides of the package, so that there is less likelihood of influence of noise. Therefore, it becomes possible to measure the polarization of the input signal light with even higher accuracy. Such a miniaturized polarization measuring apparatus having superior measurement accuracy is useful in enhancing the high performance and miniaturization of various measuring devices which are required to detect the polarization of signal light accurately at high speed, such as, a monitoring section used to determine a compensation amount in a PMDC (polarization mode dispersion compensator), for example.
[0055] In the above embodiment, the description has been made such that in the first to fourth branched optical paths P 1 to P 4 , there occur differences in the necessary optical path lengths corresponding to the number of arranged optical elements. However, in the case where the deterioration of measurement accuracy due to the differences in the optical path lengths becomes a problem, it is desirable to improve the configuration of the optical system in order to temporally match the phases on the respective branched optical paths. Specifically, for example, in order to match with the optical path length of the first branched path P 1 which needs the longest optical path length, the light receiving elements 4 2 to 4 4 on the other branched optical paths P 2 to P 4 may be arranged apart, or delay elements such as birefringent crystal may be inserted in the respective branched optical paths P 1 to P 4 to equalize the respective effective optical path lengths.
[0056] Moreover, the description has been made such that the respective Stokes parameters S 0 to S 3 are calculated in accordance with the relationship of equation (1) using the signals D Q , D 45 , D 0 , and D T detected by the respective light receiving elements 4 1 to 4 4 . However, a determinant for correcting variations of the characteristics or arrangements of the respective optical elements may be obtained in advance, and the respective Stokes parameters S O to S 3 then calculated using the determinant and the values of the actually measured signals D 0 , D 45 , D 0 , and D T . By performing such correction processing, it becomes possible to effectively reduce the deterioration of measurement accuracy due to manufacturing errors or the like. | The invention aims to provide a miniaturized polarization measuring apparatus which can measure the polarization of input signal light with high accuracy, even in an optical system where a plurality of light receiving elements are arranged adjacent to each other. To this end, in the polarization measuring apparatus which branches the input signal light into four signal lights by optical couplers in a three stage configuration, and provides the signal lights with polarizations and the phase shifts, which are different for each signal light, by a plurality of optical elements arranged on branched optical paths, and detects the signal light powers by corresponding light receiving elements, and calculates the Stokes parameters or the like, based on the detection results, to thereby measure the polarization of the input signal light, the elements are arranged to be inclined to each other, so that an interference system is not formed between the adjacent elements on the same branched optical path, and also there is provided a shielding wall so that a stray light generated between these elements does not reach the light receiving element on another branched optical path. | 6 |
BACKGROUND OF THE INVENTION
This invention relates to a refractory composition containing a basic refractory material and suitable for preparing refractories.
In the art of steel making, the open hearth process and the bottom-blown converter process have been gradually substituted by the pure oxygen top-blown converter process due to the development of the latter. With an extensive increase in the production quantity of crude steel, the demand for basic refractories has also been increased greatly, with the result that the demand for dolomite clinker and dolomite magnesia clinker which are used as the raw materials for preparing basic refractories in such converter furnaces has also been increased. For this reason, it is a recent trend that acidic refractories are substituted by basic refractories in most cases.
When molding refractories, where the binding force of the raw material refractory substance itself is low, various types of binders are added. Silica sol is an excellent binder. When silica sol is used as a binder it is possible to obtain excellent refractories owing to its strong bonding force manifested by it at the time of hardening and the refractive property of silica. Where a basic refractory raw material, for example magnesia clinker, is mixed with silica sol for molding basic refractories, the silica sol almost instantly gels so that it is difficult to obtain molded products of high mechanical strength. Even when molded under a high pressure and subsequently dried or fired, the mechanical strength of the dried or fired molded products is extrememly low because the bonding force of the silica sol has not been manifested. For this reason, it has been generally recognized that use of silica sol is not effective for the raw material of basic refractories.
Water glass such as potassium-, sodium-, lithium-silicate, etc. has also been used as the binder for basic refractories. However, since water glass contains a large quantity of alkali metals, molded refractories using water glass are difficult to sufficiently dry and have a high tendency toward deliquescence and slaking. Moreover, the refractoriness of such molded articles is low. For this reason, the field of application of the refractories using water glass is limited.
It has been proposed to use guanidine silicate as a silica type binder as disclosed in the specification of Japanese patent publication No. 128 of 1970. However, not only is the supply source of guanidine silicate limited as an industrial material, but also the mechanical strength of basic refractories using this binder is not so high.
Magnesium chloride, tar etc. are also used as the binder for basic refractories, but the mechanical strength after drying of basic refractory raw material using such binders is low so that sufficiently high mechanical strength can not be attained unless the molded articles are fired. Where tar is used, it has been recognized that the mechanical strength decreases unexpectedly when the molded articles are fired at a temperature of about 800°C. Where magnesium cloride is used the molded refractories have a tendency toward deliquescence and slaking.
Accordingly, it will be highly valued to obtain refractories having a high mechanical strength and not manifesting the properties of deliquescence and slaking by using a silica type binder for basic refractory raw materials.
SUMMARY OF THE INVENTION
It is an object of this invention to provide a refractory composition which contains a basic refractory raw material, and which can form refractories having a sufficiently high compression strength by merely molding and drying it and is not required to be fired.
A further object of this invention is to provide a novel refractory composition containing a basic refractory raw material selected from the group consisting of an oxide or hydroxide of magnesium, calcium, chromium or manganese or mixtures thereof, and utilized to form unfired refractories having a high refractoriness and not manifesting the properties of deliquescence and slaking.
The refractory composition of this invention is characterized by comprising a basic refractory raw material, a quaternary ammonium hydroxide expressed by a general formula ##EQU1## wherein R 1 , R 2 , R 3 and R 4 respectively represent alkyl radicals or hydroxy alkyl radicals having 1 to 4 carbon atoms, and a silica component which is a (1) silica sol utilizing a dispersion medium consisting of water, a hydrophilic organic solvent or a mixture thereof and/or (2) an alkyl or alkali silicate.
The basic refractory raw materials selected from the group consisting of oxides or hydroxides of magnesium, calcium, chromium or manganese are used commercially as basic or neutral refractory raw materials in the form of lumps, granules, fine particles, and fibers.
The oxide or hydroxide of magnesium has been generally used as the gelation agent for silica sol, but in this invention, these materials are not used as gelation agents but used as the essential component for imparting a high mechanical strength to the molded refractories.
The quaternary ammonium hydroxide used to form the composition of this invention is expressed by a general formula ##EQU2## wherein R 1 , R 2 , R 3 and R 4 respectively represent alkyl radicals or hydroxy alkyl radicals having 1 to 4 carbon atoms. The most suitable quaternary ammonium hydroxides include those in which R 1 through R 4 represent alkyl radicals or hydroxy alkyl radicals having 1 to 3 carbon atoms, for example, methyl, ethyl, propyl, hydroxymethyl, hydroxyethyl, and hydroxypropyl radicals. Accordingly, examples of the cationic groups of the quaternary ammonium hydroxide are [(C 2 H 4 OH) 2 .N.(CH 3 ) 2 ], [(C 2 H 4 OH) 3 .N.CH 3 ] and [(C 2 H 4 OH) 4 .N].
The silica sol utilized to form the composition of this invention means silica sol dispersed in water, or hydrophilic organic solvents or a mixture thereof as the dispersing medium. The preferred silica sol is aqueous silica sol, methanol silica sol, ethanol silica sol, water-methanol silica sol, etc. These silica sols can be prepared from alkali silicate by cation exchange process, or by the degelation of silica gel. There is no limitation of the particle size, pH and the ratio of SiO 2 /Me 2 O of the silica sol, where Me represents the atom of a monovalent alkali metal.
The silicate utilized to prepare the composition of this invention means alkyl silicate and alkali silicate. The preferred alkyl silicate is ethyl silicate, or ethyl silicate which is partially hydrolyzed and contains silica sol. The alkali metal in the alkali silicate may be lithium, postassium, or sodium.
Silica sol and silicate containing from about 10 to 45% by weight of silica are suitable to prepare the composition of this invention.
In the preparation of the novel composition any order of admixing the respective components may be used except that the silica sol and/or silicate should be admixed with the quaternary ammonium hydroxide before or concurrently with the incorporation of the silica sol and/or silicate into the basic refractory raw material. For example, after incorporation of the quaternary ammonium hydroxide into the basic refractory raw material, the silica sol and/or silicate may be incorporated. Alternatively, the basic refractory raw material may be added to and mixed with a liquid mixture of the quaternary ammonium hydroxide and the silica sol and/or silicate. Where another refractory raw material, auxiliary agent or the like is incorporated as will be described later, they can be incorporated at any stage, provided that said basic order of mixing is followed.
The foregoing description means that the object of this invention can also be attained even when other components are added after the quaternary ammonium hydroxide and silica sol and/or silicate have been mixed together and have been caused to react with each other to form quaternary ammonium silicate. This fact was confirmed by experiments. For this reason, within the scope of this invention is also included a composition containing said basic refractory raw material and quaternary ammonium silicate.
In the composition of this invention prepared by admixing various constituents it is essential that the respective constituents are homogeneously admixed and that the concentrations of the quaternary ammonium hydroxide, silica sol and or silicate, the quantity of water added, etc. should be adjusted such that the resulting composition is a slurry and wet or only slightly wet (nearly dried state), although somewhat different depending upon the application of the composition. When refractories are prepared by molding the composition of this invention, after drying, the molded articles have an extrememly high mechanical strength if the quantity of water is reduced as far as possible.
The preferred ratio of the components necessary to obtain compositions of high mechanical strength is from 0.1 to 200 parts by weight of silica sol and/or silicate in terms of SiO 2 , per 100 parts by weight of the basic refractory raw material, and is from 0.001 to 4 moles of quaternary ammonium hydroxide per mole of SiO 2 contained in the silica sol and/or silicate.
After mixing the components, the composition of this invention retains sufficiently high workability until it is molded. Although after molding the molded article hardens naturally, when the molded article is dried at normal temperature or at a low temperature less than 300°C, its mechanical strength can be greatly improved. The resulting molded article shows an apparent specific gravity of from 1.2 to 3.6 and a compression strength of from 100 to 800 kg/cm 2 , although these characteristics vary depending upon the nature and grain size distribution of the raw material powder and molding pressure. Even when the molded article is fired at a higher temperature, the cold compression strength does not increase greatly as in conventional refractories but the strength does not increase to any appreciable extent. Thus, the novel composition of this invention is characterized in that it can produce refractories having sufficiently high compression strength by mere low temperature drying. It is to be particularly noted that while the conventional refractory composition incorporated with tar or other organic binders decreases its cold compression strength when the articles manufactured by molding such composition are fired at a temperature of from 600° to 1300°C, the molded articles of the novel composition of this invention do not decrease their strength even when they are fired at such high temperatures.
Basic, neutral or acidic refractories such as brick, monolithic refractories and molded and hardened refractory mortar prepared from the novel commposition of this invention have an excellent characteristic that they always have high mechanical strength when they are dried at normal temperature or then fired at elevated temperature.
In addition to these principal ingredients described above, the composition of this invention can also be incorporated with other refractory raw materials such as powdered silica, alumina, chamotte, silicon carbide, boron nitride, etc.; a viscosity improver, for example, polyacrylic acids or their salts, polyethylene oxides, polyvinyl alcohol, phenol resin, bentonite, magnesium montmorillonite, etc.; a foaming agent; a surface active agent; and an auxiliary binder, for example alumina sol, aluminum biphosphate, basic aluminum halides, basic aluminum organic salt, zirconium oxide, etc. Especially, where a pyrolyzable foaming agent which does not gelate the composition is incorporated into the composition of this invention, it is possible to obtain excellent refractories capable of resisting shrinkage. The use of hydrogen sodium carbonate, ammonium carbonate etc., is not advantageous because they convert the composition into a gel, but azodicarbonamide is a preferred foaming agent.
The composition of this invention can be used to prepare fired or not fired basic refractories such as magnesia bricks, magnesia chromia bricks, etc; light weight magnesia bricks, basic monolithic refractories, inorganic boards; refractory coating materials (mastic coating material) for heavy coating on building walls; refractory coating materials, refractory slurries for shaping casting molds, coating materials for molds, etc. The neutral or acidic refractories incorporated with the basic refractory raw materials described above are one of the important applications of the novel composition of this invention.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
The following examples are given to aid better understanding of this invention, but it should be understood that the invention is by no means limited to these specific examples.
EXAMPLE 1
100 parts by weight of 20 mesh magnesia clinker and 60 parts by weight of 300 mesh magnesia clinker were mixed together in a mixer, and thereafter 10 parts by weight of monomethyl-triethanol ammonium hydroxide and 20 parts by weight of water were added to the mixture. After thoroughly stirring the resulting mixture, 30 parts by weight of aqueous silica sol containing 30% by weight of SiO 2 (sold under the trade name of Snowtex 30 by Nissan Chemical Industries, Ltd.) was incorporated and kneaded for about 5 minutes to obtain the composition of this invention which is somewhat wet and powdery. This composition was stamped 20 times in a molding machine for casting sand and the stamped composition was shaped into cylindrical test pieces each having a diameter of 50 mm and a height of 50 mm. After drying the test pieces at room temperature, they were fired for two hours at four different temperatures of 120°C, 300°C, 800°C and 1400°C, respectively.
For comparison, a composition of the present invention wherein the quaternary ammonium hydroxide alone is not incorporated, a composition incorporated with guanidine instead of the quaternary ammonium hydroxide and a composition utilizing sodium silicate containing 30% of SiO 2 as the binder and not utilizing quaternary ammonium hydroxide were also tested and the results of the tests are shown in the following Table 1.
Table 1__________________________________________________________________________Additive to mag- Comp. Strength (kg/cm.sup.2) at 25°Cnesia clinker(parts by weight) Treating temperaturequaternaryammoniumhydroxide binder Normal 120°C 300°C 800°C 1400°Cor substi- temp.tuent__________________________________________________________________________Test monomethyl silicapiece trietha- sol 125 280 265 225 256No.1 nol ammo- nium (10) (30)__________________________________________________________________________ tetra-No. 2 ethanol silica 105 232 228 208 235 ammonium sol (10) (30)__________________________________________________________________________Cont- silicarol -- sol 28 32 41 32 112No.1 (30)__________________________________________________________________________ guani- silicaNo.2 dine sol 35 50 48 42 85 (10) (30)__________________________________________________________________________ sodiumNo.3 -- silica- 15 122 158 185 * te (30)__________________________________________________________________________ *Impossible to measure because this control piece has deformed at the tim of heat treatment.
As can be noted from Table 1, the prior art compositions shown as control Nos. 1 to 3 have a tendency of increasing the compression strength as the firing temperature increases and the maximum value of their compression strength is at most comparable or less than that of the novel composition when it is dried at normal temperature. In contrast, articles utilizing the composition of this invention have sufficiently high strength even when they are dried at normal temperature. Table 1 also shows that when dried at a slightly higher temperature, for example 120°C, they manifest extremely high strength and that even when they are fired at a higher temperature they manifest substantially the same strength.
EXAMPLE 2
4 kg of magnesium clinker (40:60 mixture of 200 mesh pass and 400 mesh pass) was put into a mixer and 2 kg of an aqueous solution of dimethyldiethanol ammonium silicate containing 40% by weight of SiO 2 and 10% by weight of dimethyldiethanol ammonium hydroxide, and 5 g of azodicarbonamide (foaming agent) were added to the magnesium clinker while stirring. After kneading for 3 minutes, the resulting mixture was charged into a wooden mold for molding normal bricks as specified by JIS and having an inner volume of 1720 ml. A lid was applied to the mold and the mold was left to stand for one day at room temperature thus hardening the mixture. When released from the wooden mold, the resulting brick resembled an extremely hard concrete brick. When the brick was dried for 45 hours at a temperature of 150°C, an unfired light weight magnesia brick was obtained having an apparent specific gravity of 2.5 and a compression strength of 310 kg/cm 2 .
An unfired brick prepared by the same process as above described except that the 18 mesh magnesia clinker was substituted by 18 mesh chamotte powder, had an apparent specific gravity of 2.4 and a compression strength of 232 kg/cm 2 . When the brick was fired at a temperature of 130°C, it did not shrink to any appreciable extent and had a compression strength of 240 kg/cm 2 .
Conventional refractories shrink during drying and firing after they have been molded due to the release of free water, crystallization water and volatile impurities, stabilization of the volume, and the changes of the minerals, etc. It is surprising that the refractory of this example does not shrink and shows a high compression strength. It is presumed that this is caused by a strong bonding force of the binder utilized in the composition of this invention which is sufficient to overcome the shrinking force of the refractory material which is generated during the drying and firing thereof and by the fact that the swelling of the material caused by the foaming of azodicarbonamide compensates for the shrinkage while the bonding force of the binder is not effective or while the composition is still in the plastic state before hardening.
In the fabrication of a furnace, it is possible to fabricate the wall thereof by merely pouring a slurry of this composition in a wooden framework and then hardening the composition like a normal concrete slurry, instead of piling up bricks.
A flat plate prepared by pouring the slurry into a metal mold for manufacturing flat plates and having a dimension of 300 mm × 300 mm × 16 mm, followed by hardening and drying for 24 hours at at temperature of 120°C had properties suitable for use as building material.
EXAMPLE 3
100 parts by weight of 20 mesh pass chamotte powder, 50 parts by weight of a fine powder of agalmatolite and 3 parts by weight of manganese oxide were charged in a ball mill, and then 8 parts by weight of trimethyl monopropyl ammonium hydroxide, 40 parts by weight of water and 5 parts by weight of a powder of precipitated silica were added. The resulting mixture was kneaded for 72 hours to obtain a viscous slurry. During kneading the precipitated silica powder was degelled and converted into a sol which was then caused to react with quaternary ammonium hydroxide to produce quaternary ammonium silicate. 2 parts by weight of a mixture of magnesium oxide and calcium oxide was added to the slurry and then kneaded to obtain a wet powder. This powder has an extremely satisfactory moldability when used as monolithic refractories and when it is stamped and dried at a temperature of from room temperature to 300°C, refractory material having a compression strength higher than 50 kg/cm 2 was obtained. It was found that this refractory material has excellent properties suitable for use as joints for bricks in a furnace and runner, repair material. A slurry obtained by diluting this monolithic material with an equal quantity of water before drying and hardening is suitable to be used as a mold releasing agent when forming ingots of iron and non-ferrous metals.
4 parts by weight of an aqueous solution of potassium silicate was added to the composition of this example. The resulting mixture was treated in the same manner as described above. It was found that when the product was fired at a temperature of 600°C to 1100°C its compression strength was increased greatly. In contrast, when trimethyl monopropylalcohol ammonium hydroxide was omitted, the composition had no plasticity and pulverized even when it was stamped. Thus such composition could not be used.
EXAMPLE 4
2 kg of 325 mesh pass fired alumina, 1 kg of 200 mesh pass magnesia powder, 40 g of bentonite, 20 g of polyvinyl alcohol, 2 g of azodicarbonamide and 15 g of expandable styrene beads were mixed together in a mixer. 4 kg of active silica sol containing 3% of SiO 2 obtained immediately after dealkalizing sodium silicate by ion exchange process and 80 g of dimethyldiethanol ammonium hydroxide were mixed together and caused to react by heating. The reaction product was concentrated to obtain 400 g of a solution of dimethyl diethanol ammonium silicate containing 30% of SiO 2 . This solution was added to the mixture in the mixer and the resulting mixture was kneaded to obtain a slurry having a viscosity of 4800 centipoise. The slurry was uniformly poured into a metal mold for casting normal bricks and having a volume of 1720 ml. After applying the lid the mold was heated for one day at a temperature of 120°C thereby causing the slurry to foam and harden.
After being released from the metal mold, the hardened brick was heated for 24 hours at a temperature of 120°C. The resulting brick had an apparent specific gravity of 1.8. This brick had a high compression strength both before and after additional firing carried out at a temperature of 1450°C, as shown in the following Table 2. There is no difference in the strength between portions near the side surface and the central portion of the brick. Thus, the strength of the brick is uniform at all portions.
A control brick was prepared in substantially the same manner except that the magnesia powder was substituted by an equal amount of a 200 mesh pass powder of fired alumina. The apparent specific gravity of the control brick was 1.85 and its compression strength was much smaller than that of the brick utilizing magnesia powder as shown in Table 2.
Table 2______________________________________ Compression strength (Kg/cm.sup.2) temp. ofBase material treatment end cemter (°C)______________________________________ fired alumina 120 80 80Embodiment and magnesia 1450 125 123______________________________________ fired alumina 120 35 22Control alone 1450 82 34______________________________________
EXAMPLE 5
Equal quantities of coarse powder of chamotte, zircon flour, a fine powder of magnesia and a fine powder of alumina rich chamotte were mixed together and while mixing 500 g of this mixture in a mixer, 300 g of monomethyl triethanol ammonium silicate containing 35% of SiO 2 and 0.5 g of an aqueous solution of sodium polyacrylate were incorporated into the mixer and kneaded, while kneading 40 g of 10% ammonium carbonate solution was added and the mixture was immediately poured into a cavity defined by a rear mold and a model. 15 minutes later, the model was removed and its surface was compelled to be dried by heating it with a burner. However, it was found that the surface of the mold was not coarsened. The mold not heated by the burner but merely left to stand for one day also had no crack.
While the invention has been described in terms of some preferred embodiments it should be understood that the invention is not limited to these specific embodiments. | A refractory composition comprises a basic refractory raw material such as oxides or hydroxides of magnesium, calcium, chromium or maganese, quaternary ammonium hydroxide and silica sol and/or silicate. The composition is used to prepare unfired refractories having a high compression strength by merely molding and drying it without the necessity of firing. When fired, it manifests comparable compression strength. The composition can also be used as monolithic refractory, refractory mortar, refractory coating agent, mold release, etc. | 2 |
BACKGROUND OF THE INVENTION
[0001] The present invention relates to novel cationic lipids that can be used in combination with other lipid components such as cholesterol and PEG-lipids to form lipid nanoparticles with oligonucleotides, to facilitate the cellular uptake and endosomal escape, and to knockdown target mRNA both in vitro and in vivo.
[0002] Cationic lipids and the use of cationic lipids in lipid nanoparticles for the delivery of oligonucleotides, in particular siRNA and miRNA, have been previously disclosed. Lipid nanoparticles and use of lipid nanoparticles for the delivery of oligonucleotides, in particular siRNA and miRNA, has been previously disclosed. Oligonucleotides (including siRNA and miRNA) and the synthesis of oligonucleotides has been previously disclosed. (See US patent applications: US 2006/0083780, US 2006/0240554, US 2008/0020058, US 2009/0263407 and US 2009/0285881 and PCT patent applications: WO 2009/086558, WO2009/127060, WO2009/132131, WO2010/042877, WO2010/054384, WO2010/054401, WO2010/054405 and WO2010/054406). See also Semple S. C. et al., Rational design of cationic lipids for siRNA delivery, Nature Biotechnology, published online 17 Jan. 2010; doi:10.1038/nbt.1602.
[0003] Other cationic lipids are disclosed in US patent applications: US 2009/0263407, US 2009/0285881, US 2010/0055168, US 2010/0055169, US 2010/0063135, US 2010/0076055, US 2010/0099738 and US 2010/0104629.
[0004] Traditional cationic lipids such as CLinDMA and DLinDMA have been employed for siRNA delivery to liver but suffer from non-optimal delivery efficiency along with liver toxicity at higher doses. It is an object of the instant invention to provide a cationic lipid scaffold that demonstrates enhanced efficacy along with lower liver toxicity as a result of lower lipid levels in the liver. The present invention employs low molecular weight cationic lipids with one short lipid chain to enhance the efficiency and tolerability of in vivo delivery of siRNA.
SUMMARY OF THE INVENTION
[0005] The instant invention provides for novel cationic lipids that can be used in combination with other lipid components such as cholesterol and PEG-lipids to form lipid nanoparticles with oligonucleotides. It is an object of the instant invention to provide a cationic lipid scaffold that demonstrates enhanced efficacy along with lower liver toxicity as a result of lower lipid levels in the liver. The present invention employs low molecular weight cationic lipids with one short lipid chain to enhance the efficiency and tolerability of in vivo delivery of siRNA.
BRIEF DESCRIPTION OF THE FIGURES
[0006] FIG. 1 : LNP (Compound 1) efficacy in mice.
[0007] FIG. 2 . LNP (Compound 1) efficacy in rat (ApoB siRNA).
[0008] FIG. 3 . Cationic lipid (Compound 1) levels in rat liver.
DETAILED DESCRIPTION OF THE INVENTION
[0009] The various aspects and embodiments of the invention are directed to the utility of novel cationic lipids useful in lipid nanoparticles to deliver oligonucleotides, in particular, siRNA and miRNA, to any target gene. (See US patent applications: US 2006/0083780, US 2006/0240554, US 2008/0020058, US 2009/0263407 and US 2009/0285881 and PCT patent applications: WO 2009/086558, WO2009/127060, WO2009/132131, WO2010/042877, WO2010/054384, WO2010/054401, WO2010/054405 and WO2010/054406). See also Semple S. C. et al., Rational design of cationic lipids for siRNA delivery, Nature Biotechnology, published online 17 Jan. 2010; doi:10.1038/nbt.1602.
[0010] The cationic lipids of the instant invention are useful components in a lipid nanoparticle for the delivery of oligonucleotides, specifically siRNA and miRNA.
[0011] In a first embodiment of this invention, the cationic lipids are illustrated by the Formula A:
[0000]
[0000] wherein:
[0012] R 1 and R 2 are independently selected from H, (C 1 -C 6 )alkyl, heterocyclyl, and polyamine, wherein said alkyl, heterocyclyl and polyamine are optionally substituted with one to three substituents selected from R′, or R 1 and R 2 can be taken together with the nitrogen to which they are attached to form a monocyclic heterocycle with 4-7 members optionally containing, in addition to the nitrogen, one or two additional heteroatoms selected from N, O and S, said monocyclic heterocycle is optionally substituted with one to three substituents selected from R′;
[0013] R 3 is selected from H and (C 1 -C 6 )alkyl, said alkyl optionally substituted with one to three substituents selected from R′;
[0014] R′ is independently selected from halogen, R″, OR″, SR″, CN, CO 2 R″ and CON(R″) 2 ;
[0015] R″ is independently selected from H and (C 1 -C 6 )alkyl, wherein said alkyl is optionally substituted with halogen and OH;
[0016] n is 0, 1, 2, 3, 4 or 5; and
[0017] L 1 and L 2 are independently selected from C 3 -C 24 alkyl and C 3 -C 24 alkenyl, said alkyl and alkenyl are optionally substituted with one or more substituents selected from Rt;
[0018] or any pharmaceutically acceptable salt or stereoisomer thereof.
[0019] In a second embodiment, the invention features a compound having Formula A, wherein:
[0020] R 1 and R 2 are each methyl;
[0021] R 3 is H;
[0022] n is 0;
[0023] L 1 is selected from C 3 -C 24 alkyl and C 3 -C 24 alkenyl; and
[0024] L 2 is selected from C 3 -C 9 alkyl and C 3 -C 9 alkenyl;
[0025] or any pharmaceutically acceptable salt or stereoisomer thereof.
[0026] In a third embodiment, the invention features a compound having Formula A,
[0000] wherein:
[0027] R 1 and R 2 are each methyl;
[0028] R 3 is H;
[0029] n is 0;
[0030] L 1 is selected from C 3 -C 9 alkyl and C 3 -C 9 alkenyl; and
[0031] L 2 is selected from C 3 -C 24 alkyl and C 3 -C 24 alkenyl;
[0032] or any pharmaceutically acceptable salt or stereoisomer thereof.
[0033] In a fourth embodiment, the invention features a compound having Formula A,
[0000] wherein:
[0034] R 1 and R 2 are each methyl;
[0035] R 3 is H;
[0036] n is 1;
[0037] L 1 is selected from C 3 -C 24 alkyl and C 3 -C 24 alkenyl; and
[0038] L 2 is selected from C 3 -C 9 alkyl and C 3 -C 9 alkenyl;
[0039] or any pharmaceutically acceptable salt or stereoisomer thereof.
[0040] In a fifth embodiment, the invention features a compound having Formula A,
[0000] wherein:
[0041] R 1 and R 2 are each methyl;
[0042] R 3 is H;
[0043] n is 2;
[0044] L 1 is selected from C 3 -C 24 alkyl and C 3 -C 24 alkenyl; and
[0045] L 2 is selected from C 3 -C 9 alkyl and C 3 -C 9 alkenyl;
[0046] or any pharmaceutically acceptable salt or stereoisomer thereof.
[0047] Specific cationic lipids are:
(2S)—N,N-dimethyl-1-[(9Z,12Z)-octadeca-9,12-dien-1-yloxy]undecan-2-amine (Compound 1); (2S)-1-[(9Z,12Z)-octadeca-9,12-dien-1-yloxy]undecan-2-amine (Compound 2); (2S)-1-[(9Z,12Z)-octadeca-9,12-dien-1-yloxy]dodecan-2-amine (Compound 3); (2R)-1-[(9Z,12Z)-octadeca-9,12-lien-1-yloxy]dodecan-2-amine (Compound 4); (2S)-1-[(9Z,12Z)-octadeca-9,12-dien-1-yloxy]decan-2-amine (Compound 5); (2S)-1-[(9Z,12Z)-octadeea-9,12-dien-1-yloxy]nonan-2-amine (Compound 6); (2S)—N,N-dimethyl-1-[(9Z,12Z)-octadeca-9,12-dien-1-yloxy]tridecan-2-amine (Compound 7); (2S)—N,N-dimethyl-1-[(9Z,12Z)-octadeca-9,12-dien-1-yloxy]nonan-2-amine (Compound 8); (2R)—N,N-dimethyl-1-[(9Z,12Z)-octadeca-9,12-dien-1-yloxy]dodecan-2-amine (Compound 9); (2S)—N,N-dimethyl-1-[(9Z,12Z)-octadeca-9,12-dien-1-yloxy]dodecan-2-amine (Compound 10); (2S)—N,N-dimethyl-1-[(9Z,12Z)-octadeca-9,12-dien-1-yloxy]decan-2-amine (Compound 11); and (2S,12Z,15Z)-N,N-dimethyl-1-(octyloxy)henicosa-12,15-dien-2-amine (Compound 12); (2R,12Z,15Z)-1-(decyloxy)-N,N-dimethylhenicosa-12,15-dien-2-amine (Compound 13); (2R,12Z,15Z)-1-(hexyloxy)-N,N-dimethylhenicosa-12,15-dien-2-amine (Compound 14); (2R,12Z,15Z)-1-(hexadecyloxy)-N,N-dimethylhenicosa-12,15-dien-2-amine (Compound 15); (2R,12Z,15Z)-N,N-dimethyl-1-(undecyloxy)henicosa-12,15-dien-2-amine (Compound 16); N,N-dimethyl-2-{[(9Z,12Z)-octadeca-9,12-dien-1-yloxy]methyl}undecan-1-amine (Compound 17); N,N-dimethyl-3-{[(9Z,12Z)-octadeca-9,12-dien-1-yloxy]methyl}dodecan-1-amine (Compound 18); and (2S)—N,N-dimethyl-1-({8-[(1R,2R)-2-{[(1S,2S)-2-pentylcyclopropyl]methyl}cyclopropyl]octyl}oxy)tridecan-2-amine (Compound 19);
or any pharmaceutically acceptable salt or stereoisomer thereof.
[0067] In another embodiment, the cationic lipids disclosed are useful in the preparation of lipid nanoparticles.
[0068] In another embodiment, the cationic lipids disclosed are useful components in a lipid nanoparticle for the delivery of oligonucleotides.
[0069] In another embodiment, the cationic lipids disclosed are useful components in a lipid nanoparticle for the delivery of siRNA and miRNA.
[0070] In another embodiment, the cationic lipids disclosed are useful components in a lipid nanoparticle for the delivery of siRNA.
[0071] The cationic lipids of the present invention may have asymmetric centers, chiral axes, and chiral planes (as described in: E. L. Eliel and S. H. Wilen, Stereochemistry of Carbon Compounds, John Wiley & Sons, New York, 1994, pages 1119-1190), and occur as racemates, racemic mixtures, and as individual diastereomers, with all possible isomers and mixtures thereof, including optical isomers, being included in the present invention. In addition, the cationic lipids disclosed herein may exist as tautomers and both tautomeric forms are intended to be encompassed by the scope of the invention, even though only one tautomeric structure is depicted.
[0072] It is understood that substituents and substitution patterns on the cationic lipids of the instant invention can be selected by one of ordinary skill in the art to provide cationic lipids that are chemically stable and that can be readily synthesized by techniques known in the art, as well as those methods set forth below, from readily available starting materials. If a substituent is itself substituted with more than one group, it is understood that these multiple groups may be on the same carbon or on different carbons, so long as a stable structure results.
[0073] It is understood that one or more Si atoms can be incorporated into the cationic lipids of the instant invention by one of ordinary skill in the art to provide cationic lipids that are chemically stable and that can be readily synthesized by techniques known in the art from readily available starting materials.
[0074] In the compounds of Formula A, the atoms may exhibit their natural isotopic abundances, or one or more of the atoms may be artificially enriched in a particular isotope having the same atomic number, but an atomic mass or mass number different from the atomic mass or mass number predominantly found in nature. The present invention is meant to include all suitable isotopic variations of the compounds of Formula A. For example, different isotopic forms of hydrogen (H) include protium ( 1 H) and deuterium ( 2 H). Protium is the predominant hydrogen isotope found in nature. Enriching for deuterium may afford certain therapeutic advantages, such as increasing in vivo half-life or reducing dosage requirements, or may provide a compound useful as a standard for characterization of biological samples. Isotopically-enriched compounds within Formula A can be prepared without undue experimentation by conventional techniques well known to those skilled in the art or by processes analogous to those described in the Scheme and Examples herein using appropriate isotopically-enriched reagents and/or intermediates.
[0075] As used herein, “alkyl” means a straight chain, cyclic or branched saturated aliphatic hydrocarbon having the specified number of carbon atoms.
[0076] As used herein, “alkenyl” means a straight chain, cyclic or branched unsaturated aliphatic hydrocarbon having the specified number of carbon atoms including but not limited to diene, triene and tetraene unsaturated aliphatic hydrocarbons.
[0077] Examples of a cyclic “alkyl” or “alkenyl are:
[0000]
[0078] As used herein, “heterocyclyl” or “heterocycle” means a 4- to 10-membered aromatic or nonaromatic heterocycle containing from 1 to 4 heteroatoms selected from the group consisting of O, N and S, and includes bicyclic groups. “Heterocyclyl” therefore includes, the following: benzoimidazolyl, benzofuranyl, benzofurazanyl, benzopyrazolyl, benzotriazolyl, benzothiophenyl, benzoxazolyl, carbazolyl, carbolinyl, cinnolinyl, furanyl, imidazolyl, indolinyl, indolyl, indolazinyl, indazolyl, isobenzofuranyl, isoindolyl, isoquinolyl, isothiazolyl, isoxazolyl, naphthpyridinyl, oxadiazolyl, oxazolyl, oxazoline, isoxazoline, oxetanyl, pyranyl, pyrazinyl, pyrazolyl, pyridazinyl, pyridopyridinyl, pyridazinyl, pyridyl, pyrimidyl, pyrrolyl, quinazolinyl, quinolyl, quinoxalinyl, tetrahydropyranyl, tetrazolyl, tetrazolopyridyl, thiadiazolyl, thiazolyl, thienyl, triazolyl, azetidinyl, 1,4-dioxanyl, hexahydroazepinyl, piperazinyl, piperidinyl, pyrrolidinyl, morpholinyl, thiomorpholinyl, dihydrobenzoimidazolyl, dihydrobenzofuranyl, dihydrobenzothiophenyl, dihydrobenzoxazolyl, dihydrofuranyl, dihydroimidazolyl, dihydroindolyl, dihydroisooxazolyl, dihydroisothiazolyl, dihydrooxadiazolyl, dihydrooxazolyl, dihydropyrazinyl, dihydropyrazolyl, dihydropyridinyl, dihydropyrimidinyl, dihydropyrrolyl, dihydroquinolinyl, dihydrotetrazolyl, dihydrothiadiazolyl, dihydrothiazolyl, dihydrothienyl, dihydrotriazolyl, dihydroazetidinyl, methylenedioxybenzoyl, tetrahydrofuranyl, and tetrahydrothienyl, and N-oxides thereof all of which are optionally substituted with one to three substituents selected from R″.
[0079] As used herein, “polyamine” means compounds having two or more amino groups. Examples include putrescine, cadaverine, spermidine, and spermine.
[0080] As used herein, “halogen” means Br, Cl, F and I.
[0081] In an embodiment of Formula A, R 1 and R 2 are independently selected from H and (C 1 -C 6 )alkyl, wherein said alkyl is optionally substituted with one to three substituents selected from or R 1 and R 2 can be taken together with the nitrogen to which they are attached to form a monocyclic heterocycle with 4-7 members optionally containing, in addition to the nitrogen, one or two additional heteroatoms selected from N, O and S, said monocyclic heterocycle is optionally substituted with one to three substituents selected from R′.
[0082] In an embodiment of Formula A, R 1 and R 2 are independently selected from H, methyl, ethyl and propyl, wherein said methyl, ethyl and propyl are optionally substituted with one to three substituents selected from R′, or R 1 and R 2 can be taken together with the nitrogen to which they are attached to form a monocyclic heterocycle with 4-7 members optionally containing, in addition to the nitrogen, one or two additional heteroatoms selected from N, and S, said monocyclic heterocycle is optionally substituted with one to three substituents selected from R 1 .
[0083] In an embodiment of Formula A, R 1 and R 2 are independently selected from H, methyl, ethyl and propyl.
[0084] In an embodiment of Formula A, R 1 and R 2 are each methyl.
[0085] In an embodiment of Formula A, R 3 is selected from H and methyl.
[0086] In an embodiment of Formula A, R 3 is H.
[0087] In an embodiment of Formula A, R′ is R″.
[0088] In an embodiment of Formula A, R″ is independently selected from H, methyl, ethyl and propyl, wherein said methyl, ethyl and propyl are optionally substituted with one or more halogen and OH.
[0089] In an embodiment of Formula A, R″ is independently selected from H, methyl, ethyl and propyl.
[0090] In an embodiment of Formula A, n is 0, 1 or 2.
[0091] In an embodiment of Formula A, n is 0 or 1.
[0092] In an embodiment of Formula A, n is 0.
[0093] In an embodiment of Formula A, L 1 is selected from C 3 -C 24 alkyl and C 3 -C 24 alkenyl, which are optionally substituted with halogen and OH.
[0094] In an embodiment of Formula A, L 1 is selected from C 3 -C 24 alkyl and C 3 -C 24 alkenyl.
[0095] In an embodiment of Formula A, L 1 is selected from C 3 -C 24 alkenyl.
[0096] In an embodiment of Formula A, L 1 is selected from C 12 -C 24 alkenyl.
[0097] In an embodiment of Formula A, L 1 is C 18 alkenyl.
[0098] In an embodiment of Formula A, L 1 is:
[0000]
[0099] In an embodiment of Formula A, L 1 is C8 alkyl.
[0100] In an embodiment of Formula A, L 2 is selected from C 3 -C 24 alkyl and C 3 -C 24 alkenyl, which are optionally substituted with halogen and OH.
[0101] In an embodiment of Formula A, L 2 is selected from C 3 -C 24 alkyl and C 3 -C 24 alkenyl.
[0102] In an embodiment of Formula A, L 2 is selected from C 3 -C 24 alkenyl.
[0103] In an embodiment of Formula A, L 2 is selected from C 12 -C 24 alkenyl.
[0104] In an embodiment of Formula A, L 2 is C 19 alkenyl.
[0105] In an embodiment of Formula A, L 2 is:
[0000]
[0106] In an embodiment of Formula A, L 2 is selected from C 3 -C 9 alkyl and C 3 -C 9 alkenyl, which are optionally substituted with halogen and OH.
[0107] In an embodiment of Formula A, L 2 is selected from C 5 -C 9 alkyl and C 5 -C 9 alkenyl, which are optionally substituted with halogen and OH.
[0108] In an embodiment of Formula A, L 2 is selected from C 7 -C 9 alkyl and C 7 -C 9 alkenyl, which are optionally substituted with halogen and OH.
[0109] In an embodiment of Formula A, L 2 is selected from C 3 -C 9 alkyl and C 3 -C 9 alkenyl.
[0110] In an embodiment of Formula A, L 2 is selected from C 5 -C 9 alkyl and C 5 -C 9 alkenyl.
[0111] In an embodiment of Formula A, L 2 is selected from C 7 -C 9 alkyl and C 7 -C 9 alkenyl.
[0112] In an embodiment of Formula A, L 2 is C 3 -C 9 alkyl.
[0113] In an embodiment of Formula A, L 2 is C 5 -C 9 alkyl.
[0114] In an embodiment of Formula A, L 2 is C 7 -C 9 alkyl.
[0115] In an embodiment of Formula A, L 2 is C 9 alkyl.
[0116] In an embodiment of Formula A, “heterocyclyl” is pyrrolidine, piperidine, morpholine, imidazole or piperazine.
[0117] In an embodiment of Formula A, “monocyclic heterocyclyl” is pyrrolidine, piperidine, morpholine, imidazole or piperazine.
[0118] In an embodiment of Formula A, “polyamine” is putrescine, cadaverine, spermidine or spermine.
[0119] In an embodiment, “alkyl” is a straight chain saturated aliphatic hydrocarbon having the specified number of carbon atoms.
[0120] In an embodiment, “alkenyl” is a straight chain unsaturated aliphatic hydrocarbon having the specified number of carbon atoms.
[0121] Included in the instant invention is the free form of cationic lipids of Formula A, as well as the pharmaceutically acceptable salts and stereoisomers thereof. Some of the isolated specific cationic lipids exemplified herein are the protonated salts of amine cationic lipids. The term “free form” refers to the amine cationic lipids in non-salt form. The encompassed pharmaceutically acceptable salts not only include the isolated salts exemplified for the specific cationic lipids described herein, but also all the typical pharmaceutically acceptable salts of the free form of cationic lipids of Formula A. The free form of the specific salt cationic lipids described may be isolated using techniques known in the art. For example, the free form may be regenerated by treating the salt with a suitable dilute aqueous base solution such as dilute aqueous NaOH, potassium carbonate, ammonia and sodium bicarbonate. The free forms may differ from their respective salt forms somewhat in certain physical properties, such as solubility in polar solvents, but the acid and base salts are otherwise pharmaceutically equivalent to their respective free forms for purposes of the invention.
[0122] The pharmaceutically acceptable salts of the instant cationic lipids can be synthesized from the cationic lipids of this invention which contain a basic or acidic moiety by conventional chemical methods. Generally, the salts of the basic cationic lipids are prepared either by ion exchange chromatography or by reacting the free base with stoichiometric amounts or with an excess of the desired salt-forming inorganic or organic acid in a suitable solvent or various combinations of solvents. Similarly, the salts of the acidic compounds are formed by reactions with the appropriate inorganic or organic base.
[0123] Thus, pharmaceutically acceptable salts of the cationic lipids of this invention include the conventional non-toxic salts of the cationic lipids of this invention as formed by reacting a basic instant cationic lipids with an inorganic or organic acid. For example, conventional non-toxic salts include those derived from inorganic acids such as hydrochloric, hydrobromic, sulfuric, sulfamic, phosphoric, nitric and the like, as well as salts prepared from organic acids such as acetic, propionic, succinic, glycolic, stearic, lactic, malic, tartaric, citric, ascorbic, pamoic, maleic, hydroxymaleic, phenylacetic, glutamic, benzoic, salicylic, sulfanilic, 2-acetoxy-benzoic, fumaric, toluenesulfonic, methanesulfonic, ethane disulfonic, oxalic, isethionic, trifluoroacetic (TFA) and the like.
[0124] When the cationic lipids of the present invention are acidic, suitable “pharmaceutically acceptable salts” refers to salts prepared form pharmaceutically acceptable non-toxic bases including inorganic bases and organic bases. Salts derived from inorganic bases include aluminum, ammonium, calcium, copper, ferric, ferrous, lithium, magnesium, manganic salts, manganous, potassium, sodium, zinc and the like. Particularly preferred are the ammonium, calcium, magnesium, potassium and sodium salts. Salts derived from pharmaceutically acceptable organic non-toxic bases include salts of primary, secondary and tertiary amines, substituted amines including naturally occurring substituted amines, cyclic amines and basic ion exchange resins, such as arginine, betaine caffeine, choline, N,N 1 -dibenzylethylenediamine, diethylamin, 2-diethylaminoethanol, 2-dimethylaminoethanol, ethanolamine, ethylenediamine, N-ethylmorpholine, N-ethylpiperidine, glucamine, glucosamine, histidine, hydrabamine, isopropylamine, lysine, methylglucamine, morpholine, piperazine, piperidine, polyamine resins, procaine, purines, theobromine, triethylamine, trimethylamine tripropylamine, tromethamine and the like.
[0125] The preparation of the pharmaceutically acceptable salts described above and other typical pharmaceutically acceptable salts is more fully described by Berg et al., “Pharmaceutical Salts,” J. Pharm. Sci., 1977:66:1-19.
[0126] It will also be noted that the cationic lipids of the present invention are potentially internal salts or zwitterions, since under physiological conditions a deprotonated acidic moiety in the compound, such as a carboxyl group, may be anionic, and this electronic charge might then be balanced off internally against the cationic charge of a protonated or alkylated basic moiety, such as a quaternary nitrogen atom.
EXAMPLES
[0127] Examples provided are intended to assist in a further understanding of the invention. Particular materials employed, species and conditions are intended to be further illustrative of the invention and not limitative of the reasonable scope thereof. The reagents utilized in synthesizing the cationic lipids are either commercially available or are readily prepared by one of ordinary skill in the art.
[0128] Synthesis of the novel cationic lipids is a linear process starting from epichlorohydrin (i) (General Scheme 1). Epoxide opening, ring closure with lipid alkoxide delivers epoxy ether intermediate ii. Grignard addition to the epoxide provides secondary alcohol intermediate iii. Mitsinobu inversion with azide followed by reduction yields primary amine intermediates v. Reductive amination provides the tertiary amine derivatives vi.
[0000]
[0129] An alternative synthesis of the novel cationic lipids starting from epichlorohydrin (i) is depicted in General Scheme 2. Epoxide opening, ring closure with lipid Grignard delivers epoxide intermediate vii. Alkoxide addition to the epoxide provides secondary alcohol intermediate iii. Mitsinobu inversion with azide followed by reduction yields primary amine intermediates v. Reductive amination provides the tertiary amine derivatives vi.
[0000]
[0130] Synthesis of the homologated cationic lipids x (General Scheme 3) begins with oxidation of intermediate iii to ketone vii using Dess-Martin Periodinane. Conversion of the ketone to the nitrile viii is accomplished with TOSMIC. Reduction of the nitrile with lithium aluminum hydride gives primary amine ix. Reductive amination provides cationic lipids x.
[0000]
[0131] Synthesis of doubly homologated cationic lipids xiii begins with ketone vii. Peterson olefination generates the unsaturated amide xi. Conjugate reduction with L-Selectride gives amide xii. Amide reduction with lithium aluminum hydride gives cationic lipids xiii.
[0000]
(2S)—N,N-dimethyl-1-[(9Z,12Z)-oetadeca-9,12-dien-1-yloxy]undecan-2-amine (Compound 1)
[0132]
[0133] A 250 mL rb flask was charged with magnetic stirbar, tetrabutyl ammonium bromide (TBAB, 2.72 g, 8.4 mmol), linoleyl alcohol (225 g, 884 mmol), and sodium hydroxide (50.7 g, 1.2 mol), then cooled in an ice bath. The (S)-epichlorohydrin (156 g, 1.69 mol) was added slowly over 2 hours and then warmed to ambient temperature and stirred overnight. 259 mL of hexane was added and allowed to stir for 15 mins, then mixture was filtered and organic layer was concentrated in vacuo. The product was purified using 0-10% ethyl acetate/hexane gradient on 330 g silica column to give (2R)-2-{[(9Z,12Z)-octadeca-9,12-dien-1-yloxy]methyl}oxirane. 1 H NMR (CDCl 3 , 300 mHz) δ 0.90-0.86 (m, 3H), 1.29 (s, 16H), 1.55-1.64 (m, 2H), 2.00-2.07 (m, 4H), 2.58-2.61 (m, 1H), 2.74-2.80 (m, 3H), 3.12-3.15 (m, 1H) 3.34-3.52 (m, 3H), 3.67-3.72 (dd, J=12 Hz, 1H) 5.30-5.35 (m, 4H); HRMS (m+1) calcd 323.2872. found 323.2951.
[0000]
[0134] The epoxide (15 g, 46.5 mmol) was dissolved in THF and cooled to 0° C. under stream of Nitrogen. Octyl Grignard (25.6 mL 2M solution, 51.2 mmol) was added dropwise and then heate in microwave at 120° C. for one hour. The precipitate was filtered off and the solvent evaporated in vacuo. The crude oil was directly loaded onto a silica gel column and eluted with 0-10% gradient (hexane-ethyl acetate) to give (2R)-1-[(9Z,12Z)-octadeca-9,12-dien-1-yloxy]undecan-2-ol. LC/MS (m+1)=437.6.
[0000]
[0135] Triphenyl phosphine (14.4 g, 55 mmol) was dissolved in THF and cooled to 0° C. under nitrogen. Di-tertbutyl azodicarboxylate (13.7 g, 59.5 mmol) was added slowly and the reaction was stirred for 30 mins. Then the alcohol (20 g, 45.8 mmol) was added dropwise and allowed to stir for 10 mins, then diphenyl phosphorylazide (15.1 g, 55 mmol) was added and allowed to stir overnight, warming to ambient temperature. The reaction was evaporated to dryness in vacuo and directly loaded onto a silica gel column and eluted with 0-10% ethyl acetate/hexane gradient to provide (2S)-2-azidoundecyl (9Z,12Z)-octadeca-9,12-dien-1-yl ether which was carried directly into the next reaction without characterization.
[0000]
[0136] Triphenyl phosphine (4.54 g, 17.3 mmol) and the azide (8 g, 17.3 mmol) were dissolved in THF. The reaction mixture was split into 3 μw tubes and irradiated at 120° C. for 1 hour each. Considerable pressure built in each tube so care should be noted. LC indicated 100% conversion to phosphoimine intermediate. To each tube was added ˜3 mL of water and the reaction irradiated for 10 min at 120° C. The reaction mixtures were combined and concentrated to remove organic solvent. Hexane was added to precipitate phosphine oxides which were filtered through cintered glass funnel. The solvent was then removed in vacuo. The crude product was purified using HPLC with 30 min run and 60-100% water/acetonitrile gradient. The combined HPLC fractions were neutralized with sodium bicarbonate evaoporated in vacuo. The pure product was partitioned between water/hexanes. The organic layer was dried over sodium sulfate, filtered and evaporated in vacuo to afford (2S)-1-[(9Z,12Z)-octadeca-9,12-dien-1-yloxy]undecan-2-amine (2). 1 H NMR (CDCl 3 , 300 mHz) δ 0.88-0.87 (m, 6H), 1.25-1.29 (s, 32H), 1.54-1.54 (m, 2H), 2.03-2.05 (m, 4H), 2.23 (s, 2H), 2.75-2.76 (m, 2H), 2.96 (m, 1H), 3.13-3.18 (m, 1H), 3.38-3.45 (m, 3H), 5.31-5.38 (m, 4H); LC/MS (m+1) 436.7.
[0000]
[0137] The primary amine (3.5 g, 8 mmol) was dissolved in THF and formaldehyde (3.26 g, 40.2 mmol) was added, followed by triacetoxy borohydride (5.1 g, 24.1 mmol). The reaction was stirred at ambient temperature for 15 mins. LC/MS indicated 100% conversion to product. Added 1M NaOH until basic and extracted with hexane and washed with water. Retained organic layer and removed solvent in vacuo. Purified using 60-100% water/acetonitrile 30 min gradient on C8 HPLC. Combined fractions and added sodium bicarbonate and evaporated organics in vacuo. The product was partitioned between water/hexanes and the organics were dried over sodium sulfate, filtered and evaporated in vacuo to deliver (2S)—N,N-dimethyl-1-[(9Z,12Z)-octadeca-9,12-dien-1-yloxy]undecan-2-amine (1). 1 H NMR (CDCl 3 , 300 mHz) δ 0.88-0.87 (m, 6H), 1.285 (s, 33H), 1.55 (m, 2H), 1.80 (m, 1H), 2.00-2.05 (s, 4H), 2.29-2.31 (2H), 2.50 (m, 1H), 2.76-1.77 (m, 2H), 3.36-3.51 (m, 6H), 5.34-5.36 (m, 4H); LC/MS (m+1) 464.9.
[0138] Compounds 3-11 are novel cationic lipids and were prepared according to General Scheme 1 above.
[0000]
Com-
LC/MS
pound
Structure
(m + 1)
3
450.4
4
450.6
5
423.6
6
408.6
7
492.8
8
436.6
9
479.7
10
478.7
11
451.7
(2S)—N,N-dimethyl-1-[(9Z,12Z)-octadeca-9,12-dien-1-yloxy]undecan-2-amine (Compound 12)
[0139]
[0140] A round bottomed flask was charged with magnetic stir bar, copper cyanide (1.45 g, 16.2 mmol), epichlorohydrin (15 g, 162 mmol) and purged with nitrogen. THF was added, the solution cooled to −78° C. and linoleyl Grignard (68.8 g, 195 mmol) was added slowly. After addition of Grignard the reaction was allowed to warm to ambient temperature. The reaction was quenched with saturated ammonium chloride solution and extracted with ether. The organics were dried over sodium sulfate, filtered and evaporated in vacuo. The intermediate chloro-alcohol was purified via flash chromatography (silica, 0-35% ethyl acetate/hexanes). The alcohol was dissolved in THF and allowed to stir with solid NaOH pellets at ambient temperature for 16 hours, then filtered off NaOH and washed organic layer with water. The organics were dried over sodium sulfate, filtered and evaporated in vacuo to provide (2S)-2-[(10Z,13Z)-nonadeca-10,13-dien-1-yl]oxirane. 1 H NMR (CDCl 3 , 300 mHz) δ 0.87-0.90 (m, 3H), 1.27-1.52 (m, 22H), 2.01-2.19 (m, 4H), 2.40-2.46 (m, 1H), 2.71-2.76 (m, 3H), 2.89-2.91 (m, 1H), 5.30-5.36 (m, 4H); LC/MS (m+H+acetonitrile) 349.5.
[0000]
[0141] The alcohol (2.55 g, 19.6 mmol) was dissolved in DCM and cooled to 0° C. To this solution was added tin chloride (1.63 mmol, 1.63 mL of a 1M solution). The epoxide (5 g, 16.3 mmol) was added to the reaction mixture dropwise and the reaction was aged for 1 hour at 0° C. The reaction was evaporated in vacuo, dissolved in hexanes and purified by flash chromatography (0-20% ethyl acetate/hexanes) to give (2R,12Z,15Z)-1-(octyloxy)henicosa-12,15-dien-2-ol. LC/MS (m+H)=437.6.
[0000]
[0142] The alcohol was carried on to final Compound 12 as described for Compound 1. 1 H NMR (CDCl 3 , 300 mHz) δ 0.85-0.091 (m, 6H), 1.272 (s, 34H), 1.46 (m, 1H), 1.57 (m, 1H), 1.65 (s, 4H), 2.01-2.08 (3H), 2.30 (m, 6H), 2.52 (m, 1H), 2.75 2.79 (m, 2H), 3.29-3.4 (m, 2H), 3.46-3.51 (dd, 9.76 Hz, 1H), 5.30-5.39 (m, 4H); LC/MS (m+H)=464.7.
[0143] Compounds 13-16 are novel cationic lipids and were prepared according to General Scheme 2 above.
[0000]
Com-
LC/MS
pound
Structure
(m + 1)
13
492.7
14
436.7
15
577.0
16
506.8
N,N-dimethyl-2-{[(9Z,12Z)-octadeca-9,12-dien-1-yloxy]methyl}undecan-1-amine (Compound 17)
[0144]
[0145] To a solution of alcohol iii (15 g, 34.3 mmol) in dichloromethane (50 mL) was added Doss-Martin Periodinane (14.6 g, 34.3 mmol) and the reaction was stirred at ambient temperature for 16 hours. The solids were filtered and the filtrate partitioned between water/DCM. The organics were dried over sodium sulfate, filtered and evaporated in vacuo. Purification by flash chromatography (silica, 0-15% ethyl acetate/hexanes) gave ketone vii. LC/MS (M+H)=435.6.
[0000]
[0146] To a solution of ketone vii (10 g, 23.0 mmol) in DME (40 mL) was added TOSMIC (5.8 g, 29.9 mmol) and the solution was cooled to 0° C. To the cooled solution was added potassium tert-butoxide (46 mmol, 46 mL of a 1M solution in tBuOH) dropwise. After 30 minutes the reaction was partitioned between hexanes and water. The organics were dried over sodium sulfate, filtered and evaporated in vacuo. Purification by flash chromatography (silica, 0-10% ethyl acetate/hexanes) gave nitrile viii. LC/MS (M+H)=446.6.
[0000]
[0147] To a solution of nitrile viii (4.6 g, 10.4 mmol) in THF (25 mL) was added lithium aluminum hydride (0.8 g, 20.7 mmol) at ambient temperature. The reaction was quenched with sodium sulfate decahydrate solution and the solids were filtered. The filtrate was dried over sodium sulfate, filtered and evaporated in vacuo to give crude amine ix which was carried directly into next reaction. LC/MS (M+H)=450.6.
[0000]
[0148] A solution of amine ix (4.7 g, 10.3 mmol) and formaldehyde (2.5 g, 31.1 mmol) in THF (25 mL) was treated with sodium triacetoxyborohydride (6.6 g, 31.1 mmol) at ambient temperature. After aging for 15 minutes, the reaction was quenched with 1M sodium hydroxide and partitioned between water and hexanes. The organics were dried over sodium sulfate, filtered and evaporated in vacuo. Purification by preparative reverse phase chromatography (C8 column, acetonitrile/water gradient) gave compound 17. LC/MS (M+H)=479.6. 1 H NMR (CDCl 3 , 400 mHz) δ 5.36 (m, 4H), 3.38 (m, 3H), 3.26 (m, 1H), 2.75 (t, J=6.4 Hz, 2H), 2.22 (m, 1H), 2.19 (s, 6H), 2.04 (m, 5H), 1.71 (m, 1H), 1.54 (m, 2H), 1.28 (m, 32H), 0.83 (m, 6H).
N,N-dimethyl-3-{[(9Z,12Z)-octadeca-9,12-dien-1-yloxy]methyl}dodecan-1-amine (Compound 18)
[0149]
[0150] A solution of silyl amide (12.4 g, 78 mmol) in THF (50 mL) was cooled to −78° C. and treated with nBuLi (62.4 mmol, 25 mL of a 2.5M solution) and aged for 10 minutes. To this solution was transferred ketone vii (12 g, 27.6 mmol) in a small portion of dry THF. The reaction was aged 15 minutes then warmed to ambient temperature, quenched with sodium bicarbonate solution and partitioned between water and hexanes. The organics were dried over sodium sulfate, filtered and evaporated in vacuo to give amide xi. LC/MS (M+H)=505.6.
[0000]
[0151] Amide xi (7 g, 13.9 mmol) was treated with L-Selectride (55.6 mmol, 55.6 mL of a 1M solution) in a microwave vial. The reaction was sealed and irradiated in a microwave reaction set at 70° C. for 16 hours. The reaction was then diluted with dichloromethane and quenched by careful addition of sodium perborate solid until effervescence stopped. The solids were filtered and the filtrate evaporated in vacuo to give xii. LC/MS (M+FI)=507.6.
[0000]
[0152] To a solution of amide xii (7 g, 13.8 mmol) in THF (30 mL) was added lithium aluminum hydride (1.1 g, 27.7 mmol). The reaction was quenched with sodium sulfate decahydrate solution and the solids filtered. The organics were evaporated in vacuo and the product purified by preparative reverse phase chromatography (C8 column, acetonitrile/water gradient) to give compound 18. LC/MS (M+H)=493.6. 1 H NMR (CDCl 3 , 400 mHz) δ 5.38 (m, 4H), 3.38 (m, 2H), 3.26 (m, 2H), 2.78 (t, J=6.4 Hz, 2H), 2.25 (m, 8H), 2.04 (m, 4H), 1.56 (m, 4H), 1.29 (m, 32H), 0.89 (m, 6H).
(2S)—N,N-dimethyl-1-[(8-{2-[(2-pentylcyclopropyl)methyl]cyclopropyl}octyl)oxy]tridecan-2-amine (Compound 19)
[0153]
[0154] A solution of diene (24 g, 51.6 mmol) in dichloromethane (100 mL) was cooled to −15° C. To this solution was added diethyl zinc (310 mmol, 310 mL of a 1M solution) followed by diiodomethane (25 mL, 310 mmol) and the reaction was aged for 16 hours while slowly warming to ambient temperature. The reaction was quenched with ammonium chloride solution and partitioned between water and dichloromethane. The organics were dried over sodium sulfate, filtered and evaporated in vacuo. Purification by flash chromatography (silica, 0-25% ethyl acetate/hexanes) gave bis-cyclopropane intermediate xiv. LC/MS (M+H) 493.6.
[0000]
[0155] Compound xiv was carried on to final compound 19 as outlined for compound 1 above. LC/MS (M+H)=520.8.
[0156] Compound 20 is DLinKC2DMA as described in Nature Biotechnology, 2010, 28, 172-176, WO 2010/042877 A1, WO 2010/048536 A2, WO 2010/088537 A2, and WO 2009/127060 A1.
[0000]
[0157] Compound 21 is MC3 as described in WO 2010/054401, and WO 2010/144740A1.
[0000]
LNP Compositions
[0158] The following lipid nanoparticle compositions (LNPs) of the instant invention are useful for the delivery of oligonucleotides, specifically siRNA and miRNA:
Cationic Lipid/Cholesterol/PEG-DMG 56.6/38/5.4;
Cationic Lipid/Cholesterol/PEG-DMG 60/38/2;
Cationic Lipid/Cholesterol/PEG-DMG 67.3/29/3.7;
Cationic Lipid/Cholesterol/PEG-DMG 49.3/47/3.7;
Cationic Lipid/Cholesterol/PEG-DMG 50.3/44.3/5.4;
Cationic Lipid/Cholesterol/PEG-C-DMA/DSPC 40/48/2/10;
Cationic Lipid/Cholesterol/PEG-DMG/DSPC 40/48/2/10; and
Cationic Lipid/Cholesterol/PEG-DMG/DSPC 58/30/2/10.
LNP Process Description:
[0159] The Lipid Nano-Particles (LNP) are prepared by an impinging jet process. The particles are formed by mixing lipids dissolved in alcohol with siRNA dissolved in a citrate buffer. The mixing ratio of lipids to siRNA are targeted at 45-55% lipid and 65-45% siRNA. The lipid solution contains a novel cationic lipid of the instant invention, a helper lipid (cholesterol), PEG (e.g. PEG-C-DMA, PEG-DMG) lipid, and DSPC at a concentration of 5-15 mg/mL with a target of 9-12 mg/mL in an alcohol (for example ethanol). The ratio of the lipids has a mole percent range of 25-98 for the cationic lipid with a target of 35-65, the helper lipid has a mole percent range from 0-75 with a target of 30-50, the PEG lipid has a mole percent range from 1-15 with a target of 1-6, and the DSPC has a mole precent range of 0-15 with a target of 0-12. The siRNA solution contains one or more siRNA sequences at a concentration range from 0.3 to 1.0 mg/mL with a target of 0.3-0.9 mg/mL in a sodium citrate buffered salt solution with pH in the range of 3.5-5. The two liquids are heated to a temperature in the range of 15-40° C., targeting 30-40° C., and then mixed in an impinging jet mixer instantly forming the LNP. The teeID has a range from 0.25 to 1.0 mm and a total flow rate from 10-600 mL/min. The combination of flow rate and tubing ID has effect of controlling the particle size of the LNPs between 30 and 200 nm. The solution is then mixed with a buffered solution at a higher pH with a mixing ratio in the range of 1:1 to 1:3 vol:vol but targeting 1:2 vol:vol. This buffered solution is at a temperature in the range of 15-40° C., targeting 30-40° C. The mixed LNPs are held from 30 minutes to 2 hrs prior to an anion exchange filtration step. The temperature during incubating is in the range of 15-40° C., targeting 30-40° C. After incubating the solution is filtered through a 0.8 um filter containing an anion exchange separation step. This process uses tubing IDs ranging from 1 mm ID to 5 mm ID and a flow rate from 10 to 2000 mL/min. The LNPs are concentrated and diafiltered via an ultrafiltration process where the alcohol is removed and the citrate buffer is exchanged for the final buffer solution such as phosphate buffered saline. The ultrafiltration process uses a tangential flow filtration format (TEE). This process uses a membrane nominal molecular weight cutoff range from 30-500 KD. The membrane format can be hollow fiber or flat sheet cassette. The TFF processes with the proper molecular weight cutoff retains the LNP in the retentate and the filtrate or permeate contains the alcohol; citrate buffer; final buffer wastes. The TFF process is a multiple step process with an initial concentration to a siRNA concentration of 1-3 mg/mL. Following concentration, the LNPs solution is diafiltered against the final buffer for 10-20 volumes to remove the alcohol and perform buffer exchange. The material is then concentrated an additional 1-3 fold. The final steps of the LNP process are to sterile filter the concentrated LNP solution and vial the product.
Analytical Procedure:
[0160] 1) siRNA Concentration
[0161] The siRNA duplex concentrations are determined by Strong Anion-Exchange High-Performance Liquid Chromatography (SAX-HPLC) using Waters 2695 Alliance system (Water Corporation, Milford Mass.) with a 2996 PDA detector. The LNPs, otherwise referred to as RNAi Delivery Vehicles (RDVs), are treated with 0.5% Triton X-100 to free total siRNA and analyzed by SAX separation using a Dionex BioLC DNAPac PA 200 (4×250 mm) column with UV detection at 254 nm. Mobile phase is composed of A: 25 mM NaClO 4 , 10 mM Tris, 20% EtOH, pH 7.0 and 13: 250 mM NaClO 4 , 10 mM Tris, 20% EtOH, pH 7.0 with liner gradient from 0-15 min and flow rate of 1 ml/min. The siRNA amount is determined by comparing to the siRNA standard curve.
2) Encapsulation Rate
[0162] Fluorescence reagent SYBR Gold is employed for RNA quantitation to monitor the encapsulation rate of RDVs. RDVs with or without Triton X-100 are used to determine the free siRNA and total siRNA amount. The assay is performed using a SpectraMax M5e microplate spectrophotometer from Molecular Devices (Sunnyvale, Calif.). Samples are excited at 485 nm and fluorescence emission was measured at 530 nm. The siRNA amount is determined by comparing to the siRNA standard curve.
[0163] Encapsulation rate=(1-free siRNA/total siRNA)×100%
3) Particle Size and Polydispersity
[0164] RDVs containing 1 μg siRNA are diluted to a final volume of 3 ml with 1×PBS. The particle size and polydispersity of the samples is measured by a dynamic light scattering method using ZetaPALS instrument (Brookhaven Instruments Corporation, Holtsville, N.Y.). The scattered intensity is measured with He—Ne laser at 25° C. with a scattering angle of 90°.
4) Zeta Potential Analysis
[0165] RDVs containing 1 μg siRNA are diluted to a final volume of 2 ml with 1 mM Tris buffer (pH 7.4). Electrophoretic mobility of samples is determined using ZetaPALS instrument (Brookhaven Instruments Corporation, Holtsville, N.Y.) with electrode and He—Ne laser as a light source. The Smoluchowski limit is assumed in the calculation of zeta potentials.
5) Lipid Analysis
[0166] Individual lipid concentrations are determined by Reverse Phase High-Performance Liquid Chromatography (RP-HPLC) using Waters 2695 Alliance system (Water Corporation, Milford Mass.) with a Corona charged aerosol detector (CAD) (ESA Biosciences, Inc, Chelmsford, Mass.). Individual lipids in RDVs are analyzed using an Agilent Zorbax SB-C18 (50×4.6 mm, 1.8 μm particle size) column with CAD at 60° C. The mobile phase is composed of A: 0.1% TFA in H 2 O and B: 0.1% TFA in IPA. The gradient changes from 60% mobile phase A and 40% mobile phase B from time 0 to 40% mobile phase A and 60% mobile phase B at 1.00 min; 40% mobile phase A and 60% mobile phase B from 1.00 to 5.00 min; 40% mobile phase A and 60% mobile phase 13 from 5.00 min to 25% mobile phase A and 75% mobile phase B at 10.00 min; 25% mobile phase A and 75% mobile phase 13 from 10.00 min to 5% mobile phase A and 95% mobile phase B at 15.00 min; and 5% mobile phase A and 95% mobile phase 13 from 15.00 to 60% mobile phase A and 40% mobile phase B at 20.00 min with flow rate of 1 ml/min. The individual lipid concentration is determined by comparing to the standard curve with all the lipid components in the RDVs with a quadratic curve fit. The molar percentage of each lipid is calculated based on its molecular weight.
[0167] Utilizing the above described LNP process, specific LNPs with the following ratios were identified:
Nominal Composition:
Cationic Lipid/Cholesterol/PEG-DMG 60/38/2
Cationic Lipid/Cholesterol/PEG-DMG/DSPC 58/30/2/10
[0168] Luc siRNA
[0000]
(SEQ. ID. NO.: 1)
5′-iB- A U AAGG CU A U GAAGAGA U ATT -iB 3′
(SEQ. ID. NO.: 2)
3′-UU U A UUCC GA U A CUUCUC UAU -5′
AUGC - Ribose
iB - Inverted deoxy abasic
UC - 2′ Fluoro
AGT - 2′ Deoxy
AGU - 2′ OCH 3
Nominal Composition
Cationic Lipid/Cholesterol/PEG-DMG 60/38/2
Cationic Lipid/Cholesterol/PEG-DMG/DSPC 40/48/2/10
Cationic Lipid/Cholesterol/PEG-DMG/DSPC 58/30/2/10
[0169] ApoB siRNA
[0000]
(SEQ ID NO.: 3)
5′-iB-CUUU AA C AA UUCCU GAAA U TsT -iB-3′
(SEQ ID NO.: 4)
3′-UsU GAAA U UG UU AAGGA CUs UsUsA -5′
AUGC - Ribose
iB - Inverted deoxy abasic
UC - 2′ Fluoro
AGT - 2′ Deoxy
AGU - 2′ OCH 3
UsA - phophorothioate linkage
Example 1
[0170] Mouse In Vivo Evaluation of Efficacy
[0171] LNPs utilizing Compounds 1-12, in the nominal compositions described immediately above, were evaluated for in vivo efficacy. The siRNA targets the mRNA transcript for the firefly ( Photinus pyralis ) luciferase gene (Accession # M15077). The primary sequence and chemical modification pattern of the luciferase siRNA is displayed above. The in vivo luciferase model employs a transgenic mouse in which the firefly luciferase coding sequence is present in all cells. ROSA26-LoxP-Stop-LoxP-Luc (LSL-Luc) transgenic mice licensed from the Dana Farber Cancer Institute are induced to express the Luciferase gene by first removing the LSL sequence with a recombinant Ad-Cre virus (Vector Biolabs). Due to the organo-tropic nature of the virus, expression is limited to the liver when delivered via tail vein injection. Luciferase expression levels in liver are quantitated by measuring light output, using an IVIS imager (Xenogen) following administration of the luciferin substrate (Caliper Life Sciences). Pre-dose luminescence levels are measured prior to administration of the RDVs. Luciferin in PBS (15 mg/mL) is intraperitoneally (IP) injected in a volume of 150 μL. After a four minute incubation period mice are anesthetized with isoflurane and placed in the IVIS imager. The RDVs (containing siRNA) in PBS vehicle were tail vein injected n a volume of 0.2 mL. Final dose levels ranged from 0.1 to 0.5 mg/kg siRNA. PBS vehicle alone was dosed as a control. Mice were imaged 48 hours post dose using the method described above. Changes in luciferin light output directly correlate with luciferase mRNA levels and represent an indirect measure of luciferase siRNA activity. In vivo efficacy results are expressed as % inhibition of luminescence relative to pre-dose luminescence levels. Systemic administration of the luciferase siRNA RDVs decreased luciferase expression in a dose dependant manner. Greater efficacy was observed in mice dosed with Compound 1 containing RDVs than with the RDV containing the octyl-CLinDMA (OCD) cationic lipid ( FIG. 1 ). OCD is known and described in WO2010/021865.
Example 2
Rat In Vivo Evaluation of Efficacy and Toxicity
[0172] LNPs utilizing compounds in the nominal compositions described above, were evaluated for in vivo efficacy and increases in alanine amino transferase and aspartate amino transferase in Sprague-Dawley (Crl:CD(SD) female rats (Charles River Labs). The siRNA targets the mRNA transcript for the ApoB gene (Accession # NM 019287). The primary sequence and chemical modification pattern of the ApoB siRNA is displayed above. The RDVs (containing siRNA) in PBS vehicle were tail vein injected in a volume of 1 to 1.5 mL. Infusion rate is approximately 3 ml/min. Five rats were used in each dosing group. After LNP administration, rats are placed in cages with normal diet and water present. Six hours post dose, food is removed from the cages. Animal necropsy is performed 24 hours after LNP dosing. Rats are anesthetized under isoflurane for 5 minutes, then maintained under anesthesia by placing them in nose cones continuing the delivery of isoflurane until exsanguination is completed. Blood is collected from the vena cava using a 23 gauge butterfly venipuncture set and aliquoted to serum separator vacutainers for serum chemistry analysis. Punches of the excised caudate liver lobe are taken and placed in RNALater (Ambion) for mRNA analysis. Preserved liver tissue was homogenized and total RNA isolated using a Qiagen bead mill and the Qiagen miRNA-Easy RNA isolation kit following the manufacturer's instructions. Liver ApoB mRNA levels were determined by quantitative RT-PCR. Message was amplified from purified RNA utilizing a rat ApoB commercial probe set (Applied Biosystems Cat # RN01499054_m1). The PCR reaction was performed on an ABI 7500 instrument with a 96-well Fast Block. The ApoB mRNA level is normalized to the housekeeping PPIB (NM 011149) mRNA. PPIB mRNA levels were determined by RT-PCR using a commercial probe set (Applied Biosytems Cat. No. Mm00478295_m1). Results are expressed as a ratio of ApoB mRNA/PPM mRNA. All mRNA data is expressed relative to the PBS control dose. Serum ALT and AST analysis were performed on the Siemens Advia 1800 Clinical Chemistry Analyzer utilizing the Siemens alanine aminotransferase (Cat#03039631) and aspartate aminotransferase (Cat#03039631) reagents. Similar efficacy was observed in rats dosed with Compound 1 containing RDV than with the RDV containing the cationic lipid DLinKC2DMA (Compound 20) or MC3 (Compound 21, FIG. 2 ). Additionally, 3 out of 4 rats treated with 3 mg/kg DLinKC2DMA (Compound 20) failed to survive 48 hours and 2 out of 4 rats treated with 3 mg/kg MC3 (Compound 21) failed to survive 48 hours. 1 out of 4 rats treated with 10 mg/kg Compound 1 survived at 48 hours post dose.
Example 3
Determination of Cationic Lipid Levels in Rat Liver
[0173] Liver Tissue was Weighed into 20-ml Vials and Homogenized in 9 v/w of Water using a GenoGrinder 2000 (OPS Diagnostics, 1600 strokes/min, 5 min). A 50 μL aliquot of each tissue homogenate was mixed with 300 μL of extraction/protein precipitating solvent (50/50 acetonitrile/methanol containing 500 nM internal standard) and the plate was centrifuged to sediment precipitated protein. A volume of 200 μL of each supernatant was then transferred to separate wells of a 96-well plate and 10 μl samples were directly analyzed by LC/MS-MS.
[0174] Standards were prepared by spiking known amounts of a methanol stock solution of ompound into untreated rat liver homogenate (9 vol water/weight liver). Aliquots (50 μL) each standard/liver homogenate was mixed with 300 μL of extraction/protein precipitating solvent (50/50 acetonitrile/methanol containing 500 nM internal standard) and the plate was centrifuged to sediment precipitated protein. A volume of 200 μL of each supernatant was transferred to separate wells of a 96-well plate and 10 μl of each standard was directly analyzed by LC/MS-MS.
[0175] Absolute quantification versus standards prepared and extracted from liver homogenate was performed using an Aria LX-2HPLC system (Thermo Scientific) coupled to an API 4000 triple quadrupole mass spectrometer (Applied Biosystems). For each run, a total of 10 μL sample was injected onto a BDS Hypersil CS HPLC column (Thermo, 50×2 mm, 3 μm) at ambient temperature.
[0176] Mobile Phase A: 95% H 2 O/5% methanol/10 mM ammonium formate/0.1% formic acid Mobile Phase B: 40% methanol/60% n-propanol/10 mM ammonium formate/0.1% formic acid The flow rate was 0.5 mL/min and gradient elution profile was as follows: hold at 80% A for 0.25 min, linear ramp to 100% B over 1.6 min, hold at 100% B for 2.5 min, then return and hold at 80% A for 1.75 min. Total run time was 5.8 min. API 4000 source parameters were CAD: 4, CUR: 15, GS1: 65, GS2: 35, IS: 4000, TEM: 550, CXP: 15, DP: 60, EP: 10. In rats dosed with Compound 1 containing RDV liver levels were lower than with the RDV containing the cationic lipid DLinKC2DMA (Compound 20) or MC3 (Compound 21, FIG. 3 ). | The instant invention provides for novel cationic lipids that can be used in combination with other lipid components such as cholesterol and PEG-lipids to form lipid nanoparticles with oligonucleotides. It is an object of the instant invention to provide a cationic lipid scaffold that demonstrates enhanced efficacy along with lower liver toxicity as a result of lower lipid levels in the liver. The present invention employs low molecular weight cationic lipids with one short lipid chain to enhance the efficiency and tolerability of in vivo delivery of siRNA. | 2 |
RELATED APPLICATIONS
[0001] This application is a continuation of U.S. application Ser. No. 14/608,478 filed Jan. 29, 2015, titled “SYSTEM AND METHOD OF MONITORING AND CONFIRMING MEDICATION DOSAGE”, which claims the benefit of and the priority from U.S. Provisional Application No. 61/934,275 filed Jan. 31, 2014, titled “SYSTEM AND METHOD OF MONITORING AND CONFIRMING MEDICATION DOSAGE”.
BACKGROUND OF THE INVENTION
[0002] As the population ages, more and more people will find themselves requiring complicated therapies such as biotechnology self-injectable medications to manage/cure their disease or improve their quality of life. Many of the medications will require a user to become familiar with the clinical nature of the medications, how they interact with other medications they may be taking, how to store the medications and importantly how to inject themselves with a syringe to deliver the medication. The volume of information required to be learned is daunting. Injecting one's self with a needle may be an intimidating task that raises many questions on the proper method of injecting the syringe. A need exists for a method of facilitating patient knowledge associated with these complex therapies. A need exists also for facilitating and ease of use with unique and specialized healthcare services like confirming that the proper dosage of medication is injected into a user in the most effective area of the body.
SUMMARY OF THE INVENTION
[0003] One embodiment of the present invention includes a medication monitoring system including a patient information unit having a processor, a memory and a patient monitoring unit and a program executing in the memory executing the steps of communicatively coupling a first device with a second device, transmitting live images from the first device to the second device, analyzing the content of the live images to identify at least one biometric attribute of a user in the image and at least one bar code on a container in the image, determining whether the bar code is associated with at least one biometric attribute, and notifying the user whether to consume the contents of the container based on the association of the bar code with the biometric attribute.
[0004] Another embodiment includes the step of analyzing the content of the live image includes determining the contents of the container based on the bar code.
[0005] In another embodiment, a video is steamed from the first communication device to the second communication device if the contents of the container are associated with the user.
[0006] In another embodiment, the video includes instructions on how to properly administer the contents of the container.
[0007] In another embodiment, the contents of the container are a medication prescribed to the user.
[0008] In another embodiment, the medication is a liquid medication.
[0009] In another embodiment, the step of analyzing the contents of the live image includes the step of determining the level of the liquid medication in the container.
[0010] In another embodiment, the level of the liquid in the container is determined by identifying a line representing the top surface of the liquid in the container.
[0011] In another embodiment, the medication is a pill.
[0012] Another embodiment includes the step of analyzing the live image includes determining whether the proper amount of medication is withdrawn from the container by comparing levels before and after the medication is withdrawn.
[0013] Another embodiment of the present invention includes a medication monitoring system including a patient information unit having a processor, a memory and a patient monitoring unit and a program executing in the memory executing the steps of communicatively coupling a first device with a second device, transmitting live images from the first device to the second device, analyzing the content of the live images to identify at least one biometric attribute of a user in the image and at least one bar code on a container in the image, determining whether the bar code is associated with at least one biometric attribute, and notifying the user whether to consume the contents of the container based on the association of the bar code with the biometric attribute, providing information to the user on the proper method of preparing the contents of the vial for consumption, analyzing the content of the live images after notifying the user to determine whether the user has prepared the contents of the container for consumption, notifying the user of the user's compliance with the previously provided information.
[0014] In another embodiment, the information provided to the user includes a video depicting the preparation of the contents in the container for consumption.
[0015] Another embodiment includes the steps of providing instructions to the user relating to the proper administration of the contents of the container.
[0016] Another embodiment includes the step of analyzing the content of the live images to determine if the user is properly administering the contents of the container.
[0017] Another embodiment includes the step of notifying the user if the user is not properly administering the contents of the container.
[0018] In another embodiment, the notification includes providing information relating to correction actions the user can take to properly administer the contents of the container.
[0019] In another embodiment, the contents of the container are a liquid medication.
[0020] In another embodiment, the contents of the container are administered using a syringe.
[0021] In another embodiment, the medication must be administered to a specific location of the body.
[0022] In another embodiment, the step of analyzing the content of the live images to determine if the user is properly administering the contents of the container includes determining if the user is administering the liquid to the correct location of the body.
BRIEF DESCRIPTION OF THE DRAWINGS
[0023] FIG. 1 depicts a block diagram of a medication monitoring system suitable for use with the methods and systems consistent with the present invention;
[0024] FIG. 2A shows a more detailed depiction of the client device of FIG. 1 ;
[0025] FIG. 2B shows a more detailed depiction of the patient information unit of FIG. 1 ;
[0026] FIG. 3A depicts a process of remotely instructing a user in the use of a pharmaceutical;
[0027] FIG. 3B depicts an embodiment of a technician interface used during a video conference;
[0028] FIG. 3C depicts an embodiment of the technician interface used while a portion of the video stream is recorded;
[0029] FIG. 3D depicts an embodiment of an interface used by a patient;
[0030] FIG. 4 depicts a schematic representation of a process executed by the image analysis unit operating on the client device; and
[0031] FIG. 5 depicts a schematic representation of a process executed by the image analysis unit.
DETAILED DESCRIPTION OF THE INVENTION
[0032] FIG. 1 depicts a block diagram of a medication monitoring system 100 suitable for use with the methods and systems consistent with the present invention. The medication monitoring system 100 includes a client device 102 , a patient information unit 104 and a remote device 106 connected to one another via a network 108 . The network is of the type suitable for connecting the client device 102 , patient information unit 104 and remote device 106 such as a circuit-switched network or a packet-switched network. Also, the network 108 may include a number of different networks, such as a local area network, a wide area network such as the Internet, telephone networks including telephone networks with dedicated communication links, connection-less network, and wireless networks. The client device 102 includes an image capture unit 110 and an image analysis unit 112 . The image capture unit 110 may be any image capturing device such as a digital camera. The patient information unit 104 includes a patient information unit 114 , video connection unit 116 and patient management unit 118 .
[0033] FIG. 2A shows a more detailed depiction of the client device 102 . The client device 102 comprises a central processing unit (CPU) 202 , an input output (I/O) unit 204 , a display device 206 , a secondary storage device 208 , a memory 210 and an image capture unit 110 . The client device 102 may further comprise standard input devices such as a keyboard, a mouse, a digitizer, or a speech processing means (each not illustrated).
[0034] The client device 102 's memory 210 includes a Graphical User Interface (GUI) 212 which is used to gather information from a user via the display device 206 and I/O unit 204 as described herein. The GUI 214 includes any user interface capable of being displayed on a display device 206 including, but not limited to, a web page, a display panel in an executable program, or any other interface capable of being displayed on a computer screen. The secondary storage device 208 includes an image analysis unit 216 . Further, the GUI 214 may also be stored in the secondary storage unit 208 . In one embodiment consistent with the present invention, the GUI 214 is displayed using commercially available hypertext markup language (HTML) viewing software such as, but not limited to, Microsoft Internet Explorer®, Google Chrome® or any other commercially available HTML viewing software.
[0035] FIG. 2B shows a more detailed depiction of the patient information unit 104 . The patient information unit 104 comprises a CPU 222 , a I/O unit 224 , a display device 226 , a secondary storage device 228 , and a memory 230 . Patient information unit 104 may further comprise standard input devices such as a keyboard, a mouse, a digitizer, or a speech processing means (each not illustrated). The secondary storage device 228 may include a patient information unit 234 . The patient information storage unit 234 may be a database such as an Oracle, SQL or Access database.
[0036] The memory 230 in patient information unit 104 includes a GUI 232 which is used to gather information from a user via the display device 226 and I/O unit 224 as described herein. The GUI 232 includes any user interface capable of being displayed on a display device 226 including, but not limited to, a web page, a display panel in an executable program, or any other interface capable of being displayed on a computer screen. The GUI 232 may also be stored in the secondary storage unit 228 . In one embodiment consistent with the present invention, the GUI 232 is displayed using commercially available HTML viewing software such as, but not limited to, Microsoft Internet Explorer®, Google Chrome® or any other commercially available HTML viewing software.
[0037] FIG. 3A depicts a process of remotely instructing a user in the use of a pharmaceutical. In step 302 , a user of a pharmaceutical receives a package including the pharmaceutical and dispensing equipment such as syringes. The package may include instructions for the user to connect to an external location using video communication system including, but not limited to, Skype, Facetime or Vidyo. In step 304 , the user connects to the external location and initiates a video communication session via the video connection unit 114 . When the user connects to the remote location via the video connection unit 114 a professional, such as a pharmacist trained in the administration of the pharmaceuticals included in the package, will discuss the correct method of taking each of the medications included in the package. Further, the professional will answer any questions posed by the user concerning the usage, storage or any other aspect of the pharmaceutical.
[0038] In step 306 , the professional will have a similar package as the patient and may ask the user to remove each item in the package one item at a time with the professional, so the professional can describe each item and instruct the user in its proper use. The professional may also instruct the user in how to administer a dose of each pharmaceutical included in the package. As an illustrative example, the professional may instruct a user in the proper method to draw a pharmaceutical from a vial and inject the pharmaceutical. In step 308 , the professional confirms that the correct pharmaceuticals have been sent to the user, and that the user understands when and how to administer each pharmaceutical. The professional may also confirm that the proper dosage of the pharmaceutical is taken by the user. In step 310 , the professional instructs the user by demonstrating proper pharmaceutical drawing and syringe insertion on an object representing the user's body. In step 312 , the professional views the user administering the medication. In step 314 , the professional provides comments and observations to assist the user in properly administering the pharmaceutical.
[0039] FIG. 3B depicts an embodiment of a technician interface used during a video conference. The interface includes a video display portion 320 that is configured to display a video image of the user after the connection is established. The top portion of the interface includes a patient name gathering portion 322 , a date gathering portion 324 and a medication listing portion 326 . The medication listing portion 326 may allow the professional to view and select any of the medications currently prescribed to the user. In addition, the medication listing portion may allow the professional to add new medications to the list of medications prescribed to the user. A video portion 328 is positioned on one side of the video display portion 320 to allow the professional to view all recorded video associated with the user and each medication prescribed to the user. In one embodiment, when the professional selects a new medication from the medication listing portion 326 , a listing of recorded video associated with the user and the medication are displayed in the video portion 328 . A record button 330 allows the user to record any portion of the video stream from the video conference to the information storage unit 234 .
[0040] FIG. 3C depicts an embodiment of the technician interface used while a portion of the video stream is recorded. When the record button is engaged, the video portion 320 displays a notes section 332 allowing the professional to enter observations concerning the user including observations of the user injecting and taking the medication. After the recording is stopped by the stop recording button 334 , the notes are stored in the information storage unit 234 and are associated with the user, the video clip and the medication. The professional may also prevent the user from viewing the video clip by selecting the viewable by patient box 336 .
[0041] The professional may record each session with the user to allow the user to replay the session at a later time. Further, the professional may provide the user with additional information in the form of documents and video segments to assist the user in the administration of the pharmaceutical. The professional may present the documents and/or video segments during the video communication session or may forward the user to a website containing the additional information. The professional may also end the call by asking the user a series of questions directed at ascertaining the user's understanding of the information covered during the video communication session. If the user fails to answer a predefined number of questions correctly, the professional may request a follow up video communication with the user to review the information covered in the video communication session and mark the follow up in the notes section 332 of the display. In one embodiment, the follow up conversation is transmitted to a scheduling system, such as Microsoft Outlook, and a reminder notice is automatically generated and transmitted to the user and the professional after a predetermined period of time has elapsed.
[0042] When the interface is executed, the video conferencing unit 116 retrieves all video stored in the information storage unit 234 that is associated with the user along with all notes associated with the user. In one embodiment, the system allows a professional to search for video portions associated with a user or with a medication. By allowing the professional to search and view video portions on a specific user or medication, the professional can quickly learn important information on a user or medication. As an illustrative example, video and note can be stored commemorating the first instance a user took a medication by a first professional. The recorded video and note can be viewed at a later time by a second professional who is unfamiliar with the patient to familiar the second professional with the user and the user's interactions and reactions to the medication.
[0043] FIG. 3D depicts an embodiment of an interface used by a patient. The interface includes the name gathering portion 322 , date portion 324 and a video selection portion 320 . The video selection portion 320 displays a listing of all recorded video the patient is allowed to view. When the interface is executed, the video connection unit 116 retrieves all video portions associated with the patient and authorized for patient viewing from the information storage unit 234 and displays them in the video portion. When selected, each video portion will be displayed in the video display portion 320 . In one embodiment, the patient management unit 118 may monitor the number of times a user views a video and may transmit a request for an additional consultation to the patient to confirm their understanding of the treatment. In another embodiment, the patient management unit 118 may notify a professional when a patient views a video more than a predetermined number or times. In another embodiment, the patient management unit 118 may create a notification in the video conferencing unit 116 to notify the next professional contacting the patient that the patient has viewed a video multiple times.
[0044] FIG. 4 depicts a schematic representation of a process executed by the image analysis unit 112 operating on the client device 102 . In step 402 , the image analysis unit 104 retrieves a user identification associated with the client device 102 or the client. The identification may be a user name and password, a biometric identifier such as a finger print or a iris scan, a phone number associated with the client device, or any other attribute that can identify the user of the client device 102 . In one embodiment, the image capture unit 110 may capture an image of the user's body and compare the image to a known image of the user's body to determine the identification of the user. In step 404 , the image analysis unit 112 transmits a message including the client identification to the patient information unit 104 to retrieve medication and dosage information from the patient information storage unit 114 . The medication and dosage information may include bar code information of the medication previously sent to the client, the type and quantity of the medication being taken by the patient, the duration between dosages for the patient, and the size and type of syringe used to inject the medication.
[0045] In step 406 , the image capture unit 110 captures the image of a bar code affixed to the medication previously provided to the user. To capture the image of the bar code, the image capture unit 110 captures a digital image of the bar code which is passed to the image analysis unit 112 . The image analysis unit 112 determines the bar code value by analyzing the widths and spacings in the bar code to determine the bar code value. In step 408 , the image analysis unit compares the bar code value captured from the medication with the bar code value sent from the patient information storage unit 114 . In step 410 , if the values do not match, the image analysis unit 112 notifies the user to not take the medication and provides detailed instructions to the user on how to return the medication for replacement. The image analysis unit 112 may also transmit an incorrect medication notice to the remote device 106 to notify the sender of the medication that the incorrect medication was sent to the user.
[0046] In determining if the medication is the correct medication for the user, the image analysis unit 112 may also analyze the label affixed to the medication vial to determine the medication is the correct medication for the user. The image analysis unit 112 may perform object character recognition on an image of the label to determine the name and concentration of the medication sent to the user. The image analysis unit 112 may compare the name and dosage information with the name and dosage information provided by the patient information storage unit 114 . If the information from the vial does not match the information from the patient information unit 114 , the image analysis unit 112 notifies the user and the remote device 106 o the incorrect medication.
[0047] In step 412 , if the medication is the correct medication, the image analysis unit 112 may retrieve a video and information on injecting the medication properly from the memory 210 and present the video to the user for viewing. In another embodiment, the image analysis unit 112 may initiate a communication connection with a pharmacist operating the remote device 106 to describe the appropriate method of injecting the medication. The communication connection may be established using any known communication method including a cellular phone call, or by a video conferencing session using video conferencing software such as Skype or Facetime. In one embodiment, the communications between the pharmacist is recorded and stored in the patent information storage unit 104 and is associated with the patient information. The image analysis unit 112 may provide an interface where the user retrieves the stored video for later viewing.
[0048] In step 414 , the image analysis unit 112 retrieves an image of the vial holding the medication to determine the level of the liquid in the vial. The image analysis unit 112 may instruct the user to capture an image of the vial using a digital camera in the client device. In step 416 , the image analysis unit 112 determines the level of the liquid in the vial based on the captured image. To determine the level, the image analysis unit 112 identifies the outline of the vial using known pixel analysis techniques such as Canny edge detection or SUSAN edge detection or any other known edge detection technique, and measures the distance from the a known reference point, such as the top of the vial to the top surface of the liquid level. The image analysis unit 112 can then determine the volume remaining in the vial using the dimensions in the vial that are retrieved from the patient information storage unit 114 . In addition, the image analysis unit 112 identifies the top level of the liquid in the vial using the same or similar edge detection techniques. In the event the level in the vial is below a threshold value, the image analysis unit 112 may notify the remote device 106 that a refill of the medication is required. The image analysis unit 112 may notify the remote device 106 using any known messaging method including SMS messaging, e-mail, connecting to an order entry system via an ODBC connection or any other method of automatically ordering medication.
[0049] In step 418 , the image analysis unit 112 notifies the user to draw a specific dosage from the vial into a syringe. In step 420 , the image analysis unit requests the user capture an image of the syringe filled with the medication. In step 422 , the image analysis unit 112 determines the level of liquid in the syringe and the dosage amount using the edge detection techniques described previously. The image analysis unit 112 may analyze the liquid level indicator markings on the side of the syringe and compare the proximity of the liquid level to the level indicator markings on the side of the syringe to determine the level of the medication in the syringe.
[0050] The image analysis unit 112 may also analyze the image of the syringe for proper placement to determine the liquid level shown in the image is accurate. As an illustrative example, the image analysis unit 112 may determine the angle between the edge of the syringe and the liquid level line to determine if the syringe is tiled while the image was taken. If the syringe is tilted, the image analysis unit 112 recalculates the liquid volume in the syringe using the known dimensions of the syringe that are stored in the patient information storage unit 114 . In step 324 , the image analysis unit 112 compares the dosage in the syringe with the prescribed dosage from the patient information system 114 . If the dosage in the syringe is outside a dosage threshold, the image analysis unit 112 notifies the user to redraw the dosage in to the syringe. In step 326 , if the dosage is within the predetermined dosage threshold, the image analysis unit 112 notifies the user to inject the dosage.
[0051] In one embodiment, the image analysis unit 112 records the time and type of each medication taken by the user. When the user requests the next dosage of medication be taken, the image analysis unit 112 determines if the correct interval has expired for the user to take the next dose. The image analysis unit 112 may provide a user interface such as a clock showing the time remaining before the next dose may be taken, or may provide an audible alarm notifying the patient when the next dosage is due to be taken.
[0052] FIG. 5 depicts a schematic representation of a process executed by the image analysis unit 112 . In step 502 , the image analysis unit 112 retrieves the injection information associated with a user and with a medication associated with the user from the patient information storage unit 114 . In step 504 , the image analysis unit 112 displays the area of the body where the user should inject the medication. In step 506 , the image analysis unit 112 captures an image of the injection region on the user's body. In step 508 , the image analysis unit 112 identifies the edges of the injection region using the edge detection techniques previously discussed. The edges of the region may be identified by first identifying an edge of the user's body, such as the edge of an arm, and measuring a predefined distance from the edge. The image analysis unit 112 may request the user place an item of a known size, such as a coin, in the image to set a distance scale for the image.
[0053] In step 510 , the image analysis unit 112 identifies the location of the injection point on the image. The image analysis unit 112 may determine the injection point using a distance from an identified edge, such as the side of an arm, to determine where the needle should be injected. In step 512 , the image analysis unit 112 high lights the location of the injection point on the image of the user's body. In step 514 , the image analysis unit 112 requests the user place the needle of the syringe at the injection location. In step 516 , the image analysis unit 112 captures an image of the needle at the injection location. In step 518 , the image analysis unit 112 compares the location of the needle in the captured image to the calculated injection location. In step 520 , if the needle is in the proper injection location, the image analysis unit 112 requests the user inject the needle. In step 522 , if the needle is not in the proper location, the image analysis unit 112 instructs the user to move the needle to the proper location. The image analysis unit 112 may also confirm the needle is positioned at the proper angle for insertion into a vein.
[0054] FIG. 6 depicts a schematic representation of a process performed by the patient information unit 104 . In step 602 , the video connection unit 116 connects a user to a technician via a live video connection using any of the previously methods of establishing a video connection. In step 604 , a trained technician retrieves information from a user connected via the video connection. The information may include, but is not limited t the patient's name, date of birth.
[0055] It is to be understood that both the foregoing general description and the following detailed description are exemplary and are intended to provide further explanation of the invention claimed. The disclosed configuration is the preferred embodiment and is not intended to preclude functional equivalents to the various elements.
[0056] The accompanying drawings, which are incorporated in and constitute part of this specification, are included to illustrate and provide a further understanding of the invention. Together with the description, the drawings serve to explain the principles of the invention. | A medication monitoring system including a patient information unit having a processor, a memory and a patient monitoring unit and a program executing in the memory executing the steps of communicatively coupling a first device with a second device, transmitting live images from the first device to the second device, analyzing the content of the live images to identify at least one biometric attribute of a user in the image and at least one bar code on a container in the image, determining whether the bar code is associated with at least one biometric attribute, and notifying the user whether to consume the contents of the container based on the association of the bar code with the biometric attribute. | 6 |
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